untitled

1

2

3

4

5

6

7

8

9

10

11

12

SPE LC GC LC/G C MS : / (LLE) (SLE) SPE : SPE (PPT) LLE LLE SPE SPE : SPE SPE / ph, pk, log P 13

SPE SPE SOLA HRP,C18,C8 Phenyl Retain PEP SOLA HRP,C18,C8 Retain PEP SOLA HRP,Hypercard Retain PEP SCX SAX Aminopropyl & SOLA SCX,Verify CX Retain CX & SOLA SAX,Verify AX Retain AX SOLA HRP,C18,C8, Phenyl Retain PEP Silica,Aminopropyl Cyano, Diol Silica,Florisil,Aminopropyl Cyano, Diol SCX SAX Aminopropyl & Verify CX & Verify CX 14

Thermo SPE ( ) - HyperSep Retain PEP/SOLA HRP - 550 750m 2 /g 40 60µm 55 90Å PH 1-14 C18 ( 3-5 ) HyperSep Retain-CX/SOLA SCX 550 750m 2 /g 40 60µm 55 90Å HyperSep Retain-AX/SOLA SAX 550 750m 2 /g 40 60µm 55 90Å - HyperSep C18 470 530m 2 /g 40 60µm 60Å HyperSep C8 C18 470 530m 2 /g 40 60µm 60Å C8 C18 HyperSep Phenyl 470 530m 2 /g 40 60µm 60Å Phenyl HyperSep Hypercarb 100% ph SPE 15

- - HyperSep Silica 530m 2 /g 40 60µm 60Å HyperSep Florisil 289m 2 /g 40 60µm 60Å Florisil AOAC EPA (PCB) HyperSep Cyano 470 530m 2 /g 40 60µm 60Å Cyano HyperSep Diol 470 530m 2 /g 40 60µm 60Å HyperSep Aminopropyl 470 530m 2 /g 40 60µm 60Å HyperSep SAX 470 530m 2 /g 40 60µm 60Å SAX HyperSep SCX 470 530m 2 /g 40 60µm 60Å SCX HyperSep Verify-CX 470 530m 2 /g 40 60µm 60Å Verify-CX C8 HyperSep Verify-AX 470 530m 2 /g 40 60µm 60Å Verify-AX C8 THC 16

SPE - 1. 2 2. 3. 1 mm 4. 5. 3 1mm 6. 4 1 SPE PH SPE ph SPE SPE / SPE 1mL/min 5 6 17

SPE SPE SPE Silica,Florisil / C18 C8 PEP SOLA HRP / 1-2ml/min 1-2ml/min / 5:95 100% (Retain CX/SOLA SCX/Verify CX) / (Retain AX/SOLA SAX/Verify AX) / 1-2ml/min 1-2ml/min 2% 100% 2% 100% 2% 2% 18

SPE SPE SPE SPE HyperSep SPE ph 100% : ph - ph - ph - ph - - - - 1 ph ph ph - pka 2 ph ) - pka 2 ph ph ph ph pka pka2ph pka2ph 19

2 HyperSep SPE pka 3.0 pka 1.3 2.4 10.5 (1-position), 1.5 (4-position) 11.0 2.9 2.5 4.8 1.8 3.5 1.5 3.3 8.2 1.9 20

HyperSep Retain PEP 30mg 1mL SPE 60107-201 1. 1mL 1mL 2. 1mL 500ng/mL 3. 0% /100% 90% 10% 10% 4. 0.5mL 100% 4 HyperSep Retain PEP / 30% /70% 1.5mL 500µL HyperSep lietain-cx 30mg 1mL 60107-301 1. 1mL 0.1% 1mL 0.1% 2. 1mL 0.1% 500ng/mL 3. 1mL 0.1% 1 4. 1mL 0.1% 2 5. 5% / 20% /80% 80% /20% 10% 6. 0.5mL 5% 4 HyperSep lietain-cx / 50% 5% /50% 5% 1.5mL 500µL HyperSep Phenyl 100mg 1mL 60108-386 1. 1mL 1mL 2. 500ng/mL 1mL 3. 10% 90% 4. 0.5mL 100% 4 HyperSep Phenyl / 20% /80% 1.5 ml 500µL 21

/ / ph H ph / / / (SLE) SLE 200mL SLE LLE LLE LLE LLE : (1) SLE 5-10 (2) (3) 22

- SPE-LC/MS 200mg 3mL HyperSep Retain-CX ( 60107-304) 2g 0.01g 50mL 0.2mol/L ph5.2 10mL - / 40µL 3min 37 16h 3min 10min 1mol/L 1mL 10min 50mL 3mL 3mL 3mL 0.5mol/L 3mL 3mL 3mL 5% 1. LC/MS/MS LC/MS Hypersil Gold 5µm 2.1 150mm 25005-152130 A: 5mM B: 1. Time(min) A(%) B(%) 0 0.5 5 10 10.1 12 90 90 10 10 90 90 10µL 250µL/min MS ESI SRM 4500V 350 10 10 90 90 10 10 2. LOQ 0.1µg/kg 0.5 µg/kg 3. 75-120% 2. - LC/MS/MS 1ng/mL 23

SPE-LC/MS 60mg 3mL HyperSep Retain-AX ( 60107-403) 5g 50mL 10mL 1min 10min 5000r/min 15mL 1mL 50 3mL 0.1mol/L NaOH ph=11.0 5min 5000r/ min 3mL 3mL 3mL 5% 3mL 5% LC/MS Hypersil Gold 5µm 2.1 150mm 25005-152130 0.1% A : B 1. Time(min) A(%) B(%) 0 5 8 12 12.1 14 70 70 10 10 70 70 30 30 90 90 30 30 1. LC/MS/MS 1. 2. - 3. - 4. 5. - 6. - 10µL 250µL/min MS ESI SRM 3500V 350 2. LOQ - - - - 0.1µg/kg - - - - 1.0µg/kg 3. 65-115% 2. 6 LC/MC/MS 1ng/mL 24

SPE-LC/MS 500mg 3mL HyperSep C18 ( 60708-304) 5g 10% 3mL 10mL 30s 10min 4 6000r/min 10min 10mL 40 30% 5mL 3mL 3mL 2mL 30% 5mL LC/MS Hypersil Gold 5µm 2.1 150mm 25005-152130 0.1% A : B 1. Time(min) A(%) B(%) 0 5 12 12.1 14 90 10 10 90 90 10 90 90 10 10 10µL 250µL/min MS ESI SRM 4500V 350 25

1. LC/MS/MS 2.11 LC/MC/MS 1.0ng/mL 2. LOQ 0.1µg/kg 0.5µg/kg 3. 50-105% 26

SPE-LC/MS 500mg 3mL HyperSep Silica ( 60108-315) 2 0.05 g 50mL 15mL 3min 10min 4000rpm 50mL 0.1mol/L NaOH 10mL 15mL 40 1.0mL 5mL 5mL 5mL 5mL 6:4 v/v LC/MS Hypersil Gold 5µm 2.1 150mm 25005-152130 0.01% A : B 1. Time(min) A(%) B(%) 0 18 23 23.1 28 70 40 40 70 70 30 60 60 30 30 27 1. LC/MS/MS 2 LC/MC 10µL 250µL/min MS ESI SRM 3500V 350 2. LOQ 0.1µg/L 0.2 µg/kg 0.2µg/L 0.2µg/kg 0.2µg/L 0.5µg/kg 3. 60-110%

SPE-LC/MS 200mg 6mL HyperSep Retain-PEP ( 60107-212) 5g 50mL 100µL 1µg/mL 13 C- 20g 20mL 25g 2 3000r/min 10 10mL 30s 10mL 100mL 10mL 1 40 0.5mL 4mL 6mL 6mL 2mL 5min 6mL 6mL 1~2mL/min 1. LC/MS/MS LC/MS Hypersil Gold 5µm 2.1 150mm 25005-152130 A: B:0.1% 2mM 1. (min) 0 1 7 9 12 12.1 12.3 14.8 15 A 10 10 35 70 70 10 10 10 10 B 90 90 65 30 30 90 90 90 90 (µl/min) 250 250 250 250 250 250 300 300 250 10µL 250µL/min MS ESI SRM 4500V 350 28

1. 17 2µg/kg LC/MC/MS 2. 2µg/kg 3. 50%-114% 29

SPE-HPLC 200mg 3mL HyperSep Retain PEP ( 60107-204) 5.00g 25mL Mcllvaine 2mL50% 6000rpmin 10min 20mL ph 4.5 3mL 3mL 3mL 5% 3mL HPLC LC/MS Hypersil Gold C18 5µm 4.6 150mm 25005-154630 0.1% A : B 10 10-40%B 1.5mL/min UV@350nm 25 10µL (1) (2) (3) (4) (5) 30

SPE-HPLC,LC/MS 200mg 6mL HyperSep Retain-AX ( 60107-412) 2g 30mL 50mM ph7.4 6mL 6mL 5M NaOH 6mL 5mL 1-2mL/min 6mL5% 1mL 6mL 4% 0.4mL HPLC Hypersil Gold aq 5µm 150 4.6mm 25305-154630 A10mM KH 2 PO 4 ph3b 20%A~35%A 0~30min 1mL/min UV@280nm 35 5µL HPLC LC/MS Thermo Scientific Hypersil GOLD 2.1 50 mm 3µm 25003-052130 A: 0.5% B: / 0.5% 1:1 V/V 20µL 300µL/min MS ESI SRM 3000V 350 31 1. 2. 3. 4.

1.16 LC/MS SRM 20µg/kg 2. 60-110 % 32

200mg 3mL HyperSep Retain-CX ( 60107-304) 2.0g 8mL 10mmol/L KH 2 PO 4 0.4mmol/LEDTA 2% )10,000 rpm 10min 1 10,000rpm 10min 3mL 3mL 1-2mL/min 5mL 5mL 5% LC/MS LC/MS Hypersil Gold aq 5µm 100 2.1 mm 25305-102130 0.1%HFBA /0.1%HFBA 52:48 20µL 200µL/min MS ESI SRM 4500V 350 (1) C1a (2) C2 33

SPE-LC/MS 200mg 3mL HyperSep Retain PEP ( 60107-204) 4g 8mL 2min 4000rpm 5min 5mL 4mL 1min 4000rpm 3min 1mL 50:50 / 10mL 3mL 3mL 1-2mL/min 3mL 30% 3mL 1. 0.050µg/kg LC/MS Hypersil GDLD TM 50 mm 2.1 mm 1.9µm 25002-052130 A: B: (min) A% 0.0-0.6 5% 2.3 100% 2.35-3.0 5% 20µL 500µL/min MS ESI SRM 3000V 300 2. LOQ LOQ 0.050µg/kg 3. 94%-104% 34

SPE-LC/MS 200mg 3mL HyperSep C18 ( 60108-303) 5g 5% 5mL 0.17mol/L 5mL 50mL5000rpm 10min 3mL 3mL 1-2mL/min 3mL 6mL 20% LC/MS BioBasic AX 5µm 150 2.1mm 73105-152130 A:10mM B: 10%B 20µL 200µL/min MS ESI 3000V 300 1. LC/MS/MS (1) (2) (3) (4) G 35

SPE-HPLC 200mg 3mL HyperSep C18 ( 60108-303) 5g 20mL 2min 10000rpm 5min 20mL 5mL 20% 3mL 3mL 1-2mL/min 3mL 2*2 ml LC/MS Hypersil GOLD TM 150 4.6mm 5µm 25005-154630 A: 0.1% B: + 0.1% 35:65 20µL 1mL/min UV 235nm 25 1. HPLC 2. 95%-99% 36

SPE-HPLC 60mg 3mL HyperSep Retain PEP ( 60107-203) 15mL 25mL Mcllvaine 5 8000rpm 10min 3mL 3mL 3mL 5% 3mL LC/MS Hypersil Gold 5µm 4.6 150mm 25005-154630 0.1% A : B 10 10-40%B 1.5mL/min UV@350nm 25 10µL HPLC (1) (2) (3) (4) (5) 37

SPE-LC/MS 200mg 3mL HyperSep C18 ( 60108-303) 5mL 5% 5mL 0.17mol/L 5mL 50mL5000rpm 10min 3mL 3mL 1-2mL/min 3mL 6mL 20% LC/MS/MS LC/MS BioBasic AX 5µm 120 2.1mm 73105-152130 A: 10mM B: 10%B 20µL 200µL/min MS ESI 3000V 300 (1) (2) (3) (4) 38

60mg 3mL HyperSep Retain PEP ( 60107-203) 0.5g d5-cap 0.3 ppb 1mL 1min 14000rpm 10min 2mL 30% 3mL 3mL 1-2mL/min 3mL 30% 2mL 1. 0.050µg/kg LC/MS Hypersil GOLD TM 50 mm 2.1 mm 1.9µm 25002-052130 A: B: (min) A% 0.0-0.6 5% 2.3 100% 2.35-3.0 5% 20µL 500µL/min MS ESI SRM 3000V 300 0.050µg/kg 39 2.LOQ LOQ 0.050µg/kg 3. 94%-104% CAP Spiking Level (µg/kg) Within-laboratory Reproducibility n=20 Meam(%) SD(µg/kg) %RSD 0.05 97% 0.0065 14% 0.15 101% 0.020 13% 0.30 104% 0.037 11% 0.50 94% 0.042 8.0% Table 3: Recovery and Reproducibility Data

60mg 3mL HyperSep Retain PEP ( 60107-203) 15mL 1 2mL 1 1mL 4,000rpm HyperSep Retain PEP 1 5mL 1 5mL 1 2mL/min 1 10mL 1 5mL 1 2mL/min 5mL <40 1,000µL 5µL LC/MS HPLC Hypersil GOLD 5µm 100 2.1mm 25005-102130 SPE-LC/MS 50mg 1mL HyperSep Hypercarb ( 60106-303) 1g 12mL 50% 2min 4000rpm 10min 5mL ph=3 3mL 3mL 1-2mL/min 3mL LC/MS/MS LC/MS BioBasic TM AX 2.1 150mm 5µm 73105-152130 0-5min - -50mM 85:10:5 5min-10min 9:1 / 20µL 400µL/min MS ESI SRM 3000V 350 40

SPE-LC/MS 60mg 3mL HyperSep Retain-CX ( 60107-303) 5g /10mL 1% 50mL 2mL 2% 20min 3mL 3mL 6mL 2mL/min 3mL 3mL 5min 5mL 5% 1-2mL/min1mL LC/MS Syncronis HILIC 5µm 2.1 100mm 97505-102130 A: B:10mM / ph=3 85:15 10µL 250µL/min MS ESI MRM 3500V 350 LC/MS/MS 41

SPE-LC/MS 60mg 3mL HyperSep Retain-CX ( 60107-303) 1g 2mL 5mL1% 2min 3000rpm 2min 3mL 3mL 6mL 2mL/min 3mL 3mL 5min 5mL 5% 1-2mL/min1mL LC/MS Syncranis HILIC 5µm 2.1 100mm 97505-102130 A: B:10mM / ph=3 85:15 10µL 250µL/min MS ESI MRM 3500V 350 LC/MS/MS 42

SPE-HPLC,GC/MS 1g 6mL HyperSep Silica ( 60108-426) 2.5g 10mL 6:4 30s 5min 4000r/min 5min 40 30min-40min 2 40 2mL 6mL 6mL 2mL 4mL 10mL : 2:3 HPLC Hypersil Green PAH 3µm 100 4.6mm 31103-104630 A: 99:1 : B: 99:1 : 50:50-5min 50:50-25min 0:100 2mL/min 10µL UV 254nm 20 PAH HPLC (1) (2) (3) (4) (5) (6) (7) (8) (9) (a) (10) (11) (b) (12) (k) (13) (a) (14) (a,h) (15) (ghi) (16) (1,2,3-cd) 43

GC/MS TraceGOLD TG-5SiIMS 30m 0.25mm 0.25µm TG-17SiIMS 30m 0.25mm 0.25µm 26096-1420 26072-1420 90 1min 25 /min 280 4 /min 320/min 2min TraceGOLD TG-5SiIMS 90 1 min 30 /min 250 4 /min 330 5min TraceGOLD TG-17Si1 MS 1.2mL/min 1µL 250 1min 30mL/min MS 1. 100ppb 18 TIC 1. TG-17SiIMS 30m 0.25mm 0.25µm 10µg/mL18 TIC 2. 5SiIMS 30m 0.25mm 0.25µm 10µg/mL18 PAH TIC (a) (b) (j) (k) (a) (e) (1,2,3-cd) (1,2,3-cd) (g,h,i) 44

SPE-GC/MS,LC/MS QueChERS ( 60105-341 60105-204) 1. 5.0g 25mL 10mL 6g MgSO 4 1.5g Thermo QueChERS PN:60105-341 1min 4000r/min 2min 40 5mL 2. 5.0g 50mL 5mL 15mL 6g MgSO 4 1.5g Thermo QueChERS PN:60105-341 1min 4000r/min 2min 40 5mL 50mg PSA 50mg C18 150mg MgSO 4 Thermo QueChERS clean-up PN:60105-204 1min 4000r/min 2min GC/MS TG-5MS 30m 0.25mm 0.25µm 26098-1420 60 1min 15 /min 230 1min 5 /min 280 4min 1mL/min 10µL 250 0.8min 50mL/min MS GC/MS 1. 25ppb 16 2. 45

LC/MS Thermo AccuCore RP-MS 2.6m 100mm 2.1mm 17126-102130 A: B: (min ) A: B: 0 60% 40% 12 0 100% 15 0 100% 0.3mL/min 3µL MS ESI SRM 3700V 350 1.22 2. 80-120% 46

200mg 3mL HyperSep Retain-CX ( 60107-304) 1 5g 10 25mL / 50:50 5 5mL 1mL 100mM HCI 1mL 5 2mL 5 SPE HyperSep Retain-CX 1 3mL 1 3mL 3 1 2mL/min 1 3mL 100mM 1 1mL 10 5 ) 1 2mL 5%NH 4 OH 1 3mL 5%NH 4 OH 1 2mL/min 40 Syncronis HILIC 5µm 2.1 100mm 97505-102130 A: B:10mM / ph=3 85:15 10µL 250µL/min MS ESI MRM 3500V 350 LC/MS/MS 47

LC/MS/MS 200mg 6mL HyperSep Verify-CX ( 60108-722) 200mg 6mL HyperSep Retain-AX ( 60107-412) 1 5g 10 25mL CH 3 CN/ 50:50 5 5mL 1mL 100mM HCI 1mL CH 2 CI 2 5 2mL CH 2 CI 2 5 SPE HyperSep Verify CX 1 3mL CH 3 OH 1 3mL 3 1 2mL/min HyperSep Retain-AX HyperSep Verify-CX 1 1mL HyperSep Retain-AX HyperSep Retain-AX 1 3mL100mM HCI 1 1mL CH 3 OH 10 5 1 2mL 5% NH 4 OH CH 3 OH 1 3mL 5% NH 4 OH CH 3 OH 1 2mL/min 40 1,000µL CH 3 CN * 5µL LC/MS HyperSep Retain-AX ph 7** HyperSep Retain-AX 1 3mL CH 3 OH 1 3mL 3 PH 7 1 2mL/min HyperSep Retain -AX 1 3mL 1 1mLCH 3 OH 1 3mL CH 3 OH 1% HCI 1 2mL CH 3 OH 1% HCI 1 2mL/min 40 100µL * 5 LC/MS MRM 127.1/85.1 2, 4 6- * 127.1/67.0 127.8/84.9 * 2, 4 6- ** 100 200µL5%(V/V)(aq)NH 4 OH PH HPLC Hypersil GOLD HILIC 3µm 150 2.1mm 26503-152130 48

SPE-LC/MS 200mg 3mL HyperSep Retain PEP ( 60107-204) 60mg 3mL HyperSep Retain-CX ( 60707-303) 2g 10mL 20min 4000rpm 10min 5mL 5min 5mL 15mL 3 40 3mL SPE 3mL 3mL 1-2mL/min HyperSep Retain PEP 3mL 3mL1% HyperSep Retain CX 1mL LC/MS Thermo Scientific Hypercarb 2.1 50mm 5µm 35005-052130 10µL 400µL/min MS ESI SRM 3500V 375 1. 1ng/mL LC/MS 2. 1g 10% 200 500 800ng 3 93.2%~ 97.4% RSD 10% 3. Cereal 1 Cereal 2 Potato Chip 1 Potato Chip 2 Injection 1 17.17ng/mL 55.93ng/mL 57.11ng/mL 29.18ng/mL Injection 2 17.00ng/mL 56.18ng/mL 56.52ng/mL 29.14ng/mL Mean 17.09ng/mL 56.06ng/mL 56.82ng/mL 29.16ng/mL Extraction Vol. 20.0mL 20.0mL 20.0 ml 20.0mL Mass Sample 2.003g 2.007g 2.021 1.995 Acrylamide Conc 171ng/g 559ng/g 562ng/g 292ng/g Table 2: Results of acrylamide assay from food samples 49

SPE-LC/MS 200mg 3mL HyperSep Retain-AX ( 60107-404) 2g 20mL 5% 6mL 6mL 5M NaOH 6mL 5mL 1-2mL/min 3mL 5% 3mL 3mL 4% 0.4mL 60-110% LC/MS Thermo Scientific Hypersil GOLD 2.1 50 mm 3µm 25003-052130 A: 0.5% B: / 0.5% 1:1 V/V 20µL 300µL/min MS ESI SRM 3000V 350 SPE-HPLC 500mg 6mL HyperSep C18 ( 60108-305) 5g 25mL 6mL 6mL 1-2mL/min 6mL 6mL 1mL LC/MS/MS 100µL N- - 1:1 30s, 150µL - 1:1 30s 750µL 15min HPLC LC/MS Hypersil Gold 5µm 2.1 150mm 25005-152130 /0.1% =75:25 10µL 250µL/min MS APCI HPLC Hypersil GDLD TM 150mm 4.6mm 5µm 25005-154630 / =92:8 20µL 1mL/min 365nm475nm 25 50

SPE-LC/MS 200mg 6mL HyperSep Retain-PEP ( 60107-212) 5g 15mL 20mL 100mL 20mL 1 40 0.5mL 4mL 6mL 6mL 6mL 5min 6mL 6mL 1-2mL/min 1. LC/MS/MS LC/MS Hypersil Gold 5µm 2.1 150mm 25005-152130 A: B:0.1% 2mM 1. (min) 0 1 7 9 12 12.1 12.3 14.8 15 A 10 10 35 70 70 10 10 10 10 B 90 90 65 30 30 90 90 90 90 (µl/min) 250 250 250 250 250 250 300 300 250 10µL 250µL/min MS ESI SRM 4500V 350 51

1.17 2µg/kg LC/MS/MS 2. 2µg/kg 3. 60%-120% 52

SPE-HPLC 60mg 3mL HyperSep Retain PEP ( 60107-203) 5mL 25mL Mcllvaine ph 4.1 5 8000rpm 10min 3mL 3mL 3mL 5% 3mL HPLC Hypersil Gold 5µm 4.6 150mm 25005-154630 0.1% A : B 10 10-40%B 1.5mL/min UV@350nm 25 10µL HPLC (1) (2) (3) (4) (5) 53

SPE-LC/MS 200mg 3mL HyperSep SCX ( 60108-422) 200mg 3mL HyperSep C18 ( 60108-303) 10g 20mL 0.1 5min HyperSep SCX 3mL 3mL 5mL 0.1% 5mL 5mL 0.2mol/L ph=8 ph=2 HyperSep C18 HyperSep C18 3mL 3mL 5mL 5mL 1mL LC/MS LC/MS Hypersil Syncronis HILIC 5µm 2.1 50mm 97505-052130 A:100mM 100mM 0.2% B:100mM A(%) B(%) Time(min) 0 4 8 9 14 10 90 60 40 60 40 0.25mL/min 10µL 200µL/min MS ESI SRM 4500V 450 10 90 10 90 54

SPE-HPLC 200mg 6mL HyperSep Retain-PEP ( 60107-212) 5g 25mL ph8.0 0.1mol/L 6mL 6mL 2mL/min 6mL 5min 6mL 1-2mL/min1mL HPLC Betasil CN 5µm 150 4.6mm 70805-154630 A: B:20mM +20mM +2mM 20µL 1.25mL/min UV 210nm 45 HPLC 55

SPE-LC/MS 60mg 200mg 3mL HyperSep Retain PEP ( 60107-203,60107-204) 5g 20mL 100g 60mL /1% 3:2 15mL /1% 3:2 3mL 3mL 1-2mL/min 3mL30% 3mL 1. 0.1µg/kg LC/MS Hypersil GOLD TM 50 mm 2.1mm 1.9µm 25002-052130 A: B: min A% 0.0-0.6 5% 2.3 100% 2.35-3.0 5% 20µL 500µL/min MS ESI SRM 3000V 300 0.1µg/kg 2.LOQ LOQ 0.1µg/kg 3. 93%-99% 56

60mg 3mL HyperSep Retain-CX ( 60107-303) 100µg/mL (NOR-D5) 1µg/mL 5g 50mL 50µL *MNZDMZ 2-1- -5- (HMMNI) IPZ2-(2- )-1- -5- (IPZOH)RNZ 10mL 0.5mol/L 15 10mL 30 2,500rpm 3 50mL 10mL 40 10% 5mL ACN HyperSep Retain-CX 1 3mL 1 3mL 1 2mL/min 1 3mL 10 5 1 3mL 1 2mL/min 25µL LC/MS 0.20mL/min A 5mmol/L B HPLC Hypersil GOLD 3µm 150 2.1mm 25003-152130 SPE-HPLC 60mg 3mL HyperSep Retain-PEP ( 60107-203) 5.00g 100mL 50µL MC-RR YR LR LW LF 1µg 10000 r/min 1min 10mL 2min 15min 5min 3000r/min 0.5 ml 10mL 3mL 3 ml 6mL 3mL LC/MS Hypersil Gold 5µm 2.1 150mm 25005-152130 0.1% A : B 0.00min 20% 80% 4.00min 95% 5% 8.00 min 95% 5% 8.10min 20% 80% 10.00 min 20% 80% 10µL 250µL/min MS ESI SRM 3500V 350 57

1. LC/MS/MS 1.5 MCs 5µg/kg LC/MS/MS 2. MC-RR YR LR LW LF 0.7 1.0 0.8 1.2 1.3µg/kg 2. n=6 Compounds RR YR LR LW LF spiked level µg/kg Recovery % RSD % 2.0 97.3 4.0 5.0 95.4 3.2 10.0 93.7 2.1 2.0 92.6 4.1 5.0 101.3 3.4 10.0 85.3 1.3 2.0 95.5 2.9 5.0 93.1 2.1 10.0 92.1 1.1 2.0 91.6 3.9 5.0 95.2 2.4 10.0 94.7 2.0 2.0 85.2 4.1 5.0 97.6 2.8 10.0 95.1 2.2 3. 85-102% 58

SPE-LC/MS 200mg 6mL HyperSep Retain-CX ( 60107-314) 2g Mcllvaines ph2.6 / =50/50 10mL 5000rmp 20 SPE 6mL 5mL 5mL Mcllvaines ph 2.6 1-2mL/min 6mL 0.1 NHCI 6mL 50% / 6mL 10mL 50% 45% 5% V/V/V LC/MS Thermo Scientific Hypersil GOLD 2.1 50 mm 5µm 25005-052130 A: 0.1% B: 0.1% 40%A-5%A 0-5min 20µL 300µL/min MS ESI SRM 3500V 350 1. LOQ 0.05-0.1µg/kg 1. LOD µg/kg % RSD N=3 LOQ µg/kg %RSD N=3 R2 0.1 6.8 0.1 8.2 0.9984 0.1 12.0 0.11 2.0 0.9983 0.05 7.9 0.05 7.9 0.9990 0.05 13.5 0.11 1.2 0.9988 2. 500ng/kg ppt 50ng/kg ppt 59

SPE-LC/MS 60mg 3mL HyperSep Retain PEP ( 60107-203) 2g 4mL 0.5mL 0.5M HCL 200µL 50mM DMSO 1 min 37 14-16 5mL 0.1M K 2 HPO 4 0.4 M NaOH PH 7.0-7.5 3mL 3mL 1-2mL/min 5mL 2mL 30% 5mL LC/MS Thermo Scientific Hypersil GOLD 5µm 100 2.1mm 25005-102130 A: 0.5mM B: min %A %B 0 80 20 8.5 50 50 9.5 50 50 10 80 20 15 80 20 20µL 250µL/min MS ESI SRM 5000V 300 60

1. 0.05µg/kg 4 LC/MS 2.LOQ AHD AOZ SEM AMOZ LOQ0.05µg/kg 3. 4 79%-110% RSD 3 22% n=3 Fortification Level (µg/kg) AHD AOZ SEM AMOZ 0.05 82 13% 110 22% 89 15% 98 14% 0.5 88 4% 110 11% 100 11% 95 6% 2.5 109 3% 86 18% 79 19% 100 3% 61

SPE-HPLC 200mg 6mL HyperSep Retain-PEP ( 60107-212) 5g 10mL 2min 10000rpm 5min 20mL 35 10mL ph=8 6mL 6mL 10mL 2mL/min 6mL 5min 6mL 1-2mL/min1mL LC/MS Betasil CN 5µm 150 4.6mm 70805-154630 A: B: 20mM +20mM +2mM A/B 35:65 20µL 1.25mL/min UV 210nm 45 HPLC 62

SPE-HPLC,GC/MS 1g 6mL HyperSep Silica ( 60108-426) 6000r/min 10min 2.5g 10mL 6:4 30s 5min 4000r/min 5min 40 30min-40min 2 40 2mL 6mL 6mL 2mL 4mL 10mL : 2:3 HPLC 16 PAH Hypersil Green PAH 3µm 100 4.6mm 31103-104630 A: 99:1 : B: 99:1 : 50:50-5min 50:50-25min 0:100 2mL/min 10µL UV 254nm 20 16 PAH HPLC (1) (2) (3) (4) (5) (6) (7) (8) (9) (a) (10) (11) (b) (12) (k) (13) (a) (14) (a,h) (15) (ghi) (16) (1,2,3-cd) 63

HPLC 3 PAH Accucore C18 2.6µm 100 2.1mm 17126-102130 55% :45% 0.5 ml/min 2µL UV 254nm 50 3 PAH HPLC GC/MS 18 PAH TraceGOLD TG-5SiIMS 30m 0.25mm 0.25µm 26096-1420 90 1min 35 /min 280 4 /min 320 2min 18.43min He 1 ml/min 300 1µL 1min 30mL/min MS 18 100ppb PAH 1. (j) 2. (b) 3. (k) 1 3.94 2 4.82 3 4.94 4 5.31 5 6.00 6 6.03 7 6.88 8 7.07 9 (a) 8.33 10 8.38 11 (b) 10.02 12 (j) 10.02 13 (k) 10.06 14 (a) 10.53 15 (e) 10.63 16 (1,2,3-cd) 13.05 17 (a,h) 13.11 18 (g,h,i) 13.67 64

SPE-LC/MS 200mg 3mL HyperCarb ( 60106-301) 2g 15mL 10min 6000rmp 5min 3mL 1mL 1mL 3mL 1mL/min 500µL20% - 2 1. 1ppb LC/MS 2. 50ppb 121.8% LC/MS Hypercarb 5µm 2.1 100mm 35005-102130 A: +5mM B: /min %A %B 0 90 10 1 90 10 2 40 60 5 40 60 6 90 10 8 90 10 0.2mL/min 25 10µL MS HESI SRM 3700V 350 245.1 245.1 249.9 249.9 96.2 113.2 95.9 112.9 43 14 43 14 80 80 64 64 65

SPE-LC/MS 200mg 3mL HyperSep Retain-CX ( 60107-304) 2g 0.01g 50mL 2% / 20/80 20mL 20min 4000rpm 5min 40mL 2 50 1mL 2% 3mL 3mL 3mL 2% 3mL 3mL 5% LC/MS Hypersil Gold 5µm 2.1 150mm 25005-152130 A: 5mM B: 1. Time(min) A(%) B(%) 0 0.5 5 10 10.1 12 90 90 10 10 90 90 10 10 90 90 10 10 1. LOQ 0.1µg/kg 2. 75-110 % 10µL 250µL/min MS ESI SRM 4500V 350 66

SPE-LC/MS 200mg 3mL HyperSep Retain-CX ( 60107-303) 0.5g 0.1% 10mL 1min 1mL 2% 20min 8000rpm 10min 3mL 3mL 3mL 3mL 5min 5mL 5% / 1-2mL/min LC/MS Syncronis HILIC 5µm 2.1 100mm 97505-102130 A: B: 10mM / ph=3 85:15 10µL 250µL/min MS ESI MRM 3500V 350 LC/MS/MS 67

SPE-LC/MS 200mg 6mL HyperSep Retain PEP ( 60107-212) 4g 10mL 15min, 4000rpm 5min 10mL 4mL 4% 30:70 4mL 1min 4000rpm 3min 10mL 6mL 6mL 1-2mL/min 6mL 30% 6mL 1. 0.05µg/kg LC/MS Hypersil GOLD TM 50mm 2.1mm 1.9µm 25002-052130 A: B: min A% 0.0-0.6 5% 2.3 100% 2.35-3.0 5% 20µL 500µL/min MS ESI SRM 3000V 300 2.L00 L0Q 0.05µg/kg 3. 85%-90% 68

SPE-HPLC 200mg 3mL HyperSep Retain-CX ( 60107-303) 5g 10mL 10min 20mL / 3:2 2min, 6000rpm 5min 20mL / 3:2 4mL / 30:7 0.1 3mL 3mL 1-2mL/min 3mL 0.1mol/L 3mL 3mL 5% LC/MS Hypersil GOLD TM 150mm 4.6mm 5µm 25005-154630 / / = 30:70:0.5 v/v 20µL 1mL/min UV 220nm SPE-HPLC 200mg 6mL HyperSep Retain-CX ( 60107-314) 5g 25mL 5min 6000rpm 5min 25mL 50mL 10mL 50mL 6mL 6mL 1-2mL/min 6mL 5% 5mL 6mL 5% HPLC Hypersil GOLD TM 150 mm 4.6 mm 5µm 25005-154630 /0.05mo1/L =75/25 20µL 1mL/min UV 230nm 69

SPE-LC/MS 200mg 3mL HyperSep C18 ( 60108-303) 5g 30mL 10% ph 10 4g Nacl 40mL - 7:3 2min 10000rpm 5min 20mL - 7:3 5mL10% 3mL 3mL 1-2mL/min 3mL 2*2 ml HPLC Hypersil GOLD TM 150 4.6mm 5µm 25005-154630 A: 0.1% B +0.1% 35:65 20µL 1mL/min UV 235nm 25 1. HPLC 2. 75%-84% 70

SPE-LC/MS 200mg 6mL HyperSep Retain-PEP ( 60107-212) 5g 50mL 20mL 2 3000r/min 10 40 0.5mL 4mL 6mL 6mL 6mL 5min 6mL 6mL 1-2mL/min LC/MS Hypersil Gold 5µm 2.1 150mm 25005-152130 A: B: 0.1% 2mM 1. (min) 0 1 7 9 12 12.1 12.3 14.8 15 A 10 10 35 70 70 10 10 10 10 B 90 90 65 30 30 90 90 90 90 (µl/min) 250 250 250 250 250 250 300 300 250 10µL 250µL/min MS SRM ESI 4500V 350 1. 5 2µg/kg 2. 78%-89% 71

SPE-GC/MS QueChERS ( 60105-210 60105-204) 20g 20mL Thermo QueChERS extraction 1min 2min 1mL 1mL Thermo QueChERS clean-up 0.5min 2min GC/MS TG-5MS 30M 0.25mm 0.25µm 26098-1420 100 0.5min7 /min 300 1 min He 1.2 ml/min 20µL 10 1,290 MS GC/MS 1.naphthalene-d8 2dichlorvos 3.acenaphthene-d10 4.methacrifos 5. -BHC 6.hexachlorohenxene 7. -BHC(lindane) 8. -BHC 9.phenanthrene-d10 10.diaxinon 11.etrimphos 12.phosphamindon 13.chlorpyrifos-methyl 14.heptachlor 15.fenitrothion 16.pifimphos methyl 17.malathion 18.aldrin 19.chlorpyrifas 20.heptachlor epaxide 21.oxychlordane 22.trans-chlordane 23.endosulfan 24.cis-chlordane 25.2.41-DDT 26.dieldrin 27.endrin 28.endosulfan 29.4,4'DDE 30.4,4'DDD 31.endosulfan sulfate 32.4,4-DDT 33.chrysene-d12 34.perylene-d12 72

SPE-LC/MS QueChERS ( 60105-210 60105-204) 15g 30mL ACN Thermo QueChERS extraction 1min 2min 1mL 1mL Thermo QueChERS clean-up 0.5min 2min LC/MS Hypersil Gold 2.1 150mm 5µm 25005-152130 A: B: 0.1% 30%A-100%A-100%A 0-8-13.5min 20µL 300µL/min MS ESI SRM 4500V 550 SPE-LC/MS QueChERS ( 60105-211 60105-214) 15g 30mL ACN 30s 2min Thermo QueChERS extraction 1min 2min 5mL 5mL Thermo QueChERS clean-up 0.5min 2min HPLC HPLC Acclaim Carbamate 3µm 3.0 150mm 072926 A: B: -4.0-0.0min 14% 2.0min 20% 8.0min 40% 13.6-16min 70% 50 10µL 0.9mL/min 330nm 465nm : 1.Aldicarb sulfoxide 2.Aldicarb sulfone 3. Oxamyl 4. Methomyl 5. 3-Hydroxy carbofuran 6.Aldicarb 7.Propoxur 8.Carbofuran 9.Carbaryl 10.1-Naphthol 11.Methiocarb 12.BDMC(I.S.) 73

SPE-GC/MS 500mg 6mL HyperSep Florisil ( 60108-500) 10g 5g 30mL 2min 6000rpm 5min 30mL 6mL / 1:1 5mL / 1:1 10mL / 1:1 1mL GC/MS HPLC TG-5MS 30m 0.25mm 0.25µm 26098-1420 40 1.5min 25 /min 150 8min 7 /min 225 25 /min 290 10min 1.0mL/min 2.0µL 290 MS MS 250 70eV SPE-HPLC 200mg 3mL HyperSep Retain-CX ( 60107-304) 5g 5mL 0.1mol/L NaOH ph 10-11 20mL 1min, 6000rpm 5min 20mL 10mL 0.1 mol/l HCL 3mL 3mL 1-2mL/min 3mL 2% 0.1 mol/l HCL 3mL 3mL 5% HPLC Hypersil GOLD TM 150mm 4.6mm 5µm 25005-154630 /20mmol ph=3 =25/75 20µL 1mL/min UV 288nm 30 74

SPE-HPLC 500mg 3mL HyperSep Florisil ( 60108-405) 10g 5g 20mL 5min 10000rpm 5min 10mL / 10:90 3mL 1-2mL/min 6mL / 10:90 10mL / 20:80 HPLC Hypersil GOLD TM 150mm 4.6mm 5µm 25005-154630 / =25/75 20µL 1mL/min UV 260nm 40 QueChERS ( 60105-216 60105-218 60105-221) 15g 80 15mL ACN / 30 3450 2 1 6mL 1mL 60105-221 6mL 60105-218 1 3450 2 GC/MS 2 TPP 1mL 50 0.3 0.6mL 1mL 8µL GC/MS LC/MS 2 0.25mL LC TPP 0.86mL 6.7mM LC/MS 75

SPE-GC/MS QueChERS ( 60105-210 60105-206 60105-203) 15g 15mL 1% Therma QueChERSextraction 2min 3000rpm 5min, 11mL 11mL Thermo QueChERS initial clean-up 2min 3000rpm 5min 5mL 40 1 1mL / 9:1 1mL Thermo QueChERS final clean-up 2min 3000rpm 5min 1.GC/MS GC/MS Thermo Scientific TraceGOLD TG-5MS 30m 0.25mm 0.25µm 26098-1420 40 1.5min25 /min 150 7 /min 22525 /min 290 10min He 1mL/min 2µL 290 MS Figure 2: TIC for the GC/MS analysis of grapes spiked with 1ng/µL of each pesticide 2. 9 76 110% RSD n=3 21 Pesticide (peak number, name) Rt (min) Linearity (R 2 ) Average%recovery(n=3) Recovery%RSD 1. Chlorpyrifos methyl 14.92 0.9961 76 14.5 2. Metalaxyl 15.40 0.9908 100 7.9 3. Malathion 15.94 0.9989 103 19.0 4. Chlorpyrifos 16.12 0.9919 77 21.5 5. Penconazole 17.23 0.9978 94 7.2 6. Procymidon 17.45 0.9968 106 4.0 7. Dicofol 20.21 0.9964 110 9.9 8. Permethrin Isomer a 21.42 0.9980 102 3.9 9. Permethrin Isomer b 21.55 0.9965 Table 1: Summary of results 76

SPE-GC/MS QueChERS ( 60105-210 60105-206 60105-203) 15g 15mL 1% Thermo QueChERSextraction 5min 3000rpm 5min 11mL 11mL Thermo QueChERS initial clean-up 2min 3000rpm 5min 5mL 40 1 1mL / 9:1 1mL Thermo QueChERS final clean-up 5min 3000rpm 5min 1.GC/MS GC/MS Thermo Scientific TraceGOLD TG-35MS 30m 0.25mm ID 0.25µm 26094-1420 40 1.5min25 /min 150 5 /min 225 7.5min25 /min 290 12min He 1mL/min 2µL 290 MS Figure 3 Total ion chromatogram of full scan data for 50ng/g of pesticidesin onion matrix Figure 4 Total ion chromatogram of the MS/MS analysis of 50ng/g pesticides in onion matrix 77

2.LOD LOQ 45 LOQ 5-78ng/g Japan 1 US-EPA 2 EU 3 EU 3 WHO 4 Component Ave.Conc. (ng/g) Std.Dev. % Recovery %RSD LOD (ng/g) LOQ (ng/g) MRL (ng/g) MRL (ng/g) MRL (ng/g) LOD 3 MRL (ng/g) Dichlorvos 63 3.00 126 5 8 30 100 100 EPTC 22 1.95 86 9 6 20 40 Mevinphos 48 3.84 96 8 11 38 100 100 Etridazole 34 2.46 135 7 7 25 100 Molinate 6 0.62 123 10 2 6 20 Trifluralin 31 1.55 126 5 4 16 50 Cyanophos(Thionazin) 27 3.16 108 12 9 32 50 Ethoprophos 28 1.90 111 7 5 19 20 Di-allate 31 2.47 125 8 7 25 50 50 50 Propazine 66 6.47 132 10 18 65 100 Atrazine 12 1.56 116 13 5 16 20 100 100 Diazanon 15 0.88 149 6 3 9 50 750 50 Gamma-BHC (Lindane) 12 1.40 121 12 4 14 2000 1000 10 10 Disulfoton 15 1.81 152 12 6 18 50 20 20 Heptachlor 5 1.21 92 26 4 12 30 10 10 Vinclozolin 13 1.03 130 8 3 10 1000 1000 1000 50 1000 Prometryn 60 7.45 120 12 21 74 50 Metalaxyl 22 3.04 88 14 9 30 2000 3000 500 50 2000 Metribuzin 30 2.54 120 8 7 25 500 Triadimefon 28 2.24 111 8 6 22 500 500 100 Thiobencarb 30 3.00 120 10 8 30 200 Dursban (Chlorpyrifos) 15 2.07 102 13 7 21 50 300 200 50 200 Sevin (Carbaryl) 23 2.45 92 11 7 25 3000 100 Malathion 29 4.41 114 15 12 44 8000 8000 3000 1000 Methiocarb 26 2.63 103 10 7 26 50 500 Parathion 31 2.45 124 8 7 24 300 50 50 Heptachlor-2,3-exo-epoxide 4 1.08 79 27 3 11 30 Cyprodinil 32 4.17 128 13 12 42 50 600 300 Cyanazine 27 3.40 108 13 10 34 50 trans-chlordane 3 0.84 54 31 3 8 20 Terbufos Sulfone 14 2.20 138 16 7 22 50 cis-chlordane 5 0.55 99 11 2 5 20 Endosulfan A 26 3.24 103 13 9 32 200 Tetrachlorvinphos (Stirofos) 34 2.26 136 7 6 23 300 p,p-dde 29 2.74 116 9 8 27 500 Thiabendazole 28 3.54 111 13 10 35 2000 Dieldrin 28 2.58 114 9 7 26 50 Chlorobenzilate 14 1.20 138 9 4 12 20 20 20 Endrin 5 0.96 104 18 3 10 10 10 10 Endosulfan B 31 2.37 125 8 7 24 200 50 50 p,p-ddt 40 2.09 159 5 6 21 500 Endosulfan Sulfate 40 7.77 79 20 22 78 200 Bifenthrin 33 3.15 134 9 9 32 50 50 50 Methoxychlor 7 2.12 135 31 7 21 10 10 10 cis-permethrin 60 5.32 120 9 15 53 3000* 100* 50* 50* trans-permethrin 13 3.091 133 23 10 31 Average 116 12 8 27 78

3. 45 87 125% Component Avg Conc Theo Conc %Recovery %Difference %RSD Dichlorvos 241 200 107 7.12 16.64 EPTC 112 100 112 12.33 24.48 Mevinphos 193 200 96-3.54 19.36 Etridazole 112 100 112 11.94 17.12 Molinate 120 100 120 20.00 19.34 Trifluralin 80 100 80-19.51 19.09 Cyanophos(Thionazin) 101 100 101 1.36 21.82 Ethoprophos 114 100 114 13.87 20.90 Di-allate 111 100 111 10.67 21.27 Propazine 229 200 114 14.50 20.42 Atrazine 257 200 128 28.36 24.38 Diazanon 228 200 114 14.10 22.53 Gamma-BHC (Lindane) 223 200 111 11.39 20.86 Disulfoton 247 200 123 23.47 22.14 Heptachlor 124 100 124 24.06 22.85 Vinclozolin 233 200 116 16.31 22.60 Prometryn 193 200 96-3.74 20.98 Metalaxyl 77 100 77-23.22 25.68 Metribuzin 99 100 99-1.21 22.83 Triadimefon 86 100 86-13.68 23.48 Dursban (Chlorpyrifos) 364 300 121 21.17 22.38 Thiobencard 110 100 110 9.75 21.79 Sevin (Carbaryl) 98 100 98-2.21 24.95 Malathion 117 100 117 17.00 25.17 Methiocarb 90 100 90-10.14 23.42 Parathion 87 100 87-12.96 22.42 Heptachlor-2,3-exo-epoxide 125 100 125 25.23 24.25 Cyprodinil 108 100 108 7.56 26.09 Cyanazine 94 100 94-5.90 22.36 trans-chlordane 104 100 104 3.98 17.04 Terbufos Sulfone 209 200 105 4.67 25.76 cis-chlordane 109 100 109 8.94 23.67 Endosulfan A 106 100 106 5.61 23.16 Tetrachlorvinphos (Stirofos) 107 100 107 7.03 23.07 p,p-dde 102 100 102 2.00 21.46 Thiabendazole 99 100 99-0.62 24.37 Dieldrin 102 100 102 2.27 22.48 Chlorobenzilate 160 200 80-19.79 27.40 Endrin 93 100 93-7.26 25.35 Endosulfan B 94 100 94-5.52 23.00 p,p-ddt 97 100 97-2.74 20.85 Endosulfan Sulfate 203 200 102 1.57 28.03 Bifenthrin 105 100 105 4.57 22.49 Methoxychlor 100 100 100 0.34 24.71 cis-permethrin 189 200 95-5.34 20.97 trans-permethrin 197 200 99-1.32 19.13 Average 104 22 79

SPE-GC/MS QueChERS ( 60105-212 60105-203) 10g 10mL 10mL Thermo QueChERSextraction 1min 3000rpm 5min 2mL 2mL Thermo QueChERS clean-up 1min 3000rpm 5min 1mL GC 10µL 5% 1µL 1g/mL 95 80 110% GC/MS Thermo ScientificTR-Pesticide 30m 0.25mm ID 0.25µm 26RF142F 60 1min15 /min 160 1min 2.2 /min 230 1 min5 /min 290 5min He 1mL/min 2µL 280 MS Pesticide 0.01mg/kg mean CV 0.05mg/kg mean CV Pesticide 0.01mg/kg mean CV 0.05mg/kg mean CV Pesticide 0.01mg/kg mean CV 0.05mg/kg mean CV aldrin 89 11 94 3 ethofumesate 95 50 107 4 pirimiphos-ethyl 97 2 106 benalaxyl 101 6 108 3 ethoprophos 102 9 108 4 pirimiphos-methyl 95 7 104 bromopbos-ethyl 93 10 101 4 etrimfos 94 4 106 4 procymidone 93 9 105 bromopropylate 93 6 104 5 famoxadone 92 8 100 6 propachlor 92 11 107 bupirimate 97 9 110 3 fenarimol 95 7 105 3 propargite 98 11 107 buprofezin 97 9 110 3 fenazaquin 95 13 98 5 propham 95 5 104 cadusafos 97 6 105 4 fenitrothion 93 8 106 7 prothiofos 80 7 102 carbofuran 95 7 107 5 fenpropathrin 95 13 107 4 pyrazophos 97 7 106 chlordane-cis 90 13 104 1 fenvalerate 97 6 103 3 pyridaben 100 6 104 chlordane-trans 94 5 101 2 fludioxonil 103 7 104 5 pyridaphenthion 97 8 107 chlorobenzilate 103 7 108 2 flusilazole 93 11 111 6 pyrifenox 97 6 107 chlorothalonil 63 11 84 5 folpet 93 9 97 8 quinalphos 102 9 102 chlorpyrifos 91 8 102 1 fonofos 94 8 103 3 quintozene 86 9 94 chlorpyrifos-methyl 95 4 103 3 formothion 93 7 105 3 simazine 91 7 105 chlorthal-dimethyl 87 9 102 3 furalaxyl 96 6 108 5 tecnazene 81 5 95 chlozolinate 98 15 107 5 HCB 72 10 86 4 tefluthrin 90 8 103 DDD-pp 94 6 103 3 HCH-gamma 94 5 103 3 tetrachlorvinphos 99 3 110 DDE-pp 85 6 97 3 hexaconazole 99 13 105 8 tetradifon 97 6 107 DDT-op 92 7 101 3 iprodione 101 6 110 3 tetramethrin 97 8 106 DDT-pp 94 5 102 2 isocarbofos 97 9 111 7 tolclofos-methyl 95 8 101 deltametbrin 93 18 104 5 isofenphos 99 5 107 2 tolylfluanid 98 8 100 diazinon 97 7 107 5 isofenphos-methyl 100 8 105 3 trifluralin 97 8 104 dichlofluanid 80 9 94 6 methacrifos 93 7 107 3 vinclozolin 92 5 104 dichlorvos 95 9 105 3 methidathion 100 8 104 3 dicloran 92 5 105 5 methoxychlor 94 10 103 2 0.02mg/kg 0.01mg/kg dicrotophos 89 9 103 3 nitrothai-isopropyl 101 9 103 5 captan 108 8 96 9 dieldrin 89 7 100 3 oxychlordane 99 21 99 6 cyfluthrin 110 5 105 4 diflufenican 101 7 109 1 parathion-ethyl 98 6 102 3 0.05mg/kg 0.25mg/kg endosulfan- 94 14 101 3 pendimethalin 97 9 103 4 chlorpropham 98 7 108 5 endosulfan- 94 14 105 6 parathion-methyl 100 8 105 5 bitertanol 98 7 103 4 endosulfan-sulfate 102 8 109 3 permethrin 90 7 99 3 cypermethrin 103 6 102 3 EPN 95 9 105 3 phosalone 103 7 105 3 dicofol 108 10 94 10 ethion 103 9 105 3 phosmet 102 6 105 6 diphenylamine 94 6 99 4 80

SPE-GC/MS QueChERS ( 60105-212 60105-227) 10g 30mL ACN Thermo QueChERS extraction 1min 2min 5mL 5mL Thermo QueChERS clean-up 0.5min 2min GC/MS TraceGOLD TG-5MS 30m 0.25mm 0.25µm 26098-1420 501min20 /min 2805min He 1.5mL/min 1µL 280 MS GC/MS 81

SPE-GC/MS 500mg 6mL Carb/PSA ( 60105-209) 25.0g 50.0mL 2min 5g-7g 100mL 40mL-50mL 1min 10.00mL 80 1.0mL 5.0mL + 3+1 1mL 50mL 25mL + 3+1 4-5 Carb/PSA 55 0.5mL 5.0mL 0.5mL 5.0mL GC/MS TraceGOLD TG-5MS 30m 0.25mm 0.25µm 26098-1420 501min20 /min 2805min He 1.5mL/min 1µL 280 MS GC/MS 1. 82

3. 5(a) (b) SIM (c) SRM 83

SPE-HPLC 500mg 3mL HyperSep C18 ( 60108-304) 1g +0.5mL ph4 10mL 3mL10% 10mL 2-3mL/min 5mL 15min : : =1:5:4 1:4:5 1:3:6 5mL 1 40 1mL 1. Rt=7.4min HPLC HPLC Hypersil Gold C18 5µm 4.6 250mm 25005-254630 A : B =1:10 v/v 1mL/min UV@276nm 40 5µL 2. 94-101% SPE-LC/MS 60mg 3mL HyperSep Retain-AX ( 60107-403) 10mL 1mL 5mL NaOH ph 11 3mL 3mL 0.1M NaOH 3mL 3mL70% 5% 3mL 1mL 3mL 89:9:2 / / 1. I-IV LC/MS 2. 73%-90% (3) (4) (5) (6) IV GC/MS Hypersil GOLD 1.9µm 20 4.6mm 25002-024630 0.1% / +0.1% 12/88 0.5mL/min 5µL 200µL/min MS ESI SRM 2500V 350 84

QueChERS ( 60105-211 60105-220) ACN 2,000 5,000µg/mL -18 ACN MIX-1 MIX-2 10µg/mL 0.1% ACN 5µg/mL -d5-13c6 o,o - -d6 2.4-DDT -13C6 -HCH 13C6 -d10 QC -13C6 1 5µg/mL * 50mL 60105-211 10mL 15mL 10mL ACN 200µL ISTD / 1 3.000 10 1mL 2mL 60105-220 / 30 5 300µL 30µL 1µg/mL QC 125µL 250 Mini-UniPrep 0.2µm PVDF LC/MS/MS 30µL QC LC GC/MS GC/MS GC/MS * 2.5g 3.5g 5.0g 5.0g A B QueChERS ( 60105-211 60105-219) 5g 50mL 10mL ACN 85:15 50mL 60105-211 4g 1g / 1 4,000rpm 10 1mL 2mL 60105-219 150mg 50mg PSA 1 4,000rpm 10 0.45µm LC API 0.5mL/min %ACN% 0.1% 0 60 40 10 10 90 25 10 90 [Na+M] m/z NIV 355 DON 319 DAS 389 HT2 447 T2 489 HPLC Betasil C18 250mm 4.6mm 5µm 70105-254630 85

SPE-GC/MS 1mg 6mL HyperSep Florisil SPE ( 60108-431) SPE 15mL 10mL 15mL 40mL 4min 20mL 20mL 2 1mL GC/MS TraceGOLD TG-WaxMS 30m 0.25mm 0.2µm 26088-1420 50 1min 5 /min 160 25 /min 220 10min 1.0mL/min 10µL 250 MS 200 70eV B1 B2 G1 G2 SPE-HPLC Vicam Aflatest WB 25g 5g 100mL : 80:2 1 10mL 1 40mL 2 10mL SPE 10mL 10mL 10mL 2-4mL/min 10mL 10mL 10mL HPLC HPLC Hypercarb TM 5µm 100 3.0 mm 35005-103030 Dioxane/ 1:9 0.8mL/min ex=365nmem=418nm 25 5µL G2 G1 B2 B1 86

QueChERS ( 60105-205 60105-211) 87 20mL ACN 250µL 60105-211 20.0mL 2 4,500rpm 5 9.0mL 60105-205 / 10 3.0mL 1 4,500rpm 5 2.0mL 40 500µLACN 25µL 2.0µg/LQC 500µL 1 %ACN 20mM / 5 17mm 0.2µm F2513-2 3µL LC/MS MRM 184.0/143.0 223.4/126.1 S- 211.1/136.0 208.1/116.0 240.0/222.9 224.2/206.9 215.9/173.85 B1b 876.6/553.4 B1a 890.7/567.5 404.0/372.1 326.1/148.1 411.2/190.0 198.1/105.1 301.3/170.2 338.2/99.1 306.3/201.2 202.1/145.1 192.0/160.0 222.1/123.1 291.0/72.2 226.1 /93.0 167.2/85.1 328.1/70.2 230.1/199.0 388.0/301.1 327.1/206 203.5/14.0 233.0/72.1 MRM 286.9/258.9 373.2/282 312.2/236.2 337.1/125.0 301.9/261.9 304.4/147.1 307.2/220 247.0/180.0 383.2/195.1 314.0/70.2 297.1/159.0 256.1/175.0 334.1/70.2 321.2/119.0 314.1/116.0 224.4/77.3 280.1/220.1 142.0/94.0 163.0/88.0 369.5/149.0 225.1/192.8 289.1/70.2 214.1/183.0 279.1 /219.1 356.2/177.0 376.1/308.0 189.1/102.1 368.1/231.0 342.0/159.0 210.0/111.0 388.0/194.0 365.3/309.1 200.1/107.0 307.8/196.8 395.3/213.2 202.2/131.4 A 732.6/142.2 D 746.6/142.2 298.2/144.0 308.2/70.2 202.0/175.0 294.0/197.1 409.0/186.0 346.0/278.1 288.1/146.0 336.0/187.0 HPLC Hypersil GOLD 3µm 150 2.1mm 25003-152130

SPE-GC/MS 10mg 1mL SOLA HRP ( 60109-001) 1mL 1mL 200µL 200µL 200µL 200µL IS ( ) 1. 20ng/mL GC/MS 2. 20ng/mL 99.3% RSD = 2.7% n=6 Extraction Calculated Conc ng/ml Recovery% %Errorr 1 19.6 97.9-2.1 2 19.8 99.0-1.0 3 19.4 96.8-3.2 4 19.4 96.8-3.2 5 20.6 103.2 3.2 6 20.3 101.7 1.7 Average 19.9 99.3-0.7 Std Dev 0.53 2.67 - %BSD 2.7 2.7-3. 1ng/mL-1000ng/mL R2=0.9987 GC/MS TG-WAXMS A 30m 0.25mm 0.25µm 26087-1420 80 20 /min 250 6.5min 1.2mL/min 1µL 250 1min 50mL/min MS 250 250 70eV Compound Abbrev SIM(start time/min) Vanillin - 4.0 Benzyl benzoate (Internal standard) ISTD 4.0 Quan ion (Qual Ion) 152 (151) 212 (105,91) Calculated Conc Extraction ng/ml 1 25.6 2 26.7 3 26.0 4 26.0 5 25.7 6 23.3 Average 25.6 Std Dev 1.18 %BSD 4.6 Dwell time/s 0.1 0.1 4. 25.6ng/mL RSD=4.6% 88

SPE-GC/MS 20mg 60mL HyperSep SLE ( 60109-20000-60-7) 5 5mm 1.0g 50mL 20mL 20 min 16mL 70 5 0.06mol/L ph6.0 70 2 30min 3mL 200mg/ ml 70 2 10min 1.5mL 70 2 30min 15min 20mL 4 SLE 1mL/min 35 1mL 2mL 1.GC/MS GC/MS TRACE TG-5MS 30m 0.25mm 0.25µm 26098-1520 50 0.5min 20 /min 150 8min 20 /min 230 13min 20 /min 280 1min He 1mL/min 1µL 10:1 MS 1 23 7.5µg/L 1) 2) 2,4-3) 2, 6 4) 4) 5) 3-6) 2,4,5-7) 4-8) 2,4-9) 2,4-10) 2-11) 2- -4-12) 4-13) 4,4'- 14) 15) 4,4'- 16) 17) 4,4'- 18) 18 ) 3,3'- -4,4' - 19) 3,3-20) 4,4'- 21) 3,3'- 22) 4,4'- - -(2- ) 23) 3,3'- 2. 2,4-58% 2,4-2,6-66% 63.8% 75% 78%-113% 89

AMPA SPE-LC/MS 500mg 6mL HyperSep Hypercard ( 60106-402) 6mL 6mL ph=3 5min 20mL HPLC-MS/MS LC/MS Hypercarb 5µm 4.6 100mm 35005-104630 A 0.2% - B A:B=95:5 5µL 500µL/min MS ESI SRM 3500V 450 1. HPLC-MS-MS 1g 6mL HyperSep Verify-CX ( 60108-732) ph 6.0 1L HyperSep Verify-AX 1 5mL 1 10mL 1 3mL/min 1 10mL 10 10 1 4mL 1mol/L HCI/ 4/1 1mL/min 50 50µL MTBSTFA* 50µL 2 80 30 GC/MS * TS-48920 GC TraceGOLD TG-17MS 30m 0.25m 0.25µm 26089-1420 90

SPE-HPLC 500mg 6mL HyperSep Retain PEP ( 60107-206) 500mL 1% 6mL 6mL 1% 500mL 6mL1% 6mL HPLC HPLC Hypersil GOLD 5µm 150 2.1mm 25005-152130 A: +0.1% B: + 0.1% 5%B 1.5 mins 19.5 mins 95%B 1.5 mins 0.6mL/min 10µL UV 270-320nm 60 (1) (2) 4- (3) 2,4- (4) 2- (5) 4- (6) 4- (7) 2- (8)2,4- (9) 2,4- (10) 2,4,6- (11) SPE-HPLC 500mg 6mL HyperSep Retain PEP ( 60107-206) 500mL 150g ph 6 3mL 3mL 500mL 1-2mL/min 5mL 5mL HPLC HPLC Acclaim Explosives E1 and E2 4.6 250mm 5µm 064305, 064309 / 5µL 1mL/min 254nm 91 1.HMX 2. RDX 3. 1,3,5-Trinitrobenzene 4.1,3-Dinitrobenzene 5. Nitrobenzene 6. Tetryl 7. 2,4,6-Trinitrotoluene 8. 4-Amino-2,6-Dinitrotoluene 9. 2-Amino-4,6-Dinitrotoluene 10.2,6-Dinitrotoluene 11.2.4-Dinitrotoluene 12.2-Nitrotoluene 13.4-Nitrotoluene 14.3-Nitrotoluene

SPE-HPLC 500mg 6mL HyperSep Retain PEP ( 60107-206) 500mL + 5mL:5mL 500mL 1-2mL/min 10mL1:1 - HPLC (1) PCB-118 (2) PCB-80 (3) PCB127 (4) PCB-77 HPLC Hypercarb 7µm 50 4.6mm 35007-054630 A: 30% /70% 10µL 1mL/min 254nm SPE-HPLC 500mg 6mL HyperSep Retain PEP ( 60107-206) 500mL 6mL 6mL 1% 500mL 6mL 6mL HPLC (1) (2) (3) (4) (5) (6) (7) (8) (9) (a) (10) (11) (b) (12) (k) (13) (a) (14) (a,h) (15) (ghi) (16) (1,2,3-cd) HPLC Hypersil Green PAH 3µm 100 4.6mm 31103-104630 A: 99:1 : B:99:1 : 50:50-5min 50:50-25min 0:100 2mL/min 10µL UV 254nm 20 92

60mg 3mL HyperSep Retain PEP ( 60107-203) w/w 20% 10mL10ppm Retain PEP 2mL 2mL 1 2mL/min 4mL 1mL 5mL 0.5mL ACN/ 40:60 v/v 1mL/min 300C 214nm HPLC Hypersil GOLD 5µm 250 4.6mm 25005-254630 N,N- 60mg 3mL HyperSep Retain PEP ( 60107-203) 200 20 2ppm N,N- Retain PEP 3mL 3mL 1 2mL/min 3mL 1mL N,N- 3mL / 95:5 v/v 1mL / 50:50 v/v HPLC Hypersil GOLD aq 5µm 250 4.6mm 25305-254630 (ppm) (av) (av) Retain PEP (%)Retain PEP a 200 360251 213975 60 b 20 28374.536686 20672 56 c 2 3563 28701 81 N,N (ppm) (av) (av) Retain PEP (%)Retain PEP a 200 1418380 1398427 98 b 20 174334 159897 92 c 2 19483 18386 94 93

60mg 3mL HyperSep Retain PEP ( 60107-203) 10ppm 10mL 20µL Retain PEP 2mL 2mL 1 2mL/min 4mL 1mL 5mL 0.5mL ACN/0.2% 10:90 v/v 1mL/min 30 : 214nm HPLC Hypersil GOLD 5µm 250 4.6mm 25005-254630 500mg 6mL HyperSep Retain PEP ( 60107-206) 0.5 M H 2 SO 4 500mL ph 3 Retain PEP 3mL 5mL 5mL 5mL/min 500mL 5mL 20 10 / 0.8mL PEP SPE 2 3mL 3mL 10mg 6mL HyperSep C18 ( 60108-301) 1L ph 1 C18 10mL / 50:50 10mL 5% HCI 10mL 8 10mL/min 1 HCI 10mL ph 1.0 15 30 10mL / 50:50 / 500µL DMF 500µL / 100µL TCTEF 1 2µL GC 2,4-D 2,4,5 Silvex 94

500mg 6mL HyperSep Retain PEP ( 60107-206) 500mL H 2 SO 4 ph 2 HyperSep Retain PEP 1 5mL 1 5mL 1 500mL 5mL/min 1 5mL 1 1mL 1 3mL THF 3mL HPLC HPLC Hypersil GOLD PFP 3µm 150 4.6mm 25403-154630 2,4-500mg 6mL HyperSep Retain PEP ( 60107-206) H 2 SO 4 ph 2 HyperSep Retain PEP 1 5mL 1 5mL 1 500mL 5mL/min 1 5mL 1 1mL 20 1 3mL THF 3mL HPLC HPLC Hypersil GOLD PFP 3µm 150 4.6mm 25403-154630 2,4-500mg 6mL HyperSep Retain PEP ( 60107-206) 0.5 M H 2 SO 4 500mL ph 1.5-2 Retain PEP 3mL 5mL 5mL 5mL/min 500mL 5mL 20 10 / 2,4-0.8mL PEP SPE 2 3mL THF 3mL 95

500mg 6mL HyperSep Retain PEP ( 60107-206) 497.5mL ph 2.5mL Retain PEP 3mL 5mL 5mL 5mL/min 500mL 5mL 20 10 / 0.8mL PEP SPE 2 Retain PEP 5g 3mL 3mL 3mL 10mL / 90:10 40 1mL HPLC HPLC Hypersil GOLD 3µm 150 4.6mm 25003-154630 1g 6mL HyperSep C18 ( 60108-301) C18 10mL / 50:50 10mL 10mL 8 10mL/min 1 20mL 15 30 10mL / 50:50 / 500µL DMF 500µL - 4,4'-DDE - 4,4'-DDD - 4.4'-DDT 1 60mg 3mL HyperSep Retain PEP ( 60107-203) 1 10% 2ppm 2 1% 0.2ppm Retain PEP 2mL 2mL 1 2mL/min 10mL 1mL 4mL 1% 85:15 v/v 1mL :1% 85:15 v/v 1 ml/min 30 230nm HPLC Hypersil GOLD aq 5µm 150 4.6mm 25305-154630 96

60mg 3mL HyperSep Retain PEP ( 60107-203) HyperSep Retain PEP 1 3mL 10:90 v/v 1 3mL 1 3mL 20mL/min 1L 10 15 1 10mL 10 20 1 2mL 1 2mL 10:90 v/v 1mL HPLC HPLC Hypersil GOLD PFP 3µm 150 4.6mm 25403-154630 60mg 3mL HyperSep Retain PEP ( 60107-203) 10ppm 10mL / 95:5 v/v 20µL Retain PEP 2mL 2mL 1 2mL/min 4mL 1mL / 5/95 v/v 4mL ACN/ 40:60 v/v 1mL/min 30 214nm HPLC GC/MS 500mg 6mL HyperSep Retain PEP ( 60108-732) Hypersil GOLD PFP 5µm 250 4.6mm 25005-254630 1L 6N HCI ph 2 HyperSep Retain PEP 1 3mL CH 3 CI 1 3mL 1 3mL 0.05N HCI 20mL/min 1L 10 15 1 10mL 10 5 1 10mL CH 3 CI 1 3mL CH 3 CI 40 0.9mL CH 3 CI 1.0mL GC/MS GC TraceGOLD TG-5MS 30m 0.25m 0.25µm 26098-1420 97

SPE-HPLC LC/MS 500mg 6mL HyperSep Retain PEP ( 60107-206) 0.2% 3mL 3mL 500mL 1-2mL/min 5mL 5mL HPLC Hypersil GOLD C8 5µm 150 4.6mm 25205-154630 A: B: 0minsB=20% 15minsB=23% 25minsB=75% 10µL 1.5mL/min 240nm 1. HPLC LC/MS Hypersil GOLD 50mm x 2.1mm ID 3µm 25003-052130 / 0.1% 0minsB=20% 15minsB=23% 25minsB=75% 10µL 400 µl/min MS ESI SRM 4000V 300 (1) Simazine (2) Monuron (3) Chlorotoluron (4) Atrazine (5) Diuron (6) Propazine (7) Linuron 2. 90-102% 98

SPE-LC/MS 200mg 6mL HyperSep Retain PEP ( 60107-212) 500mL 6mL 6mL 5mL/min 5mL 4mL 2 1. 9 LC/MS/MS 2. 80% LC/MS Hypersil GOLD 50 2.1 mm 3µm 25003-052130 A: 5mM B: min A% B% 0.0 90 10 7.0 80 20 10.0 75 25 18.0 75 25 20.0 20 80 25.0 20 80 25.1 90 10 40.0 90 10 20µL 250µL/min MS ESI SRM 3500V 300 99

60mg 3mL HyperSep Retain PEP ( 60107-203) 1% 0.5 1ppm Retain PEP 2mL 2mL1% 1 2mL/min 10mL 1mL 1% 2mL 1% 1:1 1mL /1% 1:1 v/v HPLC Hypersil GOLD aq 5µm 250 4.6mm 25305-254630 n=3 1 2 3 1.472 0.000 1.367 1.541 1.524 1.477 0.096 100.3 4-nitro phenol 1.469 0.000 1.229 1.308 1.430 1.322 0.101 90.0 m- 1.374 0.000 1.294 1.540 1.548 1.461 0.144 106.3 2-0 0.613 0.000 0.527 0.684 0.641 0.617 0.081 100.6 2,4-1.630 0.000 1.305 1.613 1.621 1.513 0.180 90.392.8 2,4,6-1.655 0.000 1.365 1.609 1.511 1.495 0.123 95.690.3 1.470 0.000 1.259 1.487 1.472 1.406 0.128 95.6 2g 15mL HyperSep C18 ( 60108-701) 0.45µm 200mL 2mL 2 C18 15 20mL 15 20mL 10mL 8 10mL/min 200mL 20mL 20 30 20mL / / 100µL 1 2µL GC 1026 1221 1232 1242 1248 1254 1260 100

500mg 3mL HyperSep NH 2 ( 60108-518) 0.45µm 200mL 2mL 2 NH 2 20mL / (TCTFE) 15 20mLTCTFE 5 15 20mL 20mL 8 10mL/min 200mL 20mL 30 20mLTCTFE / / 100uL CTFE 1 2 GC (e) (b) (k) (a) (a,h) (g,hi) (a) (1,2,3-cd) (SPE-LC/MS) 200mg 6mL HyperSep Retain Ax ( 60107-412) 200mL 6mL 6ml 5mL/min 5mL 2% 5mL 5% LOQ 13 (LOQs) 0.5-5pg/ml LC/MS Thermo Scientific HypersiIGOLD 4.6 100 mm, 3pm 25003-104630 A: 0.5% +0.04% B: 0.5% +0.04% 20µL 200µL/min MS ( ESI) (SRM) 4000V 375 101

(SPE-LC/MS) 200mg 6mL HyperSep Retain PEP ( 60107-212) 50mL 200mL ph 4 6mL 6mL 5mL/min 5mL 4mL 2 1.5 LC/MS/MS LC/MS Hypersil GOLD 150 2.1 mm, 3pm 25003-152130 / 0.1 % FA OminsB=20%, 15mins =23%, 25minsB=75% 20µL 200µL/min MS (ESI) (SRM) 4000V 350 2 2 ng/l LC-ESI(+)-MS/MS SRM 2. LOQ:5 LOQ 11-55ng/L 3. : 72% 3.1% 19.0% 102

(SPE-LC/MS) 200mg 3mL HyperSep C18 ( 60108-303) 4 0.7µm 0.45µm 24 3mLMTBE, 3mL 3mL 1L 5mL/mi 3mL 10/90 MeOH/MT E3ML 3mL 1. LOQ: (LOQs) 0.03-2ng/L 2. : 72%~94% (%RSD) 3%~11% LC/MS Thermo Scientific HypersiIGOLD 50 2.1mm 3 µm 25003-052130 A 0.1% B : T=0, A=90%, B=10% T=1, A=90%, B=10% T=15, A=1%, B=99% T=16.5, A=1%, B=99% T=17, A=90%, B=10% T=22, A=90%, B=10% 20 µl 500 µl/min MS APCI+ 500 250 CID -10v 3 RSD (min ) LOD*(ng/L) R2** ***(%) RSD(%) 5.46 0.5 0.9998 91 7 5.79 0.07 0.9995 87 9 10.14 0.30 0.9981 84 9 10.76 0.09 0.9999 86 5 11.41 0.03 0.9995 86 3 12.62 2.00 0.9996 85 9 17- a 1 2.85 0.50 0.9931 73 10 12.88 0.10 0.9979 72 6 12.94 0.60 0.9989 79 9 14.44 0.08 0.9994 94 4 CC 15.10 0.20 0.9970 81 10 15.17 2.00 0.9991 84 6 8.82 0.90 0.9993 77 6 12.00 0.60 0.9989 83 11 *LOO( )Mille Iles River R2** 10-100ng/L *** 50ng/L, n=6 103

(SPE-LC/MS) 200mg 3mL HyperSep C18 HyperSep Retain-CX ( 60108-303, 60107-304) 1.2pm 45 µm 250mL ( 50mM) 1 ml5% Na2EDTA(w/v ) 1.0 M ph 3 3mL 3mL 1L 5mL/min HyperSepC18 3mL 2 2.5mL : (1:1), HyperSep Retain-CX, 2 2.5mL 5% : ( 1:1) 1. LOQ: 0.3-22 ng /L 2. : 54%-105% LC/MS ThermaScientific Hypersil GOLD 25003-052130 A (0.1% ) (min) A% B% 0 90 10 2 80 20 15 75 25 17 50 50 20 5 95 25 5 95 30 90 10 50 2.1mm, 3 µm 20pL 200pL/min MS (ESI) (SRM) 3500V 350 60mg 3mL HyperSep Retain PEP ( 60107-203) (ph 2.5) Retain PEP 5mL 5mL (ph 2.5) 1 2mL/min 10mL 3mL (ph 2.5) 5mL ACN/ (ph7.8)(9:1,v/v) 1mL :ACN- - (0.2% ) :1 ml/min :30 : (%) Retain PEP 91-89 - 89-86 99-81 15-82 - 93-107 HPLC Hypersil GOLD 5pm, 250 4.6mm 25005-254630 104

LC/MS/MS 10g 75mL HyperSep C18 ( 60108-703) 10 100 15 50% H 2 SO 4 ph Z HyperSep C18 1 5mL 1 5mL 10mL/min 2 5mL 1 2mL/min <40 100µL 10 100µL LC/MS : 0.1 M (A): (B) %B 25 0 60 15 +ve m z-ve m z 141 238 184 2.4-D 238 184 218 199 252 235 MCPP 232 213 2,4,5-T 272 218 2,4,5-TP Silvex 286 269 228 240 2,4-DB 266 247 2,4-D, 321 185 2,4-T, 372 195 2.4.5-T, 328 195 2.4-D, 350 161 GC ODS-Hypersil C18 5µm, 100 2mm 30105-102130 MDS2-Hypersil C18 3µm, 100 2mm 30303-102130 EPA 535 500mg 6mL HyperSep Hypercarb ( 60106-402) 250mL HyperSep Hypercarb 1 20mL / 1 30mL 1 3mL 10 15mL/min 1 5mL 1 15mL / 5mL/min 60 70 1mL5mM / LC/MS/MS MRM OA 206/134 OA 224/152 ESA 256/80 ESA 274/80 OA 270/198 ESA 320/80 OA 264/160 OA 264/146 ESA 314/80 OA 278/206 ESA 314/80 ESA 328/80 ESA (sur) 300/80 ESA (IS) 356/80 GC Hypersil GOLD 3µm, 150 2.1mm 25003-152130 105

EPA 8330B- - 500mg 6mL HyperSep Retain PEP ( 60107-206) 2.0g 25mL 2g 0.1mL ( / ) LCS, LCSD 0.5mL 10mLACN / 1 18 (<100C) 15 20 CaCI 2 (5.Og/L) 5mL 1gm 3mL 3mL 12mL 1mL 5.OmL 1 5mL ACN 1 15mL IPA 1 15mL CH 3 OH 1 5mL ACN 1 15mL ACN HyperSep Hypercarb 1 20mL ACN 1 20mL ACN 1 50mL 1 50mL 1 15mL ACN 1 30mL 10mL/min 1 4mL ACN 1 5mL ACN 40 0.7mL 0.7mL 100µL LC/MS : 0.50mL/min : 50:50 : GC Hypersil GOLD 5µm, 250 4.6mm 25005-254630 Hypersil GOLD C8 3µm, 150 4mm 25203-154030 Hypersil GOLD CN 5µm, 250 4.5mm 25805-254630 Betasil Phenyl Hexyl 5µm, 250 3mm 73005-253030 106

EPA 508 10g 75mL HyperSep C18 ( 60108-703) 1L MgCI 2 ( 10mg/L ) HyperSep C18 1 1 ml 1:1 EtAc/CH 3 Cl 2 1 10mL 1 10mL 1 5mL 50uL 1 2mL/min 1 10mL EtAc 1 10mL CH 3 Cl 2 40 0.8mL 1mL 1 2µL GC GC TraceGOLD TG-OCP I 30m 0.25m 0.25µm 26078-1420 1 3mL EtAc/CH 3 Cl 2 SPE HyperSep Aminopropyl, HyperSep Retain-AX, HyperSep SAX HyperSep Verify-AX HyperSep 1mL 1 3mL 1 3mL 1 3mL/mi 10 50mL 1 10mL ( >10 5 ) 100mM 1 3mL (100mM) 1 3mL/min 1 3mL 1 3mL/min 107

4' 4-100mg 1mL HyperSep C18 ( 60108-302) Verify-CX 3mL 3mL 1 ml/mi 1mL 4' 4 1M 0.25mL 10µL HPLC 100µg/mL :3.162 : / (50:50) :1.2mL/min :10µL : (254nm) GC Hypersil GOLD 5pm, 250 4.6mm 25005-254630 60mg 3mL HyperSep Retain PEP ( 60107-203) 100mL 10mg 100ppm 25mL (100ppm) 50mL ( 50ppm) 25mL (100ppm) 50mL 1%H 3 PO 4 ( 50% 1 %H 3 PO 4 ) Retain PEP 2mL 2mL 2mL 2mL / (5/95, v/v) (5 10 >10 / ) 2mL <50 1mL 60mg 3mL HyperSep Retain-CX ( 60107-303) 100mL 10mg 100ppm 25mL (100ppm) 50mL ( 50ppm) 25mL (100ppm) 50mL 1%H 3 PO 4 ( 50% 1 %H 3 PO 4 ) Retain PEP 2mL 2mL 2mL 2mL / (5/95, v/v) (5 10 >10 / ) 2mL <50 1mL 108

Hyclone 60mg 6mL Retain PEP CX ( 60107-203 60107-308) 100mL 10 - (100ppm) 25mL - 50mL 25mL - 50mL 1 2mL CH 3 OH 1 2mL H 2 O 2mL 2mL 1 2mL 5% CH 3 OH 1 2mL CH 3 OH SPE (1%) 1 2 HyperSep Retain PEP+50% 58.5 40.3 HyperSep Retain-CX+50% 94.6 94.6 HPLC 200mg 6mL HyperSep Verify-CX ( 60108-722) 1 ml 100mM (ph 6.0) * 1mL / ph 6.0 0.5 100mM ph HyperSep Verify-CX 1 3mL 1 3mL 1 1 ml 100mM (ph= 6.0) <3 1mL/min 1 2mL 1 2mL 20% 100mM (ph= 6.0) ( >10 10 ) 1 2mL 1 5mL 2% 1 2mL/min <40 HPLC * -D5 Alpha- - -D5 -D4 -D5 -D5 GC BETASIL Phenyl/Hexyl 5µm, 150 4.6mm 73005-154630 109

GC GC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) - 2mL 1mL - - 100mM (ph=5.0) 5.000 F /ml Patella Vulgata / 65 3 2,000rpm 10 HyperSep Verify-CX 1 3mL 1 3mL 1 1 ml 100mM (ph= 6.0) <3 1mL/min 1 2mL 1 2mL20% 100mM (ph 6.0) ( >10 5 ) 1 2mL 1 5mL 4% 1 2mL/min <40 50NL 50}L STFA** ( 1%TMCS}** / 70 20 BSTFA GC/MS 1-2µL *** -D5-TBDMS 332 334 333 -TBDMS 327 328 329 -D5-TBDMS 462 519 462 -TBDMS Serax Serax 457 513 459 -D5-TBDMS 362 390 288 -TBDMS Restoril 357 359 385 -TBDMS Ativan 491 513 493 Klonopin 372 374 326 7- -TBM 456 458 513 Valium 256 283 221 -TBDMS 345 347 402 * 269 241 324 - -TBDMS Versed 398 400 440 -TBDMS 357 310 356 7- -TBDMS 397 324 398 Xanax 308 279 204 - -D5-TBDMS 386 388 387 - -TBDMS 383 384 381 Halcion 313 314 342 - -TMS 415 417 190 * GC/MS -D5 ** TS-38831 *** GC TraceGOLD TG-5MS 30m 0.25m 0.25µm 26098-1420 110

: GC-GC/MS 200mg 6mL HyperSep Verify-CX ( 60108-722) 1 ml 100mM (ph= 6) * 1mL / 1g}1:4) / 3mL 100mM (ph=6) ph 6.0 0.5 100mM ph / 1mL 5000 F /m L b- (ph=5.0) * 1mL / 65 3 2,000rpm 10 3mL 100mM (ph 6.0) HyperSep Verify-CX 1 3mL 1 3mL100m M (ph 6) <3 1 2mL/min 1 3mL 5% p/v) 100mM (ph6) ( >10 5 ) 1 3mL ( >10 5 ) 1 3mL (98:2 v/v) 1 2mL/min <40 500L 50µL STFA( 1 % TMCS**) 70 30 1 GC/MS 308 279 204 -D* 513 284 Alpha- - 318 396 383 Alpha- - -D5* 386 401 256 283 284 -D5* 287 289 429 430 347 -D4* 433 435 34 342 343 -D5* 345 347 429 313 430 -D5* 435 433 343 257 283 -D5* 348 262 * -D Alpha- - -D5 -D4 -D5 -D5 -D5 ** TS-38831 GC TraceGOLD TG-5MS 30m 0.25m 0.25µm 26098-1420 111

: LC/MS/MS 200mg 6mL HyperSep Verify-CX ( 60108-722) 1mL100m M (ph=6) * 1mL / 1g(1:4) / 3mL 100mM (ph=6) ph 6.0 0.5 100mM ph / 1mL 5000 F /ml b- (ph=5.0) 1mL / 650C 3 2,000rpm 10 3mL 100mM (ph 6.0) HyperSep Verify-CX 1 3mL 1 3mL 100mM (ph=6) <3 1 2mL/min 1 3mL 5% w/v) 100mM (ph6) ( >10 5 ) 1 3mL ( >10 5 ) 1 3mL ; (98:2 v/v) 1 ZmL/min <40 50µL 0.02% ( ) LC/MS/MS 30:70( :0.02% ) :0.35mL/min : : 5µL MS MRM 309.1/281.2 -D* 314.1/286.2 Alpha- - 325.1/242.9 Alpha- - -D5* 330.1/302.2 300.1/227.0 285.5/192.5 * 292.2/198.2 321.1/275.1 -D4* 325.1/279.0 271.1/140.1 -D5* 275.6/40.1 287.1/241.1 -D5* 290.2/198.2 301.1/255.1 -D5* 306.1/260.1 * -D Alpha- - -D5 -D4 -D5 -D5 -D5 GC Hypersil GOLD PFP 3pm, 150 2.1mm 25403-152130 112

Beta GC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 1 ml 100mM (ph 4.5) 1mL 2mL 100mM (ph 4.5) / HyperSep Verify-CX 1 3mL 1 3mL 1 3mL 100mM (ph 4.7) <3 1 2mL/min 2 1mL / (1:1) ( >10 5 ) Beta 1 1mL / (78:20:2) 1 2mL/min ( ) IPA/NH 4 0H (ph 11-12) <40 : ( ) 5mg/mL -20 ( ) 100µL ( ) / 70 15 1 2µL ( ) GC/MS GC TraceGOLD TG-5MS 30m 0.25m 0.25µm 26098-1420 7- GC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) :B- 2mL 1mL - 100mM (ph5.0) 5.000 F L Patella Vulgata / 65 3 HyperSep Verify-CX 1 3mL 1 3mL 1 1 ml 100mM (ph 6.0) <3 1 2mL/min 1 2mL 1 2mL 20% 100mM (ph=6.0) ( >10 5 ) 1 2mL /7-1 3mL 2% NHqOH 1 2mL/min <40 50µL 50uLMTBSTFA( 1% TBDMCS) / 90 20 MTBSTFA 1 2µL GC/MS *** -TBDMS 372 374 326 7- -TBDMS 342 344 399 -D4-TBDMS 376 378 377 7- -D4-TBDMS 346 348 403 * GC/MS -D4 7- -D4 ** TS-48927 *** GC TraceGOLD TG-5MS 30m 0.25m 0.25µm 26098-1420 113

Beta GC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 1mL (ph 4.5) 1mL 2mL (ph=4.5) / HyperSep Verify-CX 1 3mL 1 3mL 1 3mL100m M (ph 4.5) <3 1 2mL/ 2 1mL / (1 :1) ( >10 5 ) Beta 1 1mL / / (78:20:2) <40 : ( ) 5mg/mL 200C( ) 100µL ( ) / 70 15 1 2 GC/MS GC TraceGOLD TG-5MS 30m 0.25m 0.25µm 26098-1420 IPA/NH 4 0H (ph 11-12) / 200mg 10mL HyperSep Verify-CX ( 60108-742) 1 ml 100mM * 1mL / 2mL 100mM / HyperSep Verify-CX 1 3mL 1 3mL 1 1 ml 100mM <3 1 2mL/min 1 3mL 1 3mL10 mm ( >10 5 ) / / 1 3mL : (90:10) 1 2mL/min <40 1000µL 0.1% ( ) 20µL LC * 8- GC Hypercarb 3µm, 50 2.1 mm 35003-052130 114

DHEA, GC GC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 5mL ph 5.5-6.5 3,000rpm 5 HyperSep Verify-CX 1 3mL 1 3mL 1 1 ml 100mM (ph 6.0) 1 3mL ( >10mm ) 1 3mL 1 2mL/min 2mL 200mM (P 7.0) 250 p / 500C 1 1; 1 NaHC0 3 /Na 2 C0 3 ph 10-11 5mL n- 10 3000rpm 5 30 50pLMSTFA/NH41/ (1,000:2:5, V/W/W) 70 20 3000rpm 1 GC 1 2µL GC/MS ** 432 417 432 417 DHEA 432 417 16a * 520 259 * GC/MS 20ng/mL 16a ** GC TraceGOLD TG-5MS 30m 0.25m 0.25µm 26098-1420 GC GC/MS 100mg 1 ml HyperSep Diol ( 60108-572) 1mLp 6 2mL / 5m1 ph 6 10 2700rpm 15 HyperSep Diol 1 3mL 1 3mL 1 3mL 1 3mL 0.1mM (ph= 6.0) 1 3mL 1 3mL5% 0.1 mm (ph=6.0) >10 5 1 3mL 2 3mL 55 100µL 100µL 1 % t-bdmcs MTBSTFA 70 30 GC/MS-NCI 1µL MTBSTFA * -D5 -D4 GC TraceGOLD TG-5MS 30m 0.25m 0.25µm 26098-1420 115

60mg 3mL HyperSep Retain PEP ( 60107-203) 100mL 10mL (20mg/L) 30mL 0.5% 100mL 2ppm Retain PEP 2mL 2mL 2mL 2mL 5% 0.5% 2mL1% ACN:20mmol (ph 4) (40:60, v/v) 1mL :ACN:20mmol (ph 4) (40:60, v/v) :1.0mL/min :10µL :30 :290nm GC Hypersil GOLD 5pm, 250 4.6mm 25005-254630 60mg 3mL HyperSep Retain PEP ( 60707-203) HyperSep Retain -PEP 1 3mL 1 3mL S E 1 3mL 1 3mL 5% 1 3mL (%) 97.9 96.3 74.0 71.9 93.9 54.1 98.6 58.6 45.6 GC/MS 500mg 6mL HyperSep SAX ( 60108-434) 1mL 100pL D3-MMA 1mL / 20 2000rpm 5 1 3mL 1 3mL SPE 1 10mL 3 1 5mL 3 1 2mL MTBE* 3 1 5mL3% MTBE 1 2 ml/min <35 25µL MSTFA+1%TMCS 256L 60 20 1 2µL GC/MS GC TraceGOLD TG-5MS 30m 0.25m 0.25µm 26098-1420 116

/ GC GC/MS 100mg 1mL HyperSep C18 ( 60108-302) 500µL 20% * / 500µL / / HyperSep C18 1 3mL 1 3mL 1 1 ml 100mM HCI <3 1 2mL/ 1 3mL 1 3mL 1 3mL ( >10 5 ) 1 1mL2% <40 50µL 50µL BSTFA( 1 % TMCS ) **500L 70 30 1 2µL GC/MS -TMS 210 225 182 -D10-TMS* 220 235 192 * 1- -1- (FID): -D10(GC/MS) ** TS-38831 GC TraceGOLD TG-5MS 30m 0.25m 0.25µm 26098-1420 / LC/MS 200mg 6mL HyperSep Verify-CX ( 60108-722) 0.2 0.5mL 1mL ( ) * / 3mL 100mM HCI / HyperSep Verify-CX 1 3mL 1 3mL 1 1 ml 100mM HCI <3 1 2mL/min 1 3mL 1 3mL 1 3mL ( >10 10 ) 1 3mL 2% 1 2mL/min <40 100 5 GC/MS * -D10 - GC Hypersil GOLD 3pm, 150 2.1 mm 25003-152130 117

GC GC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 2mL 100mM (ph =6.0) * 2mL ph 6.0 0.5 100mM ph / HyperSep Verify-CX 1 3mL 1 3mL 1 1 ml 100mM (ph 6.0) <3 1mL/min 1 3mL 1 2mL200mM HCI ( >10 5 ) 1 2mL 1 3mL ( >10 5 ) 1 3mL /IPA/NH 4 OH (78:20:2) 1 ml/min IPA/NH 4 0H (ph 11-12) <40 100µL 1 2µL GC/MS *** 84 133 162 -D4* 88 137 166 98 119 176 -D3* 101 122 179 * -D4 -D3 ** GC TraceGOLD TG-5MS 30m 0.25m 0.25µm 26098-1420 200mg 3mL HyperSep Cyano ( 60108-747) 1mL 1mL 8mL / HyperSep Cyano 1 3mL 1 3mL <3 1 2mL/min 1 3mL1% ( ) ( >10 5 ) 2 3mL1% 1 2mL/min <40 100µL 0.1% ( ) 50µL LC-UV/260nm) * GC Hypersil GOLD 3pm, 150 4.6mm 25003-154630 118

200mg 3mL HyperSep Retain-AX ( 60107-401) 3% 500µL HyperSep Retain-AX 1 1mL 1 1mL 0.5mL 1 1 ml 1% CH403S 1mL 1 1mL ACN(1% ) LC/MS/MS ACN:3mmol/L 85:15) MRM 281.2/281.2 315.2/315.2 C17 269.2/269.2( C17 ) GC Hypersil GOLD 5µm, 150 4.6mm 25005-154630 - GC GC/MS 200mg 6mL HyperSep Verify-CX ( 60108-742) 2mL 400µL 200µL 10% / 90 40 2,000rpm 10 500 µl 50% / 50% ph 5-60 2mL 1mL - - 100mM (ph 5.0) 5.000 F /ml Patella Vulgata 60 3 2,000rpm 10 1.0 N NaOH ph 5-6 1 3mL 1 3mL 1 1 ml 100mM (ph 6.0) <3 1 2mL/min 1 3mL 1 3mL 100mM (ph 4.5) 1 3mL ( >10 5 ) 1 3mL / / (84:12:4) <40 200µL1:1 / 60 60 <40 50µL / (70:30) 1 2µL GC/MS *** 299 242 214 355 282 229 -D3* 358 285 232 371 314 298 285 341 228 6-327 268 383 357 300 413 341 268 397 -D3* 344 271 400 * GC/MS -D3 -D3 ** GC TraceGOLD TG-5MS 30m 0.25m 0.25µm 26098-1420 119

- GC GC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 2mL 400µL 200µL 10% / 90 40 15 2,000rpm 10 500pL50% / 50% ph 5-6 2mL / 60 ( ) 200µL10% 60 30 ph 5-6 2,000rpm 10 1 3mL 1 3mL 1 3mL 100mM (ph 6.0) <3 1 2mL/min 1 3mL 1 3mL 100mM (ph 4.5) 1 3mL ( >10 5 ) 1 3mL /IPA/NH 4 OH (76:20:4) 1 2mL/min IPA/NH 4 0H (ph 11-12) <40 100µL 100µL BSTFA ( 1%TMCS}** / 70 45 MTBSTFA 1 2µL GC/MS *** -D4 251 222 250 247 218 246 -D4 TMS* 308 280 309 TMS* 305 276 304 TMS 335 245 290 O- TMS 393 378 303 N- TMS 393 378 116 TMS 357 342 289 -D3 TMS* 374 359 346 -D6 TMS* 377 349 316 TMS 371 356 343 TMS 429 414 356 TMS 373 315 358 -D3 TMS* 432 417 404 -D6 TMS* 435 420 404 TMS 429 414 401 TMS 487 472 414 369 327 268 -D3 TMS 389 300 374 -D6 TMS 392 303 377 TMS 386 297 371 - D3 TMS 447 432 358 TMS 444 429 355 -D3 TMS 477 462 420 -D6 TMS 480 465 420 TMS 474 459 417 -D3 TMS 535 520 290 TMS 532 517 287 * GC/MS D4- D4- D3- D3- D6- D6- D6- D6- LOD/ LOQ ** TS-38831 120

GC/MS 200mg 6mL HyperSep Retain-CX ( 60107-314) ( ) 1mL 1.0mL - ( - 100mM (ph 5.0) 5.000 F /ml Patella Vulgata ) 600C T 3 10 1.0N NaOH ph 6.0 0.5 ( ) 1mL 1mL 100m M (ph 6.0) 1 2mL/min 1 1mL 1 1 ml 100mM (ph 4.5) 1 1mL ( >10 3 ) 2 0.5mL / IPA/NH 4 OH (78/20/2) 1 2mL/min <40 50µL 50µL BSTFA( 1 % TMCS**), / 70 20 MTBSTFA 1 2µL GC/MS : ( ) -TMS 371 234, 343 -D6-TMS* 377 237, 349 -TMS 429 401, 414 -D6-TMS* 435 404, 420 6- -TMS 399 400, 340 6- -D6-TMS 405 406, 343 * -D6-TMS -D6-TMS ** TS-38831 GC TraceGOLD TG-5MS 30m 0.25m 0.25µm 26098-1420 / LC/MS/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 1mL100m M (ph=6) * 1mL / 2mL 100mM (ph=6) / HyperSep Verify-CX 1 3mL 1 3mL 1 3mL 100mM (ph=6) <3 1 2mL/min 1 3mL 1 3mL 100mM 1 3mL ( >10 5 ) 1 3mL : : (78:20:2) 1 2mL/min <40 100µL : 5 LC/ MS MRM 330.0/90.1 -D6* 336.0/76.1 * -D6 GC Hypersil GOLD 3µm, 50 4.6mm 25203-054630 121

60mg 3mL HyperSep Retain PEP ( 60107-203) 100mL 10mL (100mg/L) 30mL 0.5% 100mL 10ppm Retain PEP 2mL 2mL 2mL 2mL 5% 0.5% 2mL 1% ACN:20mmol (ph 4) (30:70, v/v) 1mL :ACN:20mmol (ph 4) (40:60,v/v) :1.0mL/min :1µL :30 : (290nm) GC Hypersil GOLD 5µm, 250 4.6mm 25005-254630 / HPLC 200mg 10mL HyperSep Verify-CX ( 60108-742) 4mL 2mL 100m M (PH=6.0) 1mL / / 2,000rpm 10 ph 6.0 0.5 100mM ph HyperSep Verify-CX 1 3mL 1 3mL 1 1mL100m M (ph=6.0} <3 1 ml/min 1 3mL 1 1mL 100mM 1 3mL ( >10 5 ) 1 3mL /IPA/NH 4 OH (78:20:2) 1 ml/min IPA/NH 4 0H (ph 11-12) <40 200µL : (1:3) U / 30 100µL LC 235nm : 30% 0.25 M (ph 2.7) :2mL/min * : 122

200mg 6mL HyperSep Retain PEP ( 60107-212) 50mL 50mL 0.1 M ZnS0 4 / 500mL * / 500mL / HyperSep Retain PEP 1 2mL 1 2mL <3 1 2mL/min 1 2mL ( >10 20 ) 750mL 1 2mL/min LC * -D, GC Hypersil GOLD 3µm, 150 4.6mm 25003-154630 / HPLC 200mg 10mL HyperSep Verify-CX ( 60108-742) 2mL 100mM (ph=6.0) * 1mL / / 2,000rpm 10 ph 6.0 0.5 100mM ph 1 3mL 1 3mL 1 1 ml 100mM (ph= 6.0) <3 1 ml/min 1 3mL 1 1 ml 100mM 1 3mL ( >10 5 ) 1 3mL /IPA/NH 4 OH (78:20:2) 1mL/min IPA/NH 4 0H (ph 11-12) <40 200µL : (1:3) / 30 100µL HPLC * 123

(SPE-LC/MS ) 10mg 2mL SOLA HRP 96- ( 60309-001) : 1mL 1 ml 1mL 200µL / (80; 20) 200µL 2 40 200µL : 1. 25ng/mL LC/MS LC/MS : Accucore RP-MS 2.6um 2.1 100mm : 17626-102130 : A: ++0.1% B: +0.1% : /min % A %B 0.00 75 25 0.02 75 25 4.00 25 75 4.50 25 75 4.51 75 25 6.00 75 25 : 0.6 ml/min : 25 : 2.5µL MS : ( HESI) (SRM) 3000V 300 11- (1) (2) (3) (4) IS(5) 2.4 85-130% RSD<12 %(n=6) 3.1ng/mL-1000ng/mL R2>0.99 124

- (SPE-LC/MS ) 10mg 1 ml SOLA SCX ( 60109-002) : 500µL 500µL 200µL 250µL +0.1% 250gL + 0.1% 250µL DCM/IPA+S% (80; 20) 40 : ( 80; 20 ) 200µL : 1.0.5mg/mL 5 - HPLC LC/MS : Accucore C18 2.6µm 2.1 50mm : 17126-052130 : A: +0.1% : +0.1% : /Min %A %B 0.00 90 10 2.50 60 40 : 0.7 ml/min : 45 : 1µL UV: 220nm (1) (2) (3) (4) (5) 2 0.05mg/mL5-80% RSD<5 %(n=6) 125

(SPE- HPLC) 10mg 1 ml SOLA SCX ( 60109-002) 1 ml 1 ml 350µL 350µL +2% 1 350µL 2 350µL +5% 1 2 50µL 350µL HPLC : Accucore R MS 2.6um50 3 mm : 17626-053030 : A: 20mM : : /min % A %B 0.0 95.00 5.00 0.5 95.00 5.00 5 5.00 95.00 5.5 5.00 95.00 5.6 95.00 5.00 7.5 95.00 5.00 : 0.8 ml/min : 25 : 10µL UV: 254nm : 1. 10µg/mL HPLC 1. 2. 3.IS 1. 2. 3.IS 126

2. 10µg/mL HPLC 1. 2. 3.IS 1. 2. 3.IS 3. 87-102% RSD<11.8%(n=3) 127

(SPE- HPLC) 10mg 1 ml SOLA SCX ( 60109-002) 1 ml 1 ml 250µL ++1S 250µL +2% 250gL +2% 250µL +5% 40 200µL : 1. 10µg/mL IS LC 1) 2) 2. 119% RSD = 4.03%(n=6) HPLC : Syncronis C18 50m 100 4.6 mm : 97105-104630 : A: 20mM B: : /min % A %B 0.0 95 5 1.0 95 5 5. 0 5 95 5.5 5 95 5.6 95 5 8.0 95 5 : 1 ml/min : 30 : 10µL UV: 277nm 6 - (SLE-LC/MS) 200mg 3mL HyperSep SLE ( 60109-200-3-7) : 400µL +IS( -D3) : 5min : 1.4mL 0.5-1% 1 ml/min 40 200µL : 1. 6-80% RSD <12% LC/MS : Hypersil Gold 5pm 4.6 150mm : 25005-154630 : A: +0.05% B: +0.05% : /min %A %B 0.00 75.00 25.00 20.00 0.00 100.00 : 1mL/min : 40 : 10µL MS : 128

25-OH Vit D2 25-OH Vit D3 (SPE- LC/MS) 10mg 2mL SOLA HRP 96 ( 60309-001) 500500µL 2% 200µL 200µL / (60:40) 200µL 2 40 : ( 30; 70) 100µL LC/MS : Syncronis C18 1.7µm 50 2.1 mm : 97102-052130 : A: +0.1% B: +0.1% : 2min 70-100%B : 0.8mL/min : 40 : 50µL MS : : 1. 25-OH Vit D2 25-OH Vit D3 >94% RSD<4.0% LOD 5ng/mL 2. 25- Vit D2 25- Vit D3 5-1000ng/mL r 2 =0.9994 0.9958 129

(SPE- LC/MS) 10mg 2mL SOLA SCX 96 ( 60309-002) 500µL 500µL 2% 2000L +IS( ) 200µL 2% 200µL 2% / (70.30) 200µL 5% 40 200µL : 1. 30ng/mL LC/MS LC/MS : Accucore RP-MS 2.6µm 50 2.1 mm : 17626-052130 : A: +0.1% B. +0.1% : /min % A %B 0.00 95.00 5.00 2.00 5.00 95.00 2.10 95.00 5.00 3.50 95.00 5.00 : 0.35 ml/min : 40 : 5µL MS : (ESI) (SRM) 3000V 300 3. 2-100ng/mL r 2 =0.991 2. 106%,RSD=6.81% 130

(SPE- LC/MS) 10mg 1 ml SOLA HRP ( 60109-001) 0.5mL 0.5 ml 100µL 200µL / (80; 20) 250µL 40 100µL LC/MS : Accucore PFP 2.6µm 30 2.1 mm : 17426-032130 : Accucore PFP 2.6µm 10 2.1 mm : 17426-012105 : A: B: : /min % A %B 0.0 100 0 5.0 0 100 5.1 100 0 6.5 100 0 : 1mL/min : 40 : 10µL MS : ( ESI) (SRM) 2500V 300 : 1. 500ng/mL LC/MS 2. 73.2%, RSD=2.3%/n=3) 3. 10µg/mL-1000ng/mL R=0.99 131

(SPE- LC/MS) 10mg 2mL SOLA HRP 96 ( 60309-001) 1 ml 1 ml 100µL 500µL +0.1% 500µL 200µL 90% 2 40 : ( 80; 20) 200µL LC/MS : Accucore RP-MS 2.6µm 50 2.1 mm : 17626-052130 : Accucore RP-MS 2.6µm10 2.1 mm : 17626-012105 : A: +0.1% B: +0.1% : %B 0min 5 0.1min 5 1.0min 95 1.6min 95 1.62min 5 3.6min 5 : 0.75mL/min : 60 t: 15µL MS : (ESI) (SRM) 3000V 300 132

: 1. 1ng/mL LC/MS 2. 99.3%, RSD=4.88(n=3) 3. MF 97.8-105.3% RSD<3.72(n=6) 4. 1ng/mL-1000ng/mL R 2 =0.9984 1ng/mL 133

(SPE- LC/MS) 10mg 1 ml SOLA SCX ( 60109-002) 1 ml 1 ml 100µL +1S1 ) 200µL +0.1% 250µL +3% 40 : ( 80; 20) 100µL : 1. 0.5ng/mL LC/MS LC/MS : Accucore aq 2.6µm 50 2.1 mm : 17326-052130 : A: +0.1% B: +0.1% : 2min 20%-70%B : 0.4mL/min : 40 : 2.58L MS : ( ESI) ( ) (SRM) 3000V 300 0.5ng/mL LC/MS 2. 86.4% 65.8% RSD<6.11n=3) 3. 0.5ng/mL - 500ng/mL R 2 =0.9974 0.9956 134

(SPE-LC/MS) 10mg 1 ml SOLA HRP ( 60109-001) 0.5mL 0.5mL 200µL 200µL / (90; 10 ) 200µL 2 40 : ( 50; 50) 100µL : 1. 1ng/mL LC/MS LC/MS : Accucore RP-MS 2.6µm 2.1 50mm : 17626-052130 : A: +0.1% B: +0.1% : /min % A %B 0.00 50.00 50.00 1.00 0.00 100.00 : 0.6mL/min : 40 t: 20µL MS : ( HESI) (SRM) 3000V 210 2 86% RSD<5 %(n=3) 3. 1ng/mL-1000ng/mL R 2 =0.999 135

(SLE-LC/MS) 500mg 3mL HyperSep SLE ( 60109-500-3-7) : 300gL +300µL 0.1% +20µL IS(d6- ) : 5min : 2 100 400C 200µL : ( 80:20) : 1. 2.5ng/mL LC/MS LC/MS : Accucore C18 2.6µm 2.1 50mm : 17126-052130 : A: +0.1% B: +0.1% : /min % A % B 0.0 95 5 0.2 95 5 1.0 30 60 3.0 30 60 3.2 5 95 3.8 5 95 4.0 95 5 5.0 95 5 : 0.4mL/min : 40 : 100L MS : (HESI-II) (SRM) 3500V 375 2. 83.2%, RSD=1.86%(n=6) 3. 0.05ng/mL-5ng/mL R 2 =0.999 136

(SPE- HPLC) 10mg 1 ml SOLA HRP ( 60109-001) 0.5mL 0.5mL 200µL +IS( ) 200µL / (90:10 ) 200µL +0.1% : 1. 20ng/mL ( ) HPLC HPLC : Hypersil GOLD 3µm 100 4.6 mm : 25003-104630 : A: 25mM B: : /min % A %B 0.0 80 20 1.8 70 30 2.3 60 40 2.5 80 20 4.0 80 20 : 1.5mL/min : 20 : 25µL : :480nm :560nm 1. 2. IS( ) 3. 1 ng/ml-100ng/ml R 2 =0.9991 2. 20ng/mL ( ) 101.2%, RSD=6.9%(n=6) 137

(SPE-LC/MS ) 10mg 2mL SO A R ( 60309-001) 0.5mL 0.5 ml 200µL 200µL / (70; 30) 250µL +1% 2 40 : ( 50; 50) +0.5% 20µm 200µL : 1. 0.25ng/mL LC/MS LC/MS : Accucore RP-MS 2.6µm 2.1 50mm : 17626-052130 : A: +0.1% B: +0.1% : /min % A % B 0.00 40.00 60.00 2.00 30.00 70.00 : 0.6mL/min : 30 : 2.5µL MS : ( HESI) (SRM) 4000V 365 2. 109% RSD<9 %(n=6) 3. 0.25ng/mL-10ng/mL,R 2 =0.9974 138

6-200mg 10mL HyperSep Verify-CX ( 60108-742) 1 x 2mL 100mM (ph= 6.0) * / 4mL 2000rpm 10 ph 6.0 0.5 100mM ph 6 HyperSep Verify-CX 1 x 3mL 1 x 3mL 1 x 1mL 100mM (ph=6.0) <3 1mL/min 1 x 3mL 1 x 2mL 100mM (ph 4.5) 1 x 3mL ( >10 10 ) 1 x 3mL /IPA/NH 4 OH (78:20:2) 1 2mL/min IPA/NH 4 OH (ph 11-12) <40 50µL / 50µL BSTFA 1% TMCS ** / 70 45 BSTFA 1 2µL GC/MS *** D6-6-AM-TMS* 405 406 343 6-AM-TMS 399 400 340 * GC/MS ** TS-38831 GC TraceGOLD TG-5SilMS 30m 0.25m 0.25µm 26096-1420 200mg 10mL HyperSep Verify-CX ( 60108-742) 139 1mL 1.0mL 100mM (ph 6.0) * 1mL / ph 6.0 100mM ph 1 x 3mL 1 x 3mL 1 x 1mL 100mM (ph= 6.0) <3 1mL/min 1 x 2mL 1 x 2mL 20% ACN 100mM (ph 6.0) ( >10 10 ) 1 x 2mL 1 x 5mL 2% 1 2mL/min <40 HPLC * -D5 Alpha- - -D5 -D4 -D5 -D5 HPLC BETASIL Phenyl/Hexyl 5µm, 150 4.6mm 73005-154630

GC GC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 2mL * 1mL 100mM (ph 6.0) 1mL 0.35 M / 20 ph 6.0 0.5 100mM ph 3mL 3mL 1mL 100mM (ph 6.0) <3 1 2mL/min 3mL 1mL 100mM 3mL ( >10 5 ) 3mL /IPA/NH 4 OH (78:20:2) 1 2mL/min IPA/NH 4 OH (ph 11-12) 30µL DMF*** <40 30µL 50µL PFPA (PFAA)**** 50µL PFPOH 70 20 <40 1 2µL (TMS ) *** D 5 - * 194 92 123 190 91 118 D 5 - * 208 92 163 204 91 160 * ** *** TS-20672 50mL **** TS-65193 10 x 1mL GC TRACE TR-DoA5 15m 0.25mm 0.25µm TRACE TR-DoA35 15m 0.20mm 0.33µm 26AF130P 26AC497P 500mg 6mL HyperSep Diol ( 60108-575) 1mL ph 6 * 2mL / 5mL ph 6 10 2700rpm 15 1 x 3mL 1 x 3mL 1 x 3mL 1 x 3mL 0.1mM (ph= 6.0) 1 x 3mL 1 x 3mL 5% ACN 0.1mM (ph 6.0) >10 5 1 x 3mL 2 x 3mL 55 * 100µL ACN 100µL 1% t-bdmcs MTBSTFA 70 30 1µL GC/MS-NCI MTBSTFA GC/MS * -D5 -D4 GC TraceGOLD TG-5SilMS 30m 0.25m 0.25µm 26096-1420 140

GC GC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 5mL 2mL - - :100mM (ph=5.0) 5,000 F /ml Patella Vulgata / 65 3 2,000rpm 10 700µL 1.0N NaOH ph 6.0 0.5 3mL 3mL 1mL 100mM (ph 6.0) <3 1 2mL/min 3mL 10% (v/v) ( >10 5 ) 1mL / (50:50) a 3mL /IPA/NH OH (78:20:2) 1 4 2mL/min IPA/NH OH 4 (ph 11-12) b 3mL /IPA (80:20) c 3mL d 3mL <40 50µL 50µL MSTFA( 3% ) / 70 20 MSTFA 1 2µL (GC/MS) (TMS ) * -TMS 432 301 209 19- -TMS 405 315 225 640 52 462 370,143-2TMS 432 327 297 10- -2TMS 418 287 194 #1 640 52 462 143 #2 625 462 370 143 11- - 522 417 158 409 313 281 19- -2TMS 405 315 225 Alpha- 504 417 17- - -TMS 432 341 327 209 472 381 342 149 * GC TRACE TR-DoA5 15m 0.25mm 0.25µm TRACE TR-DoA35 15m 0.20mm 0.33µm 26AF130P 26AC497P 141

/ 60mg 3mL HyperSep Retain-CX ( 60107-303) 1mL 100mM (ph= 6) * 1mL 2mL 100mM (ph= 6) / ph 6.0 0.5 100mM ph / 1 x 3mL 1 x 3mL 1 x 1mL 100mM (ph= 6) <3 1 2mL/min 1 x 3mL 1 x 3mL 1% 1 x 3mL ( >10 5 ) 1 x 3mL ACN (78:20:2 v/v) 1 2mL/min <40 100µL 5µL GC/MS MRM -TMS 432 19- -TMS 405 640-2TMS 432 10- -2TMS 418 #1 640 #2 625 11- - 522 409 19- -2TMS 405 Alpha- 504 17- - -TMS 432 472 * HPLC Hypersil GOLD 3µm, 150 2.1mm 25003-152130 SPE-HPLC 30mg 1mL HyperSep Retain- CX ( 60107-301) 1mL 1mL 1mL, 20µl 5N HCl 2mL 0.1N HCl, 2mL 2mL 2% 40:60 HPLC Hypercarb 5µm,100x4.6mm 35005-104630 A: (ph9.0): (4:6) 1mL/min 10µL 220nm 30 (1) (2) -3- (3) -6- (4) (5) 142

/ LC/MS/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 1mL 100mM (ph 6.0) * 1mL 2mL 100mM (ph 6.0) / ph 6.0 0.5 100mM ph / 3mL 3mL 1mL 100mM (ph 6.0) <3 1 2mL/min 3mL 3mL 1% 3mL ( >10 5 ) 3mL (78:20:2, v/v/v) 1 2mL/min <40 100µL 5µL LC 0.1% (33:67, v/v) 0.35mL/min HPLC Hypersil GOLD 3µm, 150 2.1mm 25003-152130 278.8/91.1 -D3* 281.2/91.2 256.2/167.1 -D3* 259.2/167.1 280.2/107.1 EDDP 278.2/234.2 EDDP-D3* 281.4/234.2 310.2/105.1 -D9* 319.2/268.3 264.2/91.1 326.2/44.1 -D5* 331.1/267.1 340.2/58.1 -D11* 351.3/64.0 308.1/161.0 264.2/58.1 -D3* 268.2/58.0 278.2/58.2 308.2/235 * 143

GC GC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 2mL * 1mL 100mM (ph 5.0) / ph 5.0 0.5 100mM ph 3mL 3mL 1mL 100mM (ph 5.0) <3 1 2mL/min 3mL 1mL 100mM ( >10 5 ) 2mL 3mL / (50:50) 1 2mL/min <40 100µL 25 50µL 0.2M TMPAH*** 1 2µL (GC/MS) *** 156 141 157 156 141 157 168 167 181 * 221 157 236 156 141 197 204 232 117 168 167 195 172 157 173 *** D 5-201 214 196 195 209 169 184 185 169 184 112 13C 4-200 185 196 195 181 D 5-237 151 232 146 175 * ** *** TS-49301 MethElut 12x1mL GC TRACE TR-DoA5 15m 0.25mm 0.25µm TRACE TR-DoA35 15m 0.20mm 0.33µm 26AF130P 26AC497P 144

200mg 10mL HyperSep Verify-CX ( 60108-742) 2mL 1mL - - 100mM (ph=5.0) 5,000 F /ml Patella Vulgata / 65 3 2,000rpm 10 1 x 3mL 1 x 3mL 1 x 1mL 100mM (ph= 6.0) <3 1mL/min 1 x 2mL 1 x 2mL 20% ACN 100mM (ph= 6.0) ( >10 5 ) 1 x 2mL 1 x 5mL 4% 1 2mL/min <40 50µL 50µL BSTFA** ( 1% TMCS)** / 70 20 BSTFA 1 2µL GC/MS *** Xananx 308 279 204 - -TMS 381 396 382 Librium 282 283 284 Klonopin 387 352 306 Valium 256 283 221 -TMS 359 341 245 -TMS 288 360 389 -TMS Ativan 429 430 347 -TMS 341 342 343 -TMS Serax 429 430 313 * 269 241 324 -TMS Restoril 343 283 257 Halcion 313 314 342 - -TMS 415 417 190 * GC/MS -D5 ** TS-38831 GC TraceGOLD TG-5SilMS 30m 0.25m 0.25µm 26096-1420 145

200mg 10mL HyperSep Verify-CX ( 60108-742) 2mL * 1mL - - :100mM (ph=5.0) 5,000 F /ml Patella Vulgata / 65 3 2,000rpm 10 1 2µL GC/MS *** -D5-TBDMS 332 334 333 -TBDMS 327 328 329 -D5-TBDMS 462 519 462 -TBDMS Serax 457 513 459 -D5-TBDMS 362 390 288 -TBDMS Restoril 357 359 385 Ativan 491 513 493 Klonopin 372 374 326 7- -TBMS 456 458 513 Valium 256 238 221 -TBDMS 345 347 402 * 269 241 324 - -TBDMS Versed 398 400 440 -TBDMS 357 310 356 7- -TBDMS 397 324 398 Xanax 308 279 204 - -D5-TBDMS 386 388 387 - -TBDMS 383 384 381 Halcion 313 314 342 - -TBDMS 415 417 190 * ** GC TRACE TR-DoA5 15m 0.25mm 0.25µm TRACE TR-DoA35 15m 0.20mm 0.33µm 26AF130P 26AC497P 146

200mg 3mL HyperSep Diol 60108-573) 1mL 100mM (ph= 6) * 1mL / 1g (1:4) / 3mL 100mM (ph= 6) ph 6.0 0.5 100mM ph / 1mL 5000 F /ml - (ph 5.0) * 1mL / 65 3 2,000rpm 10 3mL 100mM (ph 6.0) HyperSep Diol 1 x 3mL 1 x 3mL 100mM (ph 6) <3 1 2mL/min 1 x 3mL 5% (v/v) ACN 100mM (ph6) ( >10 5 ) 1 x 3mL ( >10 5 ) 1 x 3mL (98:2 v/v) 1 2mL/min <40 50µL ACN 50µL BSTFA( 1% TMCS**) 70 30 1µL GC/MS 308 279 204 -D* 513 284 Alpha- - 318 396 383 Alpha- - -D5* 386 401 256 283 284 -D5* 287 289 429 430 347 -D4* 433 435 34 342 343 -D5* 345 347 429 313 430 -D5* 435 433 343 257 283 -D5* 348 262 * -D Alpha- - -D5 -D5 -D4 -D5 -D5 -D5 GC TraceGOLD TG-5SilMS 30m 0.25m 0.25µm 26096-1420 147

Beta 200mg 10mL HyperSep Verify-CX ( 60108-742) 1mL 100mM (ph 4.5) 1mL 2mL 100mM (ph 4.5) / 1 x 3mL 1 x 3mL 1 x 3mL 100mM (ph 4.7) <3 1 2mL/min 2 x 1mL / (1:1) ( >10 5 ) 1 x 1mL / (78:20:2) 1 2mL/min IPA/NH 4 OH (ph 11-12) <40 5mg/mL ( ) -20 ( ) 100µL ( ) / 70 15 1 2µL Beta GC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 1mL 100mM (ph 4.5) 1mL 2mL 100mM (ph 4.5) / 1 x 3mL 1 x 3mL 1 x 3mL 100mM (ph 4.7) <3 1 2mL/min 2 x 1mL / (1:1) ( >10 5 ) 1mL /IPA/NH 4 OH (78:20:2) 1 2mL/min IPA/NH 4 OH (ph 11-12) <40 5mg/mL ( ) -20 ( ) 100µL ( ) / 70 15 1 2µL 148

- SPE-HPLC 30mg 1mL HyperSep Retain- PEP ( 60107-201) 1mL 1mL 1mL, 0.5% 1mL 0.5% 5% 1mL 1% - HPLC (1) (2) (3) (4) (5) (6) (7) HPLC Hypersil GOLD 5µm, 150x4.6mm 25005-154630 A: + 0.1% ; B: +0.1% ; 15 min 5-55%B 1mL/min 10µL 220nm 25 GHB 200mg 3mL HyperSep Retain-AX ( 60107-404) 1mL * 0.5mL 100mM (ph 6.0) / 10 2700rpm 10 HyperSep Retain-AX 1 x 3mL 1 x 3mL 1 x 1mL 100mM (ph 6.0) <3 1 15 1 x 2mL /NH OH (99:1) 4 1 / 60 200µL 1mL 5 2700rpm 5 50 50µL 25µL BSTFA ( 1% TMCS**) / 70 30 1 2µL GC/MS * GHB-D6-di-TMS* 239 240 241 GHB-di-TMS 233 234 235 * GC/MS D6-GHB ** TS-38831 GC TraceGOLD TG-5SilMS 30m 0.25m 0.25µm 26096-1420 149

SPE- HPLC 10mg 1mL SOLA HRP 60109-001 1 ml, 1 ml 200 µl +IS 1mL / 95 5 + 0.5% 0.2mL + 0.1% 40 / 80 20 200µL Accucore C18 2.6 µm 50x2.1 mm 17126-052130 A: + 0.1% B: + 0.1% /min % A %B 0.01 75.00 25.00 2.00 5.00 95.00 2.50 5.00 95.00 2.60 75.00 25.00 10.00 75.00 25.00 0.4 ml/min 40 10µL 245nm 1. 10µg/ml IS HPLC 2. 108 113RSD 5.6%(n=5) Extracted sample # Doxepin Peak Area Protryptyline (IS) Peak Area Response ratio Calculated Amount/ ug.ml-1 Recovery 1 1596549 584194 2.7329089 9.01 1.18 2 1461480 491260 2.9749623 9.81 1.08 3 1650009 520862 3.1678429 10.44 1.22 4 1464907 469808 3.1180972 10.28 1.08 5 1526226 507463 3.0075611 9.92 1.12 Mean 3.1542078 9.89 1.13 RSD 56% Calibration Standard (5.2 ug/ml) 678918 215242 3.1542078 150

SPE- HPLC 200mg 3mL HyperSep SLE 60109-200-3-7 400µL 5min 1.4mL 0.5-1% 1mL/min 40 200µL Hypersil Gold 5µm,150x4.6mm,Uniguard Hypersil gold & holder 25005-154630,25005-014001,850-00 A: 0.05% ; B: 0.05 : 25-100%B,20min 1 ml/min 10µL 40 MS 500mg 6mL HyperSep Aminopropyl ( 60108-519) 151 1mL 100mM (ph= 5) * / 1mL / 2mL 100mM (ph= 5) / ph 6.0 0.5 100mM ph 1mL 100mM * 1 5mL / 2mL 100mM (ph= 5) helix pomatia 5,000 /ml 60 3 1 x 3mL 1 x 3mL 1 x 1mL 100mM (ph= 5.0) <3 1 2mL/min 1 x 2mL 1 x 3mL 100mM (ph= 5.0) 1 x 3mL 5 10 >10 / ) 1 2mL/min BSTFA <40 50µL 50µL BSTFA( 1% TMCS)** 70 20 BSTFA 1 2µL GC/MS -D4-TMS* 454 486 510 -TMS 450 482 506 -TMS 468 500 524 -D3-TMS* 471 503 527 * -D4-TMS -D3-TMS ** TS-38831 GC TraceGOLD TG-5SilMS 30m 0.25m 0.25µm 26096-1420

GC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 1mL 100mM (ph 5.0) * / 1mL 2mL 100mM (ph 5.0) / ph 6.0 0.5 100mM ph 1mL 100mM * 1 5mL / 2mL 100mM (ph 5.0) helix pomatia 5,000 /ml 60 3 Verify-CX 3mL 3mL 3mL 100mM (ph 5.0) <3 1 2mL/min 2mL 3mL 100mM (ph 5.0) 3mL (5 10 >10 / ) 3mL /IPA/NH 4 OH (78:20:2) 1 2mL/min IPA/NH 4 OH (ph 11-12) BSTFA <40 50µL 50µL BSTFA ( 1% TMCS)*** 70 20 BSTFA 1 2µL GC/MS -D4-TMS* 454 486 510 -TMS 450 482 506 -TMS 468 500 524 -D3-TMS* 471 503 527 * ** ** TS-38831 10 x 1mL GC TRACE TR-DoA5 15m 0.25mm 0.25µm TRACE TR-DoA35 15m 0.20mm 0.33µm 26AF130P 26AC497P 152

/ HPLC 200mg 10mL HyperSep Verify-CX ( 60108-742) 1mL 100mM (ph 5.0) * 1mL / 2mL 100mM (ph 6.0) / ( / ) 1mL 5000 F /ml b- (ph 5.0) * 1mL / 65 3 3mL 100mM (ph 6.0) 2,000rpm 10 3mL 3mL 1mL 100mM (ph 6.0) <3 1 2mL/min 2mL 3mL 100mM 3mL (5 10 >10 / ) 3mL /IPA/NH OH (78:20:2, v/v/v) 4 3mL / / (78:20:2, v/v/v) 1 2mL/min <40 50µL 5µL GC/MS * HPLC 468.4/55.1 -D4* 472.4/59.1 414.3/83.1 -D3* 417.4/55.1 0.1% (50:50, v/v) 0.35mL/min Hypersil GOLD Phenyl 3µm 50 2.1mm 25903-054630 SPE-HPLC 30mg 1mL HyperSep Retain- CX ( 60107-301) 1mL 1mL 1mL, 20µl 5N HCl 2mL 0.1N HCl, 2 ml 100% 2mL 5% MDA,MDMA 95%-101% Hypersil GOLD aq 5µm,150x4.6mm 25305-154630 5/95 /20mM K PO,pH7 2 4 1mL/min 10µL 214nm 30 153

/LC/PDA 200mg 10mL HyperSep Verify-CX ( 60108-742) 1mL 100mM 1mL / 2mL 100mM 3mL 3mL 3mL 100mM <3 1 2mL/min 3mL 3mL 100mM ( >10 5 ) 3mL / (90:10, v/v) 1 2mL/min <40 1,000µL 0.1% ( ) 20µL LC/PDA 0.1% (10:90, v/v) 0.1mL/min (200 350nm) HPLC Hypersil GOLD 3µm 150 2.1mm 25003-152130 -delta 9-THC 500mg 6mL HyperSep Aminopropyl ( 60108-519) 2mL * 100µL 10 M NaOH / 60 20 1.0mL ph 3.0 1 x 3mL 1 x 3mL 1 x 1mL (ph= 3.0) <3 1 2mL/min 1 x 2mL 1 x 2mL 100mM HCI/ACN (95:5) ( >10 5 10 ) 1 x 200µL 1 x 3mL / (50:50) 1 2mL/min BSTFA <40 50µL 50µL BSTFA 1% TMCS ** / 70 20 BSTFA 1 2µL GC/MS (TMS ) *** -delta 9-THC-D3* 374 476 491 -delta 9-THC-D9* 380 476 497 -delta 9-THC 371 473 488 * GC/MS - -delta 9-THC-D9 9-THC-D3 ** TS-38831 GC TraceGOLD TG-35MS 30m 0.25m 0.25µm 26094-1420 154

-delta 9-THC (pka 4.5) GC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 2mL * 100µL 10 M NaOH / 60 20 1.0mL ph 3.0( ph ph 3.0) 3mL 3mL 1mL (ph 3.0) <3 1 2mL/min 2mL 2mL 100mM HCl/ (95:5) (5 10 >10 / ) 200µL ( ) 3mL / (50:50) 1 2mL/min BSTFA <40 50µL 50µL BSTFA( 1% TMCS)*** / 70 20 BSTFA 1 2µL GC/MS (TMS ) *** D 3 - -delta 9 -THC 374 476 491 D 3 - -delta 9 -THC* 380 479 497 -delta 9 -THC 371 473 488 * ** ** TS-38831 10 x 1mL GC TRACE TR-DoA5 15m 0.25mm 0.25µm TRACE TR-DoA35 15m 0.20mm 0.33µm 26AF130P 26AC497P 200mg 10mL HyperSep Verify-CX ( 60108-742) 4mL 1mL ( ) / 5 2,000rpm 10 2mL 100mM (ph =6.0) / ph 6.0 100mM ph 1 x 3mL 1 x 3mL 1 x 1mL 100mM (ph 6.0) <3 1 2mL/min 1 x 3mL 1 x 2mL 100mM HCl 1 x 3mL ( >10 5 ) 1 x 3mL /IPA/NH 4 OH (78:20:2) 1 2mL/min IPA/NH 4 OH (ph 11-12) <40 HPLC HPLC Hypersil GOLD 3µm 150 4.6mm 25003-154630 155

-delta 9-THC Delta-9-THC() Delta-9- THC GC GC/MS 200mg 6mL HyperSep Verify-CX ( 60108-730) 1 2mL * / 1mL 2.0mL 100mM ph 3.0 0.5( ph ph 3.0) 3mL 3mL 1mL (ph 3.0) <3 1 2mL/min 3mL 2mL 100mM HCl/ (95:5) (5 10 >10 / ) 200µL ( 200µL ) (5 >10 / ) delta-9-thc( ) / 200µL ( 200µL ) 2mL ( delta-9-thc) 3mL / (50:50) 1 2mL/min ( BSTFA ) <40 50µL 50µL BSTFA( 1% TMCS)*** / 70 20 BSTFA 1 2µL (TMS ) *** D 3 - -delta-9-thc* 374 476 491 D 9 - -delta-9-thc* 380 479 497 -delta-9-thc 371 473 488 D 3 - -delta-9-thc* 374 462 477 -delta-9-thc 371 459 474 D 3 -delta-9-thc* 374 389 Delta-9-THC (303,315,330,343)** 371 386 * ** delta-9-thc ** TS-38831(10 x 1mL ) GC TRACE TR-DoA5 15m 0.25mm 0.25µm TRACE TR-DoA35 15m 0.20mm 0.33µm 26AF130P 26AC497P 156

THC 30mg 3mL HyperSep Retain-CX ( 60107-302) 2mL * 100µL 10N NaOH / 60 20 1.0mL ph 3.5 0.5 1 2mL/min 1 x 1mL 1 x 1mL 0.1M HCI/ACN (70:30) ( >10 3 ) 1 x 200µL 2 x 0.5mL / (50:50) 1 2mL/min <40 50µL / 50µL BSTFA 1% TMCS ** / 70 20 BSTFA 1 2µL GC/MS (TMS ) ( ) -THC-TMS 371 473 488 -THC-D3-TMS* 374 476 491 * -THC-D3-TMS ** TS-38831 GC TraceGOLD TG-35MS 30m 0.25m 0.25µm 26096-1420 /GC GC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 1mL 100mM (ph 3.0) * 1mL / 1g (1:4) 2mL 100mM (ph 3.0) / 3mL 3mL 1mL 100mM (ph 3.0) <3 1 2mL/min 4mL 2mL 100mM HCl ( >10 5 ) 3mL 3mL /IPA/NH 4 OH (78:20:2) 1 2mL/min IPA/NH 4 OH (ph 11-12) <40 100µL 1 2µL ** 158 104 245 83 114 144 * 221 157 81 -D7* 90 121 151 * ** GC TRACE TR-DoA5 15m 0.25mm 0.25µm TRACE TR-DoA35 15m 0.20mm 0.33µm 26AF130P 26AC497P 157

7- GC GC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 2mL * 1mL - - :100mM (ph=5.0) 5,000 F /ml Patella Vulgata / 65 3 3mL 3mL 1mL 100mM (ph 6.0) <3 1 2mL/min 2mL 2mL 20% 100mM (ph= 6.0) ( >10 5 ) 2mL 3mL 2% NH 4 OH 1 2mL/min <40 50µL 50µL MTBSTFA( 1% TBDMCS)*** / 90 20 MTBSTFA 1 2µL (GC/MS) ** -TBDMS 372 374 326 7- -TBDMS 342 344 399 -D4-TBDMS 376 378 377 7- -D4-TBDMS 346 348 403 * ** *** TS-48927(10 x 1mL ) GC TRACE TR-DoA5 15m 0.25mm 0.25µm TRACE TR-DoA35 15m 0.20mm 0.33µm 26AF130P 26AC497P / HPLC 200mg 10mL HyperSep Verify-CX ( 60108-742) 1mL 100mM (ph 6.0) / 1 5mL 1mL 1g (1:4) / 2mL 100mM (ph 6.0) ph 6.0 0.5 100mM ph 3mL 3mL 1mL 100mM (ph 6.0) <3 1 2mL/min 3mL 1mL 100mM 3mL >10 5 2mL CH 4 OH/NH 4 OH (98:2) 1 2mL/min 2.0mL 500µL / 2,000rpm 10 <40 HPLC 158

200mg 10mL HyperSep Verify-CX ( 60108-742) 1mL 100mM (ph 6) * 1mL / 1g (1:4) 2mL 100mM (ph 6) / 1 x 3mL 1 x 3mL 1 x 1mL 100mM (ph 6) <3 1 2mL/min 1 x 3mL 1 x 3mL 100mM HCl 1 x 3mL ( >10 5 ) 1 x 3mL ACN (78:20:2 v/v) 1 2mL/min 50µL 5µL LC/MS MRM 304.2/182.3 -D3* 307.2/185.2 290.1/168.0 -D8* 298.2/171.3 318.2/196.2 -D8* 326.2/204.2 * -D3 -D8 -D8 HPLC Hypersil GOLD 3µm 150 2.1mm 25003-152130 / GC GC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 159 1mL 100mM (ph 6.0) * 1 5mL / 1g (1:4) / 2mL 100mM (ph 6.0) ph 6.0 0.5 100mM ph 3mL 3mL 1mL 100mM (ph 6.0) <3 1 2mL/min 3mL 1mL 100mM 3mL ( >10 5 ) 3mL /IPA/NH OH (78:20:2) 4 1 2mL/min IPA/NH OH 4 (ph 11-12) <40 50µL 1 2µL ** 245 146 189 D 5 - * 250 151 194-259 203 146 263 164 207 3-259 160 203 245 146 189 289 140 303 187 317 201 289 289 268 194 * ** GC TRACE TR-DoA5 15m 0.25mm 0.25µm TRACE TR-DoA35 15m 0.20mm 0.33µm 26AF130P 26AC497P

/ GC GC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 1mL 100mM (ph 6.0) * 2mL / 1g (1:4) / 2mL 100mM (ph 6.0) / ph 6.0 0.5 100mM ph 3mL 3mL 1mL 100mM (ph 6.0) <3 1 2mL/min 3mL 2mL 100mM HCl 3mL ( >10 5 ) 3mL /IPA/NH 4 OH (78:20:2) 1 2mL/min IPA/NH 4 OH (ph 11-12) <40 50µL 50µL BSTFA** ( 1% TMCS)*** / 70 20 BSTFA 1 2µL (GC/MS) ** D 3 - * 185 201 306 182 198 303 D 3 - -TMS* 243 259 364 -TMS 240 256 361 * ** ** TS-38831 10 x 1mL GC TRACE TR-DoA5 15m 0.25mm 0.25µm TRACE TR-DoA35 15m 0.20mm 0.33µm 26AF130P 26AC497P 160

GC GC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 2mL 0.5 1g 3mL 100mM (ph 6.0) 3mL 3mL 1mL 100mM (ph 6.0) <3 1 2mL/min 3mL 2mL 100mM HCl 3mL ( >10 5 ) 3mL /IPA/NH 4 OH (78:20:2) 1 2mL/min IPA/NH 4 OH (ph 11-12) 50µL 50µL BSTFA**( 1% TMCS***) / 70 20 BSTFA 1 2µL (GC/MS) ** D 3 - * 185 201 306 182 198 303 D 3 - -TMS* 243 259 364 -TMS 240 256 361 * ** ** TS-38831 10 x 1mL GC TRACE TR-DoA5 15m 0.25mm 0.25µm TRACE TR-DoA35 15m 0.20mm 0.33µm 26AF130P 26AC497P 161

Delta 9-THC Delta 9-THC -Delta-9-THC 200mg 6mL HyperSep Verify-CX ( 60108-730) 1 2mL * 2mL ACN ACN ACN 200µL 2mL (ph~6.0-7.0) ACN 1mL (84/15/1) /ACN/NH 4 OH 1 x 3mL / / (49:49:2) 1 2mL/min <40 50µL / 50µL BSTFA 1% TMCS *** 70 20 BSTFA 2µL GC/MS BSTFA 371 343 386 (374,346,389) * GC/MS D9- -delta 9-THC D3- - delta 9-THC D3-delta 9-THC ** delta-9 THC *** TS-38831 371 459 474 (374,462,477) 371 473 488 (380,479,497) GC TraceGOLD TG-35MS 30m 0.25m 0.25µm 26096-1420 162

DHEA GC GC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 5mL * ph 5.5-6.5 3,000rpm 5 3mL 3mL 1mL 100mM (ph 6.0) 3mL >10 10 3mL 1 2mL/min 2mL 0.2M (ph 7.0) 250 - / 50 1 1:1 NaHCO 3 / Na 2 CO 3 ph 10-11 5mL n- 10 3000rpm 5 30 50µL MSTFA***/NH l/ (1000:2:5, 4 v/w/w) 70 20 3000rpm 1 GC 1 2µL ** 432 417 432 417 DHEA 432 417 16 * 520 259 * GC/MS 20ng/mL ** *** TS-48910(10 x 1mL ) GC TRACE TR-DoA5 15m 0.25mm 0.25µm TRACE TR-DoA35 15m 0.20mm 0.33µm 26AF130P 26AC497P 200mg 10mL HyperSep Verify-CX ( 60108-742) 1mL 100mM (ph= 6) * 1mL 2mL 100mM (ph= 6) / ph 6.0 0.5 100mM ph / 1 x 3mL 1 x 3mL 1 x 1mL 100mM (ph= 6) <3 1 2mL/min 1 x 3mL 1 x 3mL 100mM 1 x 3mL ( >10 5 ) 1 x 3mL / / (78:20:2 v/v) 1 2mL/min <40 200µL 0.1% 5µL LC/MS * 314.2/152.2 298.1/44.1 * 163

GC GC/MS 100mg 1mL HyperSep C18 ( :60108-302) 500µL * 500µL20% 3mL 3mL 1 ml 100mM HCI <3 1 2mL/min 3mL 3mL 3mL ( >10 5 ) 1mL2% <40 50µL 50µL BSTFA( 1% MCS)** 50µL MTBSTFA( 1% TMCS)** 50µL 70 30 1 2µL : ** 210 225 182 -D10* 220 235 192 * ** TS-38831(10 x 1mL ) *** TS-48927(10 x 1mL ) GC TRACE TR-DoA5 15m 0.25mm 0.25µm TRACE TR-DoA35 15m 0.20mm 0.33µm 26AF130P 26AC497P Wolf, C.E. II, Sady J., and Pokalis, A. (1996). Determination of gabapentin in serum using solid phase extraction and gas chromatography. Journal of Analytical Toxicology.20.498-501 GC GC/MS 200mg 10mL HyperSep Verify-CX ( :60108-742) 2mL * 1mL - - :100mM (ph 5.0) 5,000 F /ml Patella Vulgata / 65 3 2,000rpm 10 3mL 3mL 1mL 100mM (ph 6.0) <3 1 2mL/min 3mL 2mL 20% 100mM (ph= 6.0) ( >10 5 ) 2mL 7-3mL 2% NH 4 OH 1 2mL/min <40 50µL 50µL MTBSTFA( 1 % TBDMCS)** / 70 20 M BS FA 1 2µL : ** 312 286 266 7 283 255 254 356 357 310 D 5 * 462 464 463 * ** *** TS-48927(10 x 1mL ) GC TRACE TR-DoA5 15m 0.25mm 0.25µm TRACE TR-DoA35 15m 0.20mm 0.33µm 26AF130P 26AC497P 164

Gamma-(GHB) 200mg 6mL Retain-AX ( 60107-412) GHB 200µg/mL GHB - D6 100µg/mL 10µL 200µL 10µg/mL 25µL 200µL 25µg/mL 50µL 200µL 50µg/mL 100µL 200µL 100µg/mL 200µL QC 1.5mL 25µL * 1mL / 15 70 N 2 200µL 100mM (ph 6.0) / 15 1 x 3mL 1 x 3mL 1 x 1mL 100mM (ph 6.0) Eppendorf 1mL /NH 4 OH (99:1) / 1 N 70 2 100µL 100 L BSTFA( 1% TMCS**) / 70 30 1 2µL GC/MS * GHB-D6-di-TMS* 239 240 241 GHB-di-TMS 233 234 235 * GC/MS D6-GHB ** TS-38831 GC TraceGOLD TG-35MS 30m 0.25m 0.25µm 26094-1420 200mg 6mL HyperSep Retain-CX ( 60107-314) 1mL 100mM (ph 6) * 1mL 2mL 100mM (ph 6) / 1 x 3mL 1 x 3mL 1 x 1mL 100mM (ph 6) <3 1 2mL/min 1 x 3mL 1 x 3mL 100mM 1 x 3mL ( >10 10 ) 1 x 3mL ACN (78:20:2) 1 2mL/min <40 50µL 5µL LC/MS * -D3 MRM PCP 244.3/159.2 PCP-D5 249.3/264.1 272.1/128.1 -D3* 275.1/131.0 HPLC Hypersil GOLD 3µm 150 4.6mm 25003-154630 165

Gamma- (GBL) Gamma(GHB) 200mg 6mL Retain-AX ( 60107-412) 200µL * 100µL 100mM ( ph 6.0 ) / 1 x 3mL 1 x 3mL 1 x 1mL 100mM (ph= 6.0) 1 1mL /NH 4 OH (99:1) / N 2 60 200µL 1mL 5 3,000rpm 5 N <50 2 100µL 100µL BSTFA( 1% TMCS)** / 1 2µL GC/MS * GHB-D6-di-TMS* 239 240 241 GHB-di-TMS 233 234 235 * GC/MS D6-GHB ** TS-38831 GC TraceGOLD TG-35MS 30m 0.25m 0.25µm 26094-1420 /GC GC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 1mL 100mM (ph 6.0) * 1 2mL / / 2mL 100mM (ph 6.0) ph 6.0 0.5 100mM ph Verify-CX 3mL 3mL 1mL 100mM (ph 6.0) < 3 1 2mL/min 3mL 3mL 100mM 3mL ( >10 5 ) 3mL /IPA/NH 4 OH (78:20:2) 1 2mL/min IPA/NH 4 OH (ph 11-12) <40 100µL 1 2µL * D 4 - * 184 213 156 180 209 152 * ** GC TRACE TR-DoA5 15m 0.25mm 0.25µm TRACE TR-DoA35 15m 0.20mm 0.33µm 26AF130P 26AC497P 166

//LC/MS/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 1mL 100mM (ph 6.0) * 1mL / 2mL 100mM (ph 6.0) / 3mL 3mL 1mL 100mM (ph 6.0) < 3 1 2mL/min 3mL 1mL 100mM 3mL ( >10 5 ) 3mL /IPA/NH 4 OH (78:20:2) 1 2mL/min IPA/NH 4 OH (ph 11-12) <40 100µL 5µL LC/MS/MS * MRM 333.2/188.3 - D 5 * 342.3/188.2 233.2/84.1 - D 5 * 238.3/84.1 0.1% (50:50, v/v) 0.35mL/min HPLC Hypersil GOLD PFP 3µm 150 2.1mm 25403-152130 HPLC 200mg 10mL HyperSep Verify-CX ( 60108-742) 1mL * 2mL 100mM (ph 6.0) / 2,000rpm 10 ph 6.0 0.5 100mM ph 3mL 3mL 1mL 100mM (ph 6.0) < 3 1 2mL/min 3mL 1mL 100mM 3mL ( >10 5 ) 3mL /IPA/NH 4 OH (78:20:2) 1 2mL/min IPA/NH 4 OH (ph 11-12) <40 200µL (1:3) / 30 30 A 0.1% B:ACN + 0.1% 15 B 30% 50% 1mL/min (254nm) HPLC Hypersil GOLD 5µm 150 4.6mm 25005-154630 167

(LSD) GC GC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 1mL 4mL * / 5 2,000rpm 10 2mL 100mM (ph 6.0) / ph 6.0 0.5 100mM ph 3mL 3mL 1mL 100mM (ph 6.0) < 3 1 2mL/min 3mL 3mL 100mM 3mL ( >10 5 ) 3mL /IPA/NH 4 OH (78:20:2) 1 2mL/min IPA/NH 4 OH (ph 11-12) <40 20µL 20µL BSTFA**( 1% TMCS)*** / 70 30 BSTFA 1 2µL * D 3 -LSD-TMS* 298 296 271 LSD-TMS 395 293 268 * ** ** TS-38831(10 x 1mL ) GC TRACE TR-DoA5 15m 0.25mm 0.25µm TRACE TR-DoA35 15m 0.20mm 0.33µm 26AF130P 26AC497P 168

(LSD) GC GC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 5mL 2mL 100mM ( ph6.0 ) / ph 6.0 0.5 100mM ph 3mL 3mL 1mL 100mM (ph 6.0) <3 1 2mL/min 3mL 3mL 100mM 3mL ( >10 5 ) 3mL /IPA/NH 4 OH (78:20:2) 1 2mL/min IPA/NH 4 OH (ph 11-12) <40 20µL 20µL BSTFA** ( 1% TMCS)*** / 70 20 BSTFA 1 2µL * D 3 -LSD-TMS* 298 296 271 LSD-TMS 395 293 268 * ** ** TS-38831 10 x 1mL GC TRACE TR-DoA5 15m 0.25mm 0.25µm TRACE TR-DoA35 15m 0.20mm 0.33µm 26AF130P 26AC497P (SPE - HPLC) 30mg 1mL HyperSep Retain- PEP ( 60107-201) 1mL 1mL 1mL, 20µL 1mL 5% 1mL 50:50 HPLC (1) 11-Ketotestosterone (2) (3) (4) Hypersil GOLD 5µm, 150 x 4.6 mm 25005-154630 /, 43/57 1 ml / min 10µL 254 nm 25 169

LSD 200mg 3mL HyperSep Aminopropyl ( 60108-425) 1mL 100mM (ph 6) * 1mL / 2mL 100mM (ph 6) / 1 x 3mL 1 x 3mL 1 x 1mL 100mM (ph 6) 1 2mL/min 1 x 3mL 1 x 3mL 100mM 1 x 3mL ( >10 5 ) 1 x 3mL ACN (78:20:2 v/v) 1 2mL/min 50µL 5µL GC/MS ACN 0.1 0 30 70 3.0 90 10 3.1 30 70 5.0 30 70 0.5mL/min :Thermo Scientific TSQ MRM LSD 324.2/223.1 lso-lsd 324.2/281(223.1) Nor-LSD 310.2/209.1 OH-LSD 356.2/338.1 LSD-D3* 327.2/226.1 * LSD-D3 >90% (N=10) 0.1ng/mL HPLC Hypersil GOLD PFP 3µm 100 2.1mm 25403-102130 200mg 3mL HyperSep Aminopropyl ( 60108-425) 1mL 100mM (ph 6) * 1mL / 2mL 100mM (ph 6) / 1 x 3mL 1 x 3mL 1 x 1mL 100mM (ph 6) < 3 1 2mL/min 1 x 3mL 1 x 3mL 100mM 1 x 3mL >10 5 1 x 3mL ACN (78:20:2 v/v) 1 2mL/min 50µL 5µL GC/MS ACN 0.1 0 90 10 5 30 70 6 90 10 10 90 10 0.35mL/min :Thermo Scientific TSQ MRM 248.2/220.0 - D4 * 252.2/224.1 234.1/160.0 - D4 * 238.1/164.0 * -D4 -D4 >90% (n=10) 10ng/mL HPLC Hypersil GOLD 3µm 150 2.1mm 25003-152130 170

/( ) GC GC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 1mL 100mM (ph 6.0) * 1mL / 1g (1:4) / 5 2mL 100mM (ph 6.0) / ph 6.0 0.5 100mM ph 2,000rpm 10 3mL 3mL 1mL 100mM (ph 6.0) < 3 1 2mL/min 3mL 3mL 100mM (ph 4.5) 3mL ( >10 5 ) 3mL /IPA/NH 4 OH (78:20:2) 1 2mL/min IPA/NH 4 OH (ph 11-12) <40 50µL 50µL BSTFA ( 1% TMCS)*** / 70 30 BSTFA 1 2µL ** - D3 - TMS * 374 237 346 - TMS 371 234 343 - D3 - TMS * 432 290 327 - TMS 429 287 324 * ** *** TS-38831(10 x 1mL ) GC TRACE TR-DoA5 15m 0.25mm 0.25µm TRACE TR-DoA35 15m 0.20mm 0.33µm 26AF130P 26AC497P 171

/ /EDDP GC GC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 1mL 100mM (ph 6.0) * 1mL / 1g (1:4) 2mL 100mM (ph 6.0) ph 6.0 0.5 100mM ph / 3mL 3mL 1mL 100mM (ph 6.0) < 3 1 2mL/min 3mL 1mL 100mM 3mL ( >10 5 ) 3mL / / (78:20:2, v/v/v) 1 2mL/min <40 100µL 5µL GC/MS * ( ) % 0.1% 0 25 75 5 25 75 14 90 10 15 25 75 20 25 75 0.35mL/min MRM 310.2/105.1 -D9* 319.2/268.3 EDDP 278.2/234.2 EDDP-D3* 281.4/234.3 HPLC Hypersil GOLD aq 3µm 150 2.1mm 25303-152130 172

GC GC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 2mL * 1mL 100mM ( ph 6. 0 ) / ph 6.0 0.5 100mM ph 3mL 3mL 1mL 100mM (ph 6.0) < 3 1 2mL/min 3mL 1mL 100mM 3mL ( >10 5 ) 3mL /IPA/NH 4 OH (78:20:2) 1 2mL/min IPA/NH 4 OH (ph 11-12) <40 100µL 1 2µL ** D 9 - * 78 226 303 72 223 294 * ** GC TRACE TR-DoA5 15m 0.25mm 0.25µm TRACE TR-DoA35 15m 0.20mm 0.33µm 26AF130P 26AC497P / GC GC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 2mL / * 1mL 100mM (ph 6.0) / 2mL 100mM (ph 6.0) / ph 6.0 0.5 100mM ph 3mL 3mL 1mL 100mM (ph 6.0) < 3 1 2mL/min 3mL ( >10 5 ) 2mL 3mL / (50:50) <40 100µL 1 2µL ** 235 250 233 * 221 157 156 - D7 * 240 257 240 * ** GC TRACE TR-DoA5 15m 0.25mm 0.25µm TRACE TR-DoA35 15m 0.20mm 0.33µm 26AF130P 26AC497P 173

/ LC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 1mL100mm (PH 6.0) * 1mL / 2mL 100mm (PH 6.0) Verify-CX 3mL 3mL 1mL100mm (PH 6.0) : <3 1 2mL/min 3mL ( >10 5 ) 2mL 3mL / (50:50) 1 2mL/min <40 100µL 5µL GC/MS : MRM 251.2/132.1 -D7* 258.2/138.2 * : 0.1 % (30:70,v/v) :0.35mL/min GC GC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 2mL * 2mL100mm (ph 6.0) ph 6.0 0.5 100mm ph / Verify-CX 3mL 3mL 1 ml 100mm (ph 6.0) : <3 1 ZmL/min 3mL 2mL200mm HCI ( >10 5 2mL 3mL ( >10 5 3mL /IPA/NH 4 0H (78:20:2) 1 2mL/min : ; IPA/NH 4 0H (ph 11-12) <40 100µL 1 2µL (GC/MS) ** 84 133 162 -D4* 88 137 166 98 119 176 -D3* 101 122 179 * D,- D 4 - ** GC TRACE TR-DoA5 15m x 0.25mm x 0.25µm 26AF130P TRACE TR-DoA35 15m x 0.20mm x 0.33µm 26AC497P 174

GC GC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 2mL 400µL HCI 200µL 10% / 90 40 15 2,000rpm 10 500µL 50% / 50% ph 5-6 2mL / 60 ( ) 200µL 10% 60 30 ph 5-6 2,000rpm 10 Verify-CX 3mL 3mL 1mL 100mm (ph 6.0) : <3 1 2mL/min 3mL 3mL 100mm (ph 4.5) 3mL ( >10 5 ) 3mL /IPA/NH 4 0H (78:20:2) 1 2mL/min : ; IPA/N H 4 0H (ph 11-12) <40 100µL 100µL BSTFA ( 1%TMCS)*** / 70 45 : BSTFA 1 2µL : ** D 4 - * 251 222 250 247 218 246 D 4 - TMS* 308 280 309 TMS* 305 276 304 TMS 335 245 290 0- TMS 393 378 303 N- TMS 393 378 116 TMS 357 342 289 D 3 - TMS* 374 359 346 D 6 - TMS* 377 349 316 TMS 371 356 343 TMS 429 414 356 TMS 373 315 358 D 3 - TMS* 432 417 404 D 6 - TMS* 435 420 404 TMS 429 414 401 TMS 487 472 414 369 327 268 D 3 - TMS 389 300 374 D 6 - TMS* 392 303 377 TMS 386 297 371 D 3 - TMS 447 432 358 TMS 444 429 355 D 3 - TMS 477 462 420 D 6 - TMS* 480 465 420 TMS 474 459 417 D 3 - TMS 535 520 290 TMS 532 517 287 * GC/MS D 6 - D 6 - L0D/L0Q ** *** TS38831(10x 1mL ) GC TRACE TR-DoA5 15m x 0.25mm x 0.25µm TRACE TR-DoA35 15m x 0.20mm x 0.33µm 26AF130P 26AC497P 175

- GC GC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) - 2mL 400µL HCI 200µL 10% / 90 40 15 2,000rpm 10 500µL 50% / 50% ph 5-6 - 2mL * 1mL - ( - 5000F /ml) 60 3 2,000rpm 10 1.0 M Na0H ph 5-6 Verify-CX 3mL 3mL 1 ml 100mm (ph 6.0) : <3 1 2mL/min 3mL 3mL100mm (ph 4.5) 3mL ( >10 5 ) 3mL /IPA/NH 4 0H (84:12:4) 1 2mL/min : ; IPA/NH 4 0 H (ph 11-12) <40 200µL 1:1 : / 60 60 <40 50µL / (70:30, v/v) 1 2µL : ** 299 242 214 355 282 229 -D3* 358 285 232 371 314 298 285 341 228 6-327 268 383 357 300 413 341 268 397 -D3* 344 271 400 * GC TRACE TR-DoA5 15m x 0.25mm x 0.25µm 26AF130P TRACE TR-DoA35 15m x 0.20mm x 0.33µm 26AC497P 176

/ LC/MS/MS 200mg 10mL HyperSep Verify-CX ( :60108-742) 1mL 100mm (ph 6.0) * 1mL / 2mL 100mm (ph 6.0) Verify-CX 3mL 3mL 3mL 100mm (ph 6.0) : <3 1 2mL/min 3mL 3mL 100mm 3mL ( >10 5 ) 3mL / / (78:20:2,v/v/v) 1 2mL/min <40 100µL 5µL GC/MS/MS : MRM 330.0/190.1 -D6* 336.0/76.1 * : ( ) % % 0.1% 0 10 90 15 50 50 16 10 90 20 10 90 0.35mL/min HPLC Hypersil GOLD Phenyl 3µm, 150 x 2.1 mm 25903-152130 30mg 3mL HyperSep Retain-CX ( :60707-302) 1mL 1mL 100mM (ph 6.0) / HyperSep Retain-CX 1 ZmL/min 1x1mL 1 x 1 ml 100mm 1x1mL ( >10 3 ) 2 x 0.5mL /IPA/NH 4 0H(78/20/2) 1 ZmL/min 1 1% <40 100µL 1 2µL GC/MS : ( ) 200 91 242 -D5* 205 96 247 * -D5 GC TraceGOLD TG-5SiIMS 30m x 0.25mm x 0.25µm 26096-1420 177

/ GC GC/MS 200mg 10mL HyperSep Verify-CX ( :60108-742) 1mL 100mm (ph 6.0) * 1mL / 1g (1:4) / ph 6.0 0.5 100mm ph Verify-CX 3mL 3mL 1 ml 100mm (ph 6.0) : <3 1 2mL/min 3mL 3mL 100mm 3mL ( >10 5 ) 3mL /IPA/NH 4 0H (78:20:2) 1 2mL/min : ; IPA/NH 4 0H (ph 11-12) <40 100µL 1 2µL. : ** D5- * 205 96 247 205 96 247 200 91 242 200 91 242 * ** GC TRACE TR-DoA5 15m x 0.25mm x 0.25µm TRACE TR-DoA35 15m x 0.20mm x 0.33µm 26AF130P 26AC497P / GC/MS 200mg 10mL HyperSep Verify-CX ( :60108-742) 1mL 100mm (ph 6.0) * 1mL / 2mL 100mm (ph 6.0) / ph 6.0 0.5 100mm ph / Verify-CX 3mL 3mL 1 ml 100mm (ph 6.0) : <3 1 2mL/min 3mL 3mL 100mm 3mL ( >10 5 ) 3mL / / (78:20:2,v/v/v) 1 2mL/min : <40 100µL 5µL GC/MS/MS : MRM 330.0/190.1 -D6* 336.0/76.1 * : /0.1% (33:67,v/v) :0.35mL/min : HPLC Hypersil GOLD 3µm, 150 x 2.1 mm 25003-152130 178

/ GC GC/MS 200mg 10mL HyperSep Verify-CX ( :60108-742) 1mL 100mm (ph 6.0) * 1mL / 2mL 1g (1 :4) / p 6.0 0.5 100mM ph Verify-CX 3mL 3mL 1 ml 100mm (ph 6.0) : <3 1 2mL/min 3mL 3mL 100mm 3mL ( >10 5 ) 3mL /IPA/NH 4 0H (78:20:2) 1 2mL/min : ; }PA/N H40 H (ph 11-12/ <40 100µL 1 2µL : ** D5- * 63 120 213 255 270 58 115 208 250 265 * ** : ( ) 1 35% ph 6 SP ( ) GC TRACE TR-DoA5 15m x 0.25mm x 0.25µm TRACE TR-DoA35 15m x 0.20mm x 0.33µm 26AF130P 26AC497P / LC/PDA 200mg 10mL HyperSep Verify-CX ( :60108-742) 1mL 100mm (ph 6.0) * 1mL / 1g(1:4) 2mL100mm (ph 6.0) ph 6.0 0.5 100mm ph Verify-CX 3mL 3mL 1 ml 100mm (ph 6.0) : <3 1 2mL/min 3mL 3mL 100mm 3mL ( >10 5 ) 3mL ( >10 5 ) 3mL / / (78:20:2, v/v/v) 1 2mL/min : <40 100µL 0.1% ( ) 50µL LC/MS/MS : * * :1 ml/min : : 0.1% (25:75) : (250nm) HPLC Hypersil GOLD 3µm, 150 x 4.6 mm 25003-154630 179

/ LC/MS/MS 200mg 10mL HyperSep Verify-CX ( :60108-742) 1mL 100mm (ph 6. ) 1mL / 1g}1:4) 2mL 100mM (ph 6.0) Verify-CX 3mL 3mL 1 ml 100mm (ph 6.0) : <3 1 2mL/mi 3mL 3mL 100mm 3mL ( >>1 5 ) / 3mL / / (78:20:2,v/v/v) 3mL /IPA/NH 4 0H(78:20:2,v/v/v) 1 2mL/mi : ; IPA/NH 4 0H (ph11-12) <400C 100µL 0.1% / <40 100µL 5µL LC/MS/MS : MRM 340.0/58.0 -D11* 351.2/64.0 326.0/252.0 -D5* 331.0/257.0 0.35mL/min : ( ) % % 0.1% 0 30 70 10 30 70 HPLC Hypersil GOLD Phenyl 3µm, 50 x 2.1 mm 25903-052130 (SPE-LC/MS ) 30mg 3mL HyperSep Retain-CX ( :60707-302) : 1mL 1mL 1 ml 30mm : 1mL 0.5% : 1mL 1mL : 1mL5% LC/MS : Hypersil GOLD 3µm, 50 x 2.1 mm : 25003-052130 : 100mm : =70:30 : 200µL/min MS : (ESI) (SRM) 4500V 350 : : 97-99% 180

-4- GC GC/MS 200mg 10mL HyperSep Verify-CX ( 60108-742) 5mL *( -4- -D10-TMS) 2mL 100mm (ph 6.0) / 12,500 25,000 b- / 45 90 3,000rpm 10 ( ) SPE Verify-CX 3mL 3mL 1mL100mm (ph 6.D) : <3 1 2mL/min 3mL 2mL 20% 1 ml 100mm ( >10 3 ) 2mL 3mL / (50:50) 3mL ( >10 3 ) -4-3mL /IPA/NH 4 0H (78:20:2) 1 2mL/min : ; }PA/N QOH (ph 11-12) <35 5µL / 5µL MSTFA*** 70 30 : MSTFA 1 2µL : ** -4- -TMS 290 348 73(291) -4- -D10-TMS* 300 258 83(301) * ** TS-48910 ( 10x1mL ) GC TRACE TR-DoA5 15m x 0.25mm x 0.25µm TRACE TR-DoA35 15m x 0.20mm x 0.33µm 26AF130P 26AC497P Greishaber A. Moore, K. Levine, B, and Smith M.(1999, Novembe). The detection of psilocin in human urine. Presented at the TRI Services Meeting 181

( ) 200mg 10mL HyperSep Verify-CX ( 60108-742) 1mL 4mL (ph 5 7) / 5 2,000rpm 10 2mL 100mm (ph 6.0) / ph 6.0 0.5 100mm ph Verify-CX 3mL 3mL 1 ml 100mm (ph 6.0) : <c3 1 2mL/min 3mL 3mL ( >10 5 ) 2mL 3mL / (50:50) <5mL/min 3mL ( >10 5 ) 3mL /IPA/NH 4 0H (78:20:2) 1 2mL/min : ; IPA/NH 4 0H (ph 11-12) <40 100µL 90µL ( 1.0mL) H PLC 200mg 10mL HyperSep Verify-CX ( :60108-742) 4mL 2mL 100mm (ph 6.0) 1mL / / 2,000rpm 10 ph 6.0 0.5 100mm ph Verify-CX 3mL 3mL 1 ml 100mm (ph 6.0) : <3 1 2mL/min 3mL 1 ml 100mm 3mL ( >10 5 ) 3mL /IPA/NH 4 0H (78:20:2) 1 2mL/min : ; IPA/N H 4 0H (ph 11-12) <40 200µL : (1:3) / 30 10µL LC 235nm : 30% 0.25 M (ph 2.7) :2mL/min HPLC Hypersil GOLD C8 3µm, 150 x 4.6 mm 25203-154630 182

-4-200mg 10mL HyperSep Verify-CX ( 60108-742) 1 ml 100mm (ph 6) 1mL 2mL 100mm (ph 6) / 1mL 1mL (p :100mm (ph=5.0) 5.000 F /ml Patella Vulgata) / 65 3 2,000rpm 10 HyperSep Verify-CX 1x3mL 1x3mL 1 x 1 ml 100mm (ph 6) : <3 1 2mL/min 1x3mL 1 x 3mL 100mm 1x3mL ( >10 5 ) 1x3mL ;ACN; (78:20:2 v/v) 1 2mL/min 5µL 5µL GC/MS : %ACN 0.1% 0 20 80 5 20 80 0.20mL/min :Thermo Scientific TSQ MRM -4-205.2/58.2-4- -D10* 215.2/68.2 * -4- -D10 >90% (n=10) :10ng/mL HPLC Hypersil GOLD PFP 3µm, 100 x 2.1 mm 25403-102130 (SPE-HPLC) 200mg 10mL HyperSep Verify-CX ( 60108-742) : 1mL 1mL2% : 1mL 2% : 1mL2% 1mL : 1mL 5% : : 72%-98% HPLC : Hypersil GOLD 5µL, 150 x 4.6mm : 25005-54630 : A.0.05M ph3; B: (85:15) : 1 ml/min t: 10µL UV; 210nm : 20 183

/ GC GC/MS PFPA (PFAA) - 200mg 10mL HyperSep Verify-CX ( :60108-742) 1mL100mm (ph 6.0) * 1mL / 1g(1:4) / ph 6.0 0.5 100mm ph Verify-CX 3mL 3mL 1 ml 100mm (ph 6.0) : <3 1 2mL/min 3mL 1 ml 100mm 3mL ( >10 5 ) SMA 3mL /IPA/NH 4 0H (78:20:2) 1 2mL/min : ; IPA/NH 4 0H (ph 11-12) 30µL DMF*** <40 30µL PFPA (PFAA) - 50µL PFPA(PFAA)**** 50µL PFPOHt 70 20 <40 100µL 1 2µL : ** D 5 - * 194 92 123 190 91 118 D 5 - * 208 92 163 204 91 160 204 160 119 204 160 119 190 119 267 135 162 325 204 162 339 * GC/MS D 5 - D 5 - ** *** TS-20672(50mL ) *** TS-65193(10x1mL ) *** TS-65195(10x1mL ) GC TRACE TR-DoA5 15m x 0.25mm x 0.25µm TRACE TR-DoA35 15m x 0.20mm x 0.33µm 26AF130P 26AC497P 184

/ GC GC/MS TMS - 200mg 10mL HyperSep Verify-CX ( :60108-742) 2mL * 1 ml 100mm (ph 6.0) / ph 6.0 0.5 100mm ph Verify-CX 3mL 3mL 1mL 100mm (ph 6.0) : <3 1 2mL/min 3mL 1 ml 100mm 3mL ( >10 5 ) SMA 3mL /IPA/NH 4 0H (78:20:2) 1 2mL/min : ; IPA/N H 4 0H (ph 11-12) 3µL DMF <40 30µL TMS - 50µL BSTFA( 1 % TMCS) 5µL 70 45 1 2µL : ** D 5 - * 120 197 92 D 6 - * 120 198 93 D 10 - * 120 202 97 D 11 - * 120 203 98 116 192 91 D 5 - * 134 211 92 D 8 - * 137 214 92 D 9 - * 137 215 93 130 206 91 130 147 294 130 147 294 116 236 135 130 250 131-116 222 121 * GC/MS ** *** TS-20672(50mL ) *** TS-38831(10x1mL ) GC TRACE TR-DoA5 15m x 0.25mm x 0.25µm 26AF130P TRACE TR-DoA35 15m x 0.20mm x 0.33µm 26AC497P 185

/ GC GC/MS - 4-CB(4- ) 200mg 10mL HyperSep Verify-CX ( :60108-742) 2mL * 1 ml 100mm (ph 6.0) / ph 6.0 0.5 100mM ph Verify-CX 3mL 3mL 1 ml 100mm (ph 6.0) : <c3 1 2mL/min 3mL 1 ml 100mm 3mL ( >>10 5 ) SMA 3mL /IPA/NH 4 0H (78:20:2) 1 2mL/min : ; IPA/NH 4 0H (PH11-12) 30µL DMF*** <40 30µL 4-CB(4- ) - 20µL 4-CB 00µL 70 45 1 2µL : (4-CB) ** D 5 - * 298 270 399 294 266 248 D 5 - * 312 284 266 308 280 262 D 5 - * 136 434 270 162 429 266 D 5 - * 312 284 266 308 280 262 D 6 - * 328 165 300 322 162 294 * ** *** TS-20672(50mL ) GC TRACE TR-DoA5 15m x 0.25mm x 0.25µm TRACE TR-DoA35 15m x 0.20mm x 0.33µm 26AF130P 26AC497P (cs), (CN) ((0C) GC/MS 200mg 10mL HyperSep Verify-CX ( :60108-742) Kimwipe Verify-CX 3mL 3mL 1 ml 100mM (ph 6.0) : : <3 <3 1 ml/mi 3mL 3mL ( >10 5 ) 1mL <40 200µL / GC/MS 1 2 186

/ / GC GC/MS 200mg 10mL HyperSep Verify-CX ( :60108-742) : 2mL 1 ml 100mm (ph 6.0) / ph 6.0 0.5 100mm ph : 1mL * 1mL (ph 6.0) 4mL / 5 2,000rpm 10 2mL 100mm (ph 6.0) / ph 6.0 0.5 100mm ph Verify-CX 3mL 3mL 1 ml 100mm (ph 6.0) : <3 1 2mL/min 3mL 1mL100mm ( >10 5 ) 2mL ( 1 ) 3mL / (50:50) <2mL/min <40 100µL 1 2µL 3mL ( >10 5 ) ( 2 ) 3mL /IPA/NH 4 0H (78:20:2) 1 2mL/min : ; IPA/NH 4 0H (PH 11-12) <40 100µL 1 2µL GC TRACE TR-DoA5 15m x 0.25mm x 0.25µm 26AF130P TRACE TR-DoA35 15m x 0.20mm x 0.33µm 26AC497P : (1) 1 ( ) 2 ( ) (2) ( DMF) ; 30 50µm DMF( 2 ) (3) 1% 2 100µm 1 187

60mg 6mL HyperSep Retain-CX ( 60107-308) 100 50µL 10 800µL 100mm (ph= 6.0) / 10 PH 6.0 0.5 100mm ph HyperSep Retain-CX 1 x 200µL 1x200µL 1 x 200µL 100mm (ph=6.0) 1 ml/min 1 x 500µL 1 x 500µL 100mm 1 x 500µL ( >10 5 ) 1 x 800µL /IPA/NH 4 0H (70:26:4) 1 ml/min : ; IPA/NH 4 0H (ph 11-12) PCP 5 100µL 5% 5 <40 *: 50µL PFPA(PFAA) / 70 20 <40 50µL : 200µL 1:1 / / 40 60 <40 50 1 2µL * GC/MS 50mg 1mL HyperSep Verify-CX ( :60108-741) 100 50µL 10 800µL 100mm (ph 6.0) / ph 6.0 0.5 100mm ph Verify-CX 200µL 200µL 200µL 100mm (ph 6.0) 1mL/min ( ) 500µL 500µL 100mm 500µL ( >10 5 800µL /IPA/NH 4 0H (70:26:4) 1mL/min ( ) : ; IPA/N H 4 0H (ph 11-12) PCP 5 10µL 5% (5 ) <40 *: 50µL PFPA(PFAA)** 70 20 <40 50µL * 200µL 1:1 PFPA(PFAA)** (10x1mL TS-65193) 40 60 50µL 1 µl * ** TS-65193(10X1ML ) : GC TRACE TR-DoA5 15m x 0.25mm x 0.25µm TRACE TR-DoA35 15m x 0.20mm x 0.33µm 26AF130P 26AC497P 188

60mg 6mL HyperSep Retain-CX ( 60107-308) 100 500µL * 10 800µL 100mm (ph=6.0) / 10 ph 6.0 100mm ph HyperSep Retain-CX 1 x 200µL 1 x 200µL 1 x 200µL 100mm HCI 1mL/min 1 x 500µL 1 x 500µL 100mm 1 x 500µL / (50:50) ( >10 5 ) 1 x 800µL /IPA/NH 4 0H (70:26:4) 1mL/min : ; IPA/NH 4 0H (ph 11-12) <40 : 100µL PFPA (PFAA) HFIP 70 20 <40 50µL TMS: 25µL BSTFA( 1 % TMCS)** 25µL / 70 30 : BSTFA 2µL GC/MS : MRM 182 198,303 -D3* 185 201,306 -TMS 240 256,361 -D8-TMS* 243 259,369 * -D3 -D8-TMS ** TS-3B831 HPLC Hypersil GOLD TG-5MS 30mx0.25m x0.25µm 26098-1420 189

/ 200mg 10mL HyperSep Verify-CX ( :60108-742) 0 1 5 10ng / 100µL / 30 15 200µL (ph 6) * 1 100µL 10 3µL 100mm (ph 6) / HyperSep Verify-CX 1x3mL 1x3mL 1 x 1µL 100mm (ph 6) : <3 1 2mL/min 1x3mL 1x3mL1% 1x3mL ( >10 5 ) 1x3mL ACN; (78:20:2 v ) 1 2mL/min <<400C 2 L 5 LC/MS MRM 333.2/188.3 -D5* 342.2/188.2 233.2/84.1 -D5* 238.3/84.1 * -D5 -D5* HPLC Hypersil GOLD aq 5µm, 50 x 3mm 25305-053030 (THC) GC/MS 200mg 10mL HyperSep Verify-CX ( :60108-742) 1mL 50ng/mL (THCA D9-TMS) 10 10 0.5mL 10 Verify-CX 3mL 3mL 1mL 0.1N HCI 1 ml/min ( ) 2mL 2mL 0.1N HCI/ (70:30) ( >10 5 ) 200µL THC 2mL / (50:50) 1 ml/min ( ) <40 50µL MSTFA*** 10 60 20 10 50µL 1 2µL : ** THCA-TMS 371 386 387 THCA D9-TMS* 380 479 * ** *** TS-48910 ( 10x1mL ) GC TRACE TR-DoA5 15m x 0.25mm x 0.25µm TRACE TR-DoA35 15m x 0.20mm x 0.33µm 26AF130P 26AC497P Janet Putnam, Assistant Laboratory DirectorlRP Advanced Toxicology Network, Memphis, TN 190

GC/MS 50mg 1 ml HyperSep Verify-CX ( 60108-741) 100 500µL 800µL 100mm (ph 6.0) / 10 ( ph 6.0 0.5) 100mm ph Verify-CX 200µL 200µL 200µL 0.1N HCI 1 ml/min ( ) 500µL 500µL 100mm HCI 500µL / (50:50) ( >10 5 ) 800µL /IPA/NH 4 0H (70:26:4) 1mL/min ( ) : ; IPA/NH 4 0H (ph 11-12) <40 : 100µL PFPA (PFAA) HFIP 70 20 <40 50µL TMS: 25µL BSTFA( 1 % TMCS)** 25µL / 70 30 : BSTFA 1 2µL : ( ) 182 198 303 -D3* 185 201 306 240 256 361 -D8-TMS* 243 259 369 * ** TS-65193 10x1mL *** TS-38831 10x1mL GC TRACE TR-DoA5 15m x 0.25mm x 0.25µm TRACE TR-DoA35 15m x 0.20mm x 0.33µm 26AF130P 26AC497P 191

(THC) GC/MS 50mg 1mL HyperSep Verify-CX ( :60108-741) 100 500µL * 10 0.5mL / 10 Verify-CX 200µL 200µL 200µL 100mm HCI 1mL/min ( ) 500µL 500µL 0.2N HCI 500µL 100mm HCI/ (70:30) ( >10 5 ) THC 800µL / (75:25) 1mL/min ( ) <40 25µL BSTFA( 1 % TMCS}*** 25µL 70 30 : BS FA 1 2µL : ** THCA-TMS 371 386 303 THCA D9-TMS* 374 489 318 THC * ** *** TS-38831(10x 1mL ) GC TRACE TR-DoA5 15m x 0.25mm x 0.25µm TRACE TR-DoA35 15m x 0.20mm x 0.33µm 26AF130P 26AC497P THC 60mg 6mL HyperSep Retain-CX ( :60107-308) 100 500µL * 10 500µL / 10 Verify-CX 1x200µL 1x200µL 1x200µL 100mm HCI 1mL/min 1x500µL 1x500µL 0.2N HCI 1x500µL 100mm HCI/ACN(70:30) ( >10 5 ) 1X800µL : (25:75) 25µL BSTFA( 1 % TMCS}** 25µL / 70 30 : BSTFA 2µL GC/MS : ** THCA-TMS 371 386 303 THCA D3-TMS* 374 489 318 * THC-D3-TMS ** TS-38831 GC Trace GOLD TG-35MS 30m x 0.25m x 0.25µm 26094-1420 1mL/min <40 192

SOLA SPE 10mg/1 ml 10mg/2mL 96 SOLA SPE (ml) SOLA HRP 10mg 1mL 60109-001 100/ SOLA SCX 10mg 1mL 60109-002 100/ SOLA SAX 10mg 1mL 60109-003 100/ SOLA 96 (ml) SOLA HRP 10mg 2mL 60309-001 1/ SOLA SCX 10mg 2mL 60309-002 1/ SOLA SAX 10mg 2mL 60309-003 1/ SOLA SPE 1 SOLA SPE SOLA SPE 2 SOLA 30 SPE (i) SOLA. 3 SOLA 193

HyperSep SPE Thermo Scientific SPE HyperSepSPE 96- HyperSep SPE HyperSep MEPS 1mL 75mL 25mg 10g SPE 3.6µL HyperSep-96 HyperSep SPE 96 HPLC HPLC HyperSep Hypercarb HyperSep Hypercarb SPE 25mg 1mL 60106-304 50 / 50mg 1mL 60106-303 50 / 100mg 1mL 60106-302 30 / 200mg 3mL 60106-301 30 / 500mg 6mL 60106-402 20 / 1g 6mL 60106-403 10 / 2g 15mL 60106-404 10 / HyperSep Hypercarb SPE 50mg 1mL 60302-601 100 / 100mg 1mL 60302-602 100 / 200mg 1mL 60302-603 100 / 500mg 1mL 60302-606 1 1g 1mL 60302-607 1 2g 1mL 60302-608 1 HyperSep Retain PEP HyperSep Retain PEP SPE 30mg 1mL 60107-201 100 / 30mg 3mL 60107-202 50 / 60mg 3mL 60107-203 50 / 60mg 6mL 60107-208 30 / 100mg 6mL 60107-207 30 / 150mg 6mL 60107-211 30 / 200mg 3mL 60107-204 50 / 200mg 6mL 60107-212 30 / 500mg 3mL 60107-205 50 / 500mg 6mL 60107-206 30 / 1g 25mL 60107-215 20 / 2g 25mL 60107-214 20 / HyperSep-96Retain PEP 5mg 1mL 60303-201 100 / 10mg 1mL 60303-202 30mg 1mL 60303-203 100 / 60mg 1mL 60303-204 100 / 5mg 1mL 60303-205 1 10mg 1mL 60303-206 1 30mg 1mL 60303-207 1 60mg 1mL 60303-208 1 194

HyperSep Retain-CX HyperSep Retain-CX SPE 30mg 1mL 60107-301 100 / 30mg 3mL 60107-302 50 / 60mg 3mL 60107-303 50 / 60mg 6mL 60107-308 30 / 100mg 6mL 60107-307 30 / 150mg 6mL 60107-311 30 / 200mg 3mL 60107-304 50 / 200mg 6mL 60107-314 30 / 500mg 3mL 60107-305 50 / 500mg 6mL 60107-306 30 / 1g 25mL 60107-315 20 / 2g 25mL 60107-312 20 / HyperSep-96Retain PEP 5mg 1mL 60303-301 100 / 10mg 1mL 60303-302 100 / 30mg 1mL 60303-303 100 / 60mg 1mL 60303-304 100 / 5mg 1mL 60303-305 1 10mg 1mL 60303-306 1 30mg 1mL 60303-307 1 60mg 1mL 60303-308 1 HyperSep Retain-AX HyperSep Retain-AX SPE 30mg 1mL 60107-401 100 / 30mg 3mL 60107-402 50 / 60mg 3mL 60107-403 50 / 60mg 6mL 60107-408 30 / 100mg 6mL 60107-407 30 / 150mg 6mL 60107-411 30 / 200mg 3mL 60107-404 50 / 200mg 6mL 60107-414 30 / 500mg 3mL 60107-405 50 / 500mg 6mL 60107-406 30 / 1g 25mL 60107-415 20 / 2g 25mL 60107-412 20 / HyperSep-96Retain-AX 5mg 1mL 60303-401 100 / 10mg 1mL 60303-402 100 / 30mg 1mL 60303-403 100 / 60mg 1mL 60303-404 100 / 5mg 1mL 60303-405 1 10mg 1mL 60303-406 1 30mg 1mL 60303-407 1 60mg 1mL 60303-408 1 HyperSep C18 HyperSep Silica C18 SPE 50mg 1mL 60108-390 100 / 100mg 1mL 60108-302 100 / 200mg 3mL 60108-303 50 / 500mg 3mL 60108-304 50 / 500mg 6mL 60108-305 30 / 1g 6mL 60108-301 30 / 2g 15mL 60108-701 20 / 5g 25mL 60108-702 20 / 10g 75mL 60108-703 10 / HyperSep-96 C18 10mg 1mL 60300-421 100 / 25mg 1mL 60300-422 100 / 50mg 1mL 60300-423 100 / 100mg 1mL 60300-424 100 / 10mg 1mL 60300-425 1 25mg 1mL 60300-426 1 50mg 1mL 60300-427 1 100mg 1mL 60300-428 1 195

HyperSep C8 HyperSep C8 SPE 50mg 1mL 60108-391 100 / 100mg 1mL 60108-392 100 / 200mg 3mL 60108-393 50 / 500mg 3mL 60108-394 50 / 500mg 6mL 60108-395 30 / 1g 6mL 60108-427 30 / 2g 15mL 60108-704 20 / 5g 25mL 60108-705 20 / 10g 75mL 60108-706 10 / HyperSep-96 C18 10mg 1mL 60300-441 100 / 25mg 1mL 60300-442 100 / 50mg 1mL 60300-443 100 / 100mg 1mL 60300-444 100 / 10mg 1mL 60300-445 1 25mg 1mL 60300-446 1 50mg 1mL 60300-447 1 100mg 1mL 60300-448 1 HyperSep Phenyl HyperSep Phenyl SPE 50mg 1mL 60108-516 100 / 100mg 1mL 60108-386 100 / 200mg 3mL 60108-387 50 / 500mg 3mL 60108-388 50 / 500mg 6mL 60108-389 30 / 1g 6mL 60108-517 30 / 2g 15mL 60108-707 20 / 5g 25mL 60108-708 20 / 10g 75mL 60108-709 10 / HyperSep-96 Phenyl 10mg 1mL 60300-681 100 / 25mg 1mL 60300-682 100 / 50mg 1mL 60300-683 100 / 100mg 1mL 60300-684 100 / 10mg 1mL 60300-685 1 25mg 1mL 60300-686 1 50mg 1mL 60300-687 1 100mg 1mL 60300-688 1 HyperSep Silica HyperSep Silica SPE 50mg 1mL 60108-409 100 / 100mg 1mL 60108-317 100 / 200mg 3mL 60108-410 50 / 500mg 3mL 60108-315 50 / 500mg 6mL 60108-411 30 / 1g 6mL 60108-426 30 / 2g 15mL 60108-710 20 / 5g 25mL 60108-711 20 / 10g 75mL 60108-712 10 / HyperSep-96 Silica 10mg 1mL 60300-481 100 / 25mg 1mL 60300-482 100 / 50mg 1mL 60300-483 100 / 100mg 1mL 60300-484 100 / 10mg 1mL 60300-485 1 25mg 1mL 60300-486 1 50mg 1mL 60300-487 1 100mg 1mL 60300-488 1 196

HyperSep SAX HyperSep SAX SPE 50mg 1mL 60108-418 100 / 100mg 1mL 60108-360 100 / 200mg 3mL 60108-417 50 / 500mg 3mL 60108-419 50 / 500mg 6mL 60108-434 30 / 1g 6mL 60108-521 30 / 2g 15mL 60108-713 20 / 5g 25mL 60108-714 20 / 10g 75mL 60108-715 10 / HyperSep-96 SAX 10mg 1mL 60300-561 100 / 25mg 1mL 60300-562 100 / 50mg 1mL 60300-563 100 / 100mg 1mL 60300-564 100 / 10mg 1mL 60300-565 1 25mg 1mL 60300-566 1 50mg 1mL 60300-567 1 100mg 1mL 60300-568 1 HyperSep SCX HyperSep SCX SPE 50mg 1mL 60108-420 100 / 100mg 1mL 60108-421 100 / 200mg 3mL 60108-422 50 / 500mg 3mL 60108-423 50 / 500mg 6mL 60108-520 30 / 1g 6mL 60108-433 30 / 2g 15mL 60108-716 20 / 5g 25mL 60108-717 20 / 10g 75mL 60108-718 10 / HyperSep-96 SCX 10mg 1mL 60300-581 100 / 25mg 1mL 60300-582 100 / 50mg 1mL 60300-583 100 / 100mg 1mL 60300-584 100 / 10mg 1mL 60300-585 1 25mg 1mL 60300-586 1 50mg 1mL 60300-587 1 100mg 1mL 60300-588 1 HyperSep Verify AX HyperSep Verify-AX SPE 50mg 1mL 60108-420 100 / 100mg 1mL 60108-421 100 / 200mg 3mL 60108-422 50 / 500mg 3mL 60108-423 50 / 500mg 6mL 60108-520 30 / 1g 6mL 60108-433 30 / 2g 15mL 60108-716 20 / 5g 25mL 60108-717 20 / 10g 75mL 60108-718 10 / HyperSep-96 Verify-AX 10mg 1mL 60300-809 100 / 25mg 1mL 60300-810 100 / 50mg 1mL 60300-811 100 / 100mg 1mL 60300-812 100 / 10mg 1mL 60300-813 1 25mg 1mL 60300-814 1 50mg 1mL 60300-815 1 100mg 1mL 60300-816 1 197

HyperSep Verify-CX HyperSep Verify-CX SPE 130mg 1mL 60108-719 100 / 200mg 6mL 60108-722 50 / 300mg 3mL 60108-720 50 / 500mg 3mL 60108-721 50 / 500mg 6mL 60108-722 30 / 1g 10mL 60108-723 50 / 2g 6mL 60108-724 30 / HyperSep-96 Verify-CX 10mg 1mL 60300-801 100 / 25mg 1mL 60300-802 100 / 50mg 1mL 60300-803 100 / 100mg 1mL 60300-804 100 / 10mg 1mL 60300-805 1 25mg 1mL 60300-806 1 50mg 1mL 60300-807 1 100mg 1mL 60300-808 1 HyperSep Florisil HyperSep Florisil SPE 50mg 1mL 60108-402 100 / 100mg 1mL 60108-403 100 / 200mg 3mL 60108-404 50 / 500mg 3mL 60108-405 50 / 500mg 6mL 60108-500 30 / 1g 6mL 60108-431 30 / 2g 15mL 60108-735 20 / 5g 25mL 60108-736 20 / 10g 75mL 60108-737 10 / HyperSep-96 Florisil 10mg 1mL 60300-721 100 / 25mg 1mL 60300-722 100 / 50mg 1mL 60300-723 100 / 100mg 1mL 60300-724 100 / 10mg 1mL 60300-725 1 25mg 1mL 60300-726 1 50mg 1mL 60300-727 1 100mg 1mL 60300-728 1 HyperSep Aminopropyl HyperSep Aminopropyl SPE 50mg 1mL 60108-424 100 / 100mg 1mL 60108-364 100 / 200mg 3mL 60108-425 50 / 500mg 3mL 60108-518 50 / 500mg 6mL 60108-519 30 / 1g 6mL 60108-432 30 / 2g 15mL 60108-738 20 / 5g 25mL 60108-739 20 / 10g 75mL 60108-740 10 / HyperSep-96 Aminopropyl 10mg 1mL 60300-510 100 / 25mg 1mL 60300-502 100 / 50mg 1mL 60300-503 100 / 100mg 1mL 60300-504 100 / 10mg 1mL 60300-505 1 25mg 1mL 60300-506 1 50mg 1mL 60300-507 1 100mg 1mL 60300-508 1 198

HyperSep Cyano HyperSep Cyano SPE 50mg 1mL 60108-746 100 / 100mg 1mL 60108-745 100 / 200mg 3mL 60108-747 50 / 500mg 3mL 60108-748 50 / 500mg 6mL 60108-749 30 / 1g 6mL 60108-750 30 / 2g 15mL 60108-751 20 / 5g 25mL 60108-752 20 / 10g 75mL 60108-753 10 / HyperSep-96 Cyano 10mg 1mL 60300-817 100 / 25mg 1mL 60300-818 100 / 50mg 1mL 60300-819 100 / 100mg 1mL 60300-820 100 / 10mg 1mL 60300-821 1 25mg 1mL 60300-822 1 50mg 1mL 60300-823 1 100mg 1mL 60300-824 1 HyperSep Diol HyperSep Diol SPE 50mg 1mL 60108-571 100 / 100mg 1mL 60108-572 100 / 200mg 3mL 60108-573 50 / 500mg 3mL 60108-574 50 / 500mg 6mL 60108-575 30 / 1g 6mL 60108-576 30 / 2g 15mL 60108-755 20 / 5g 25mL 60108-756 20 / 10g 75mL 60108-757 10 / HyperSep-96 Diol 10mg 1mL 60300-635 100 / 25mg 1mL 60300-636 100 / 50mg 1mL 60300-637 100 / 100mg 1mL 60300-638 100 / 10mg 1mL 60300-630 1 25mg 1mL 60300-631 1 50mg 1mL 60300-632 1 100mg 1mL 60300-633 1 199

HyperSep SPE HyperSep Javelin SPE Retain PEP Retain-CX Retain-AX Hypercarb 2.1mm 10mm 60310-201 60310-301 60310-401 60310-501 4 / 3.0mm 10mm 60310-202 60310-302 60310-402 60310-502 4 / HyperSep UNIGUARD SPE Retain PEP Retain-CX Retain-AX Hypercarb 2.1mm 10mm 60311-201 60311-301 60311-401 60311-501 4 / 3.0mm 10mm 60311-202 60311-302 60311-402 60311-502 4 / SPE HyperSep HPLC Retain PEP Retain-CX Retain-AX Hypercarb 2.1mm 20mm 60312-201 60312-301 60312-401 60312-501 4 / 3.0mm 20mm 60312-202 60312-302 60312-402 60312-502 4 / HyperSep HyperSep SPE 96- / / 60104-230 1 60104-241 1 60104-243 1 24-60104-234 24 / 48-60104-235 48 / HyperSep-96 HyperSep-96 96- HyperSep-96 60103-351 1 60104-241 1 60104-243 1 HyperSep-96 60300-301 1 HyperSep-96 60300-303 5 / 1mL 60300-402 50 / 2mL 60300-403 50 / 1mL 3mL 6mL SPE 60104-259 15 / 1mL 60300-311 100 / 200

HyperSep 16 Corian0 16 Teflon0 Luer 16 24 Corian0 24 Teflon0 Luer 24 16 60104-232 1 24 60104-233 1 60104-243 1 60104-241 1 60104-240 1 16 60104-242 16 / 24 60104-244 24 / 60104-245 12 / 60104-261 1 16 60104-262 1 24 60104-248 16 60104-249 1 24 60104-250 1 16 60104-251 1 24 60104-252 1 16 60104-253 1 24 60104-254 1 60104-260 1 60104-255 12 Luer 60104-256 12 / 60104-257 4 / Luer Lock 60104-258 12 / 201

HyperSep SLE 96 / (SLE) SLE 200mL, SLE : LLE LLE LL LLE : (1) SLE 5-10 (2) (3) HyperSep SLE 96 HyperSep SLE SLE(pH=7) 200mg 3 60109-200-3-7 50 500mg 3 60109-500-3-7 50 500mg 6 60109-500-6-7 30 1g 6 60109-1000-6-7 30 2g 12 60109-2000-12-7 20 4g 25 60109-4000-25-7 15 20g 60 60109-20000-60-7 10 HyperSep SLE SLE(pH=9) 200mg 3 60109-200-3-9 50 500mg 3 60109-500-3-9 50 500mg 6 60109-500-6-9 30 1g 6 60109-1000-6-9 30 2g 12 60109-2000-12-9 20 4g 25 60109-4000-25-9 15 20g 60 60109-20000-60-9 10 HyperSep SLE 96 SLE(pH=7) 200mg 2 60109-200-2-7W 1/ 300mg 2 60109-300-2-7W 1/ 400mg 2 60109-400-2-7W 1/ 500mg 2 60109-500-2-7W 1/ HyperSep SLE SLE(pH=9) 200mg 2 60109-200-2-9W 1/ 300mg 2 60109-300-2-9W 1/ 400mg 2 60109-400-2-9W 1/ 500mg 2 60109-500-2-9W 1/ 202

HyperSep SPE -QuEChERS Thermo Scientific QuEChERS( ) SPE QuEChERS HyperSep SPE -QuEChERS QuEChERS 6g MgSO 4, 1.5g 50mL 60105-210 250 / 4g MgSO 4, 1g 50mL 60105-211 250 / 1.5g 1.5g 750mg 50mL 60105-212 250 / 4g 1g 1g 500 mg 50mL 60105-216 250 / QuEChERS 6g 1.5g 50mL 60105-310 25 50mL 60105-310 25 / 4g 1g NaCI 50mL 60105-311 25 50mL 60105-311 25 / 6g 1.5g 1.5g 750mg 50mL 60105-312 25 50mL 60105-312 25 / 4g 1g 1g 500mg 50mL 60105-316 25 50mL 60105-316 25 / 900mg MgSO 4 300mg PSA 150mg 15mL 15mL 60105-205 50 / 900mg MgSO 4 300mg PSA 150mg C18 15mL 15mL 60105-206 50 / 750mg MgSO 4 250mg PSA, 250mg C18 250 15mL 15mL 60105-213 50 / 900mg MgSO 4, 300mg PSA 15mL 15mL 60105-214 50 / 900mg MgSO 4 150mg PSA 15mL 15mL 60105-215 50 / 900mg MgSO 4 150mg PSA 45mg 15mL 15mL 60105-217 50 / 900mg MgSO 4 150mg PSA 15mg 15mL 15mL 60105-218 50 / 1200mg MgSO 4 400mg PSA 15mL 15mL 60105-224 50 / 1200mg MgSO 4 400mg PSA 400mg C18 15mL 15mL 60105-225 50 / 1200mg MgSO 4 400mg PSA, 400mg C18 400mg 15mL 60105-226 50 / 900mg MgSO 4 150mg PSA 150mg C18 15mL 60105-227 50 / 150mg MgSO 4 50mg PSA 50mg 15mL 60105-230 50 / 150mg MgSO 4 300mg PSA 150mg Chlorofiltr 15mL 60105-231 50 / 900mg MgSO 4 300mg PSA 150mg 15mL 60105-305 10 / 900mg MgSO 4 300mg PSA 150mg C18 15mL 60105-306 10 / 150mg MgSO 4 50mg PSA, 50mg 15mL 60105-313 10 / 900mg MgSO 4 300mg PSA 15mL 60105-314 10 / 900mg MgSO 4 150mg PSA 15mL 60105-315 10 / 900mg MgSO 4 50mg PSA 45mg 15mL 60105-317 10 / 900mg MgSO 4 150mg PSA 15mg 15mL 60105-318 10 / 1200mg MgSO 4 400mg P SA 15mL 60105-324 10 / 1200mg MgSO 4 400mg PSA 400mg C18 15mL 60105-325 10 / 1200mg MgSO 4 400mg PSA, 400mg C18 400mg 15mL 60105-326 10 / 203

QuEChERS 900mg MgSO 4 150mg PSA 150mg C18 15mL 60105-327 10 / 150mg MgSO 4 10mg PSA 50mg 15mL 60105-330 10 / 150mg MgSO 4 300mg PSA 150mg Chlorofiltr 15mL 60105-331 10 / 400mg PSA 200mg 6mL 60105-207 30 / 500mg PSA 250mg 6mL 60105-208 30 / 500mg PSA 500mg 6mL 60105-209 30 / 400mg PSA 200mg 6mL 60105-307 10 / 500mg PSA 250mg 6mL 60105-308 10 / 500mg PSA 500mg 6mL 60105-309 10 / 150mg MgSO 4 50mg PSA 50mg 2mL 60105-202 100 / 150mg MgSO 4 50mg PSA 2mL 60105-203 100 / 150mg MgSO 4 50mg PSA 50mg C18 2mL 60105-204 100 / 150mg MgSO 4 25mg PSA 2mL 60105-219 100 / 150mg MgSO 4 25mg PSA 25mg C18 2mL 60105-220 100 / 150mg MgSO 4 25mg PSA 2.5mg 2mL 60105-221 100 / 150mg MgSO 4 25mg PSA 7.5mg 2mL 60105-222 100 / 150mg MgSO 4 50mg PSA 50mg C18 50mg 2mL 60105-223 100 / 150mg MgSO 4 50mg PSA 50mg 2mL 60105-302 10 / 150mg MgSO 4 50mg PSA 2mL 60105-303 10 / 150mg MgSO 4 50mg PSA 50mg C18 2mL 60105-304 10 / 150mg MgSO 4 25mg PSA 2mL 60105-319 10 / 50mg MgSO 4 25mg PSA 25mg C18 2mL 60105-320 10 / 150mg MgSO 4 25mg PSA 2.5mg 2mL 2mL 60105-321 10 / 150mg MgSO 4 25mg PSA 7.5mg 2mL 60105-322 10 / 150mg MgSO 4 50mg PSA, 50mg C18 50mg 2mL 60105-323 10 / HyperSep SPE Mylar Mylar 4000mg 1000mg 60105-340 50 / Mylar 6000mg 1500mg ( ) 60105-341 50 / Mylar 6000mg 1500mg 60105-342 50 / Mylar 6000mg 1500mg 1500mg 750mg 60105-343 50 / Mylar 4000mg 1000mg 500 1000mg 60105-344 50 / Mylar 1.2g 60105-345 50 / Mylar 4g 0.5g 60105-346 50 / HyperSep SPE 50 4000mg 100mg 60105-332 50 / 4000mg 100mg 500mg 1000mg 60105-333 50 / 4000mg 1g 60105-334 50 / 6000mg 1500mg 60105-335 50 / 6000mg 1500mg 60105-336 50 / 6000mg 1500mg 1500mg 1750mg 60105-337 50 / 8000mg 200mg 60105-338 50 / 8000mg 3500mg 60105-339 50 / 204