CDFA MRSM CDFA MRSM [California Department of Food and Agriculture CDFA ] [Center for Analytical Chemistry CAC ] [Multiresidue screen method MRSM ] 20

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1 CDFA-MRSM CDFA MRSM SOP Retention Time Locking

2 CDFA MRSM CDFA MRSM [California Department of Food and Agriculture CDFA ] [Center for Analytical Chemistry CAC ] [Multiresidue screen method MRSM ] # FR-40 # MRLs 40 # DPR 1991 CDFA DPR CDFA Anaheim Fresno Sacramento 12 CDFA MRSM MDL 0.005~0.2ppm CDFA CAC CDFA MRSM Mill DB-1 DB-17 C 8 C 18 CDFA MRSM

250 700 4500 1902 DPR 1991 CDFA DPR CDFA 1926 30 Anaheim Fresno Sacramento 12 CDFA MRSM

3 CDFA MRSM GC HPLC MRSM GC Agilent6890 GC Agilent6890 HPLC( HP-1 DB-1 30m 0.25mm 0.25 m HP-50+ DB-17 30m 0.25mm 0.25 m HP-1 DB-1 30m 0.53mm 1.5 m HP-17 DB-17 30m 0.53mm 1.0 m ) C8 4.6mm 250mm 5 Agilent1100 C18 4.6mm 250mm 5 Pickering5200 GC-MS Agilent5973 ECD ECD FPD FPD FLD HP-5MS 30m 0.25mm 0.25 m MSD ( 1-7)

53mm 1.0 m ) C8 4.6mm 250mm 5 Agilent1100 C18 4.

4 7. CDFA MRSM SOP MRLs CDFA MRSM OP CH N CARB Hobart Chopper model L, ) OMNI MIXER HOMOGENIZER N EVAP Nitrogen Evaporation System Models 112 ECD FPD FLD 2 3

1L, ) OMNI MIXER HOMOGENIZER 17106 N EVAP

5 ACS NaOH 0.5N pickering (cat.no CB130) 2 OPA diluent pickering (cat.no CB910 O-Phthaladehyde(OPA) pickering (cat.no 0120) Thiofluor pickering (cat.no ) 100ml 5.0ml 1.0ml ml 300ml ml 10.0ml Florisil 1g Agilent AccuBOND II Part No Supelco Supelclean Envi-Florislil Reorder No.57053) Aminopropyl 500mg Agilent AccuBOND II Part No Supelco Supelclean LC-NH2 Reorder No m 25mm 0.45 m 13 2ml Agilent Part No Agilent Part No ml ml GC 1.0m Agilent 0.25mm Part No mm Part No HPLC C-18 Pickering 4.6mm 4.5cm Part No.18ECG002 ECD FPD 100% DB-1 HP-1 30m 0.25mm 0.25 m Agilent HP-1 Part No.19091Z-433 J&W DB-1 Part No % DB-17 HP m 0.25mm 0.25 m Agilent HP-50+ Part No.19091L-433 J&W DB-17 Part No % (DB-1 HP-1) 30m 0.53mm 1.50 m Agilent HP-1 Part No.19095Z-323 J&W DB-1 Part No % (DB-17 HP-50+) 4

188-1050 Supelco Supelclean LC-NH2 Reorder No.57014 0.2 m 25mm 0.45 m 13 2ml Agilent Part No.5182-0554 5018-0864 Agilent Part No.5183-4529 16ml5183-4530 40ml GC 1.0m Agilent 0.25mm Part No.

6 30m 0.53mm 1.0 m Agilent HP-50+ Part No.19095L-023 J&W DB-17 Part No MSD HP-5MS 30m 0.25mm 0.25 m Agilent HP-5MS Part No S-433 HPLC C 8 4.6mm 25cm 5 m Pickering Part No C mm 25cm 5 m Pickering Part No MRSM : / GC-FPD FL 1g NH 2 0.5g GC-MS GC-ECD LC-FLD 5

190191S-433 HPLC C 8 4.6mm 25cm 5 m Pickering Part No.1846250 C 18 4.

7 3.1 a OP CH CARB #(40-Code of Federal Requlations) ( ) ( ) 6

8 b c g 25.0g ml 50ml ml 10-15g 5-7.5gNaCl

9 ml-100ml 40ml-50ml a 10ml ml b 80 2ml 2ml 2ml 1% / v/v OP CH CARB a 2ml 15ml 3.0ml 5.0ml b c GC-FPD d 0.2 m 5ml GC a Florisil 1g 5ml 10% / v/v 5ml b 2ml Florisil 15ml 17. c 5ml 10% / v/v d C e15ml 55 8

10 5.0ml f 5.0ml g h GC-ECD N- a aminopropyl 4ml 1% / v/v b 2ml 1% / V/V 15ml 18. c 2ml 1% / V/V d C e 15ml 55 <0.1ml 19. f 2.5ml g 20. h 0.2 m 5ml HPLC DB-1 DB-17 FPD P Agilent l min 8 9

c 2ml 1% / V/V d 3.3.4.C e 15ml 55 <0.1ml 19. f 2.5ml g 20.

11 /min min 10ml/min DB-1 12ml/min DB-17 12ml/min 13min 2ml/min 15ml/min 5min 75ml/min 100ml/min DB-1 DB-17 ECD Agilent l min 6 /min 270 8min 23min 1ml/min 2.3ml/min 60ml/min ELCD 2 l min 10 /min min 20ml/min 65ml/min DB-5 10m 0.53mm 2.65 m DB-17 30m 0.53mm 0.25 m. 4.4 N HPLC Agilent 1100 Pickering Post Column System l a CDFA 42 1ml/min ex330nm em465nm min % b % min ml/min % ml/min 0.00 B 15% 2.00 B 25% 10

53mm 2.65 m DB-17 30m 0.53mm 0.25 m. 4.4 N- 4.4.1 HPLC Agilent 1100 Pickering Post Column System 4.4.2 20 l 4.4.3 a CDFA 42 1ml/min ex330nm em465nm min % 0 20 80 2 20 80 16 90 10 18 90 10 18.

12 8.00 B 25% ml/min 9.00 B 40% B 45% B 80% ml/min B 80% ml/min B 15% N NaoH 0.3ml/min 2-OPA 0.3ml/min RT GC RT RT 0.01 HPLC RT ( ) ( ) ng = a b >125% <75% C 1 l, 20 l = (ng) g( ) 100ml( ) 1000mg 1g 10ml( ) 5ml( ) 1ml 1000 l 1 l =1mg 11

3ml/min 100 5 RT GC RT 0.005 RT 0.01 HPLC RT 0.15 6 6.1 6.1.1 ( ) ( ) ng = a b >125% <75% C 1 l, 20 l 6.

13 25.0g( ) 50ml( ) 1000mg 1g 10ml( ) 5ml( ) 1ml 1000 l 1 l =1mg g( ) 100ml( ) 1000mg 1g 10ml( ) 2.5ml( ) 1ml 1000 l 20 l =40mg 25.0g( ) 50ml( ) 1000mg 1g 10ml( ) 2.5ml( ) 1ml 1000 l 20 l =40mg 6.3 ng/mg ppm X(ppm)= (ng) (mg) X(ppm)=[ ( ) ( ) (ng)]/1(mg) = ( ) ( ) X(ppm)= ( ) X(ppm)= (ng) = ( ) 40mg ( )

14 % (ppm) (50g 1.0ml ) Profenofos 1.27 Methidathion 1.09 Trifluralin 0.25 Oxyflurofen 0.11 Propoxur 1.05 Oxamyl 0.93 Chlorpyrifos 0.05 Methidathion 0.05 Vinclozolin 0.10 Heptachlor 0.10 Oxamyl 0.25 Propoxur 0.25 Phosalone 2.18 Methyl Parathion 0.30 Dicloran 0.20 Carbofuran 0.54 Aldicarb Sulfoxide 0.59 Aldicarb Sulfone SOP DB-1/DB-17 FPD HP-5 NPD FPD S DB-1/DB-17 ECD HP-5 13

10 Oxamyl 0.25 Propoxur 0.25 Phosalone 2.18 Methyl Parathion 0.30 Dicloran 0.20 Carbofuran 0.

15 ELCD C 18 C 8 NPD / CH OP Chlorpyrifos Carb Carbaryl 7.2 GC/MS ng/ l / ml 0.5ml 2 2.0ml 3 5ml 25% / Florisil lg 5ml 4 5 5ml 25% / 6 0.5ml PTFE / 1 50g 150gNa 2 SO 4 150ml 2 2min ml 5 0.5ml 6 PTFE a b c d Florisil 0.5ml 2 PTFE PTFE 1 1 PTFE 0.45 m 4mm 1ml

0ml 3 5ml 25% / Florisil lg 5ml 4 5 5ml 25% / 6 0.5ml 7 7.2.4 PTFE 7.2.2 / 1 50g 150gNa 2 SO 4 150ml 2 2min 3 4 60ml 5 0.

16 8 8.1 (ppm) (ppm) (%) (MDL)(ppm) 15

17 8.2 (ppm) (MRL S ) LOD 16

18 A OP-9 ( g/ml) ( g/ml) Acephate Chlorphyrifos-methyl DEF Ethion Methamidophos Omethoate Parathion Parathion-methyl Tetrachlorvinphos B OP-10 ( g/ml) ( g/ml) Azinphos-methyl Chlorpyrifos DDVP DDVP Diazinon Dimethoate ( ) -Mevinphos ( ) -Mevinphos Malathion Methidathion Phosmet Profenofos A CH-6 ( g/ml) ( g/ml) Chlorothalonil Chlorthal-dimethyl Cypermethrin Endosulfan Endosulfan Endosulfan Hexachlorobenzene Trifluralin

072 0.7 ( ) -Mevinphos 0.028 0.3 Malathion 0.10 1.0 Methidathion 0.05 0.5 Phosmet 0.20 2.0 Profenofos 0.10 1.0 9.1.2 A CH-6 ( g/ml) ( g/ml) Chlorothalonil 0.10 1.0 Chlorthal-dimethyl 0.

19 B CH-10 ( g/ml) ( g/ml) Captan Chloropyrifos CIPC P.P-DDE P.P-DDE Dichlobenil Dicloran Iprodione PCNB cis-permethrin trans-permethrin Vinclozolin CDRB-10 ( g/ml) ( g/ml) Aldicarb Aldicarb Sulfoxide Aldicarb Sulfone Carbaryl Carbofuran Carbouran,3-OH Isoprocarb Methiocarb Methomyl Promecarb

0 9.1.3 CDRB-10 ( g/ml) ( g/ml) Aldicarb 0.50 5.0 Aldicarb Sulfoxide 0.50 5.0 Aldicarb Sulfone 0.50 5.0 Carbaryl 0.50 5.0 Carbofuran 0.

20 l Agilent 6890FPD OP-9 HP-1 30m 0.53mm 1.0 m RT, Area Height (ppm)(rt * ) 0.10 (2.26) 0.20 (6.37) 0.20 (6.37) 0.05 (10.50) 0.05 (10.61) 0.05 (11.81) 0.10 (13.44) 0.05 (14.20) 0.05 (15.26) RT (min) A/H RT (min) A/H RT (min) A/H RT (min) A/H RT (min) A/H RT * RT 19

21 RT RT RT %-125% SR # SR # ~ SR # g/ml 1000 g/ml mg/ml SS # SR # A B C SM #

22 % 5% % GC-MSD/IRD , g/ml 10ppm 1.0ppm 0.1ppm g/ml ml a 10ng/ l 0.5ml 1mg/ml 50ml 60ml b 1ng/ l : 5ml 10ng/ l 50ml 21

23 c 0.1ng/ l : 0.5ml 10ng/ l 50ml ng/ l GC HPLC 10% ppm GC HPLC RT RRT g/ml

24 1 SR# CAS % mg 23

25 2 SS# + g g g % mg ml mg/ml 24

26 : : SM # : (#) ( g/ml) (ml) g/ml 25

27 4 : SS# mg/ml ml ml mg/ml SS#: g/ml 26

28 5 SS# mg/ml SS# mg/ml ml ml mg/ml g/ml SS# 27

29 6 SS# SS#

30 11 RT CDFA- CDFA- CDFA- acephate captan ( ) ( 10 ) ( ) 29

31 Retention Time Locking Agilent 6890N EPC 1. Agilent Instrument RTLock RTSearch, 1 1. RTL 2 52

32 RTLock New RTL Calibration.. Run1-Run5 Desired Ret Time

33 4 RTLock Re Lock current method Calc new pressure Update current HP6890 Method 5 RTSearch Edit RT Table 54

34 Auto Retention Time Locking Agilent 6890N EPC Agilent 6890N 1. autolock.zip ALCK1HPL.TXT ALCK2HPL.TXT AUTOLOCK.DOC AUTORTCL.MAC ALCK1HPL.TXT ALCK2HPL.TXT AUTORTCL.MAC CORE C:\HPCHEM\CORE\ instrument on line MACRO AUTORTCL.MAC, GO [ENTER] 1 RTLock 1. 55

35 2. - A. A B *A.m *B.m test.m testa.m testb.m A B A testa.m RTLock Auto RTL Calbration ( 3) 3. 56

36 OK 4 4. A 5 5. testa.m 20% 10% Abort Abort 6. 6 RTL_TEMP.M YES

37 A 8 8. RTLock Edit RTL Calibration OK A testa.m B testb.m A B testb.m 2 B 58

38 B. A B testa.m testb.m 9 A testa.m, RTLock Auto (Re)Lock current method testa.m

39 13. testa.m 14. test.m 1 testa.m 1 test.m, B testb.m A 2 B test.m 2 60

40 1 Pesticide Analytical Manual Volume l, Section 303: Method for Non-fatty Foods and reference therein. 2 J. Assoc.Off.Anal.Chem.(1985) Vol.68(2),29 3 Fresenius J Anal.Chem.(1991) 339, J. Assoc.Off.Anal.Chem.(1991) 74, Chromatographia (1987) 24, J. Agric.Food Chem (1991) 39(9), California Department of Food and Agriculture Multiresidue Screen For Pesticides in Fruits and Vegetables MRSM

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