1993 B1 A [2] 17 B1B2G1 G2M1M2 B1B2G1G2 M1 B1 B1 RNA 1
CH 3 CH 3 CH 3 B 1 B 2 G 1 H H H N H C H3 CH 3 CH 3 Cl H G 2 M1 chratoxin A H H H N N H 3C N H CH 3 H H ST Citrinin VERR H CH3 H3C H H 3 C H H H CH2 CH3 H ZN (DN) CCH 3 H H CH 3 Fusarenon X H 3C CH 3 H 3 C H CH 2 AC CH 3 H H AC H H A C H H H 3 C CH2 H CH 3 H T-2 HT-2 3-3-ADN AC 2
H 3 C H H H H H H CH2 AC CH3 15-15-ADN NIV H H H ZAN H 1 (ppb)ug/kg (ppb) 20 4 2 B1 2 0. M1 0.5 0.025 0.05 A 5 0.5 DN 1000 10001250 150 200 ZN 100 50 20 (ppb) B1 20 10 5 5 M1 0.5 A 5 DN 1000 ZN 60 3
4
5 Verruculogen
3 (ev) (ev) 6
1&2 10&11 1&2 5&6 10&11 1&2 3 4 5 6 7 8 9 10 11 1&2 5&6 8 11 min 2-A 1.Aflatoxin M12.Aflatoxin G23.Aflatoxin G14.Aflatoxin B25.Aflatoxin B16.Citrinin, 7.HT-28.T-29. ZAN 10.Sterigmatocystin11.Verrulogen 2.5 7&8 1 2&3 4 5&6 1 2 5&6 7&8 1 2 3 4 5&6 7&8 1&2 3&4 5&6 7&8 7
min 2-B 1.NIV2.DN3.FX4.TA5.3-ADN6.15-ADN7.ZN8. ZAN- 2.5 08848.00000000 MIC-2006-04-19-003+ Sm (Mn, 2x3) 100 MRM of 11 Channels ES+ 325 > 310 2.54e6 08848.00000000 MIC-2006-04-16-009- Sm (Mn, 2x3) 100 MRM of 9 Channels ES- 295.1 > 265.1 2.84e5 % 1 2 3 5.68 % 4 5 6 1.69 0 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50 5.00 5.50 6.00 6.50 7.00 Time 08848.00000000 MIC-2006-04-13-006+ Sm (Mn, 2x3) 100 3 MRM of 11 Channels ES+ 325 > 310 2.54e6 0 08848.00000000 100 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50 5.00 5.50 MIC-2006-04-16-010- Sm (Mn, 2x3) 5 6 Time MRM of 9 Channels ES- 295.1 > 265.1 2.84e5 % 1 2 5.69 % 4 1.69 0 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50 5.00 5.50 6.00 6.50 7.00 Time 0 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50 5.00 5.50 Time min min 3 8
10&11 18 1 2 3 4 9 7&8 5&6 12 13 14 15 16 17 19 min 4 17 1.NIV2.DN3.FX4.TA5.3-ADN6.15-ADN7.AFG28.AFM19.AFG110.ZN11. ZAN 12.AFB213.AFB1 14.Citrinin15.HT-216.T-217. ZAN 18.Sterigmatocystin19.Verrulogen Waters ACQUITY UPLC BEH C18 2.1100 mm 1.7 um35 25 5 L0.3mL/min A(ESI+) 10mM (ESI-) 0.1% B 20% B(0 min), 85% B(5.5 min), 100% B5.8min20% B(7.0 min) A 19 4 B 16 3 15 5 7 8 9 17 6 11 10 18 12 1 13 2 14 min min 5 10 M+1+ 7 1.NIV2.DN3.FX4.TA5.3-ADN6.15-ADN7.AFG28.AFM19.AFG110.ZN11. ZAN 12.AFB213.AFB1 9
14.Citrinin15.HT-216.T-217. ZAN 18.Sterigmatocystin19.Verrulogen 4 H 3 C AC H 3 C AC CH 2 H CH 3 H 307 173 CH 2 H CH 3 H 10
H 3C H H 3 C H 150 H CH 2 CH 3 AC 219 H CH 2 CH 3 AC 11
7 SPE 100% 226# SPE 228# SPE HLB A1 A2 B1 B2 min 8 A1 10 ES, A2 ES B1 7 ES,B2 ES, 5 A B min min 9 12
9 -A ESI- ZAN 9-B ESI+ ZAN 5 13
A B 14
15
5 µg/kg 1# 2# 3# 4# 5# 6# 7# 8# 9# 10# AFBI / / / / / / / / / 0.51 AFB2 / / / / / / / / / 0.26 AFG1 / / / / / / / / / / AFG2 / / / / / / / / / / AFM1 / / / / / / / / / / T-2 / / / / / / / / / / HT-2 / / / / / / / / / / Verrulogen / / / / / / / / / / Sterigmatocystin / / / / / / / / / 0.28 Citrinin / 8.16 / / / / / / / 5.06 TA 6.25 / 5.62 5.16 2.56 6.35 7.24 8.12 26.51 8.23 FX 1.05 / 0.62 1.95 / / / / / / 3-ADN 0.31 / 0.43 0.31 4.00 10.85 5.68 8.05 / 3.75 15-ADN 12.31 5.14 44.26 3.56 80.25 451.23 362.51 510.32 20.26 70.45 NIV 11.02 / 3.62 1.56 2.21 16.23 8.56 8.26 2.86 2.65 ZN 95.32 0.42 16.58 8.56 51.26 186.26 105.62 8.16 1.57 102.21 DN 168 15 136 37 310 2000 1525 1206 61 385 6 µg/kg 1# 2# 3# 4# 5# 6# 7# 8# 9# 10# AFBI / 0.08 3.57 7.46 0.89 23.15 6.25 0.07 1.62 0.86 AFB2 / / 1.25 2.15 0.51 8.16 2.56 0.03 0.45 0.26 AFG1 / 0.27 1.12 0.81 0.21 16.24 13.65 0.06 2.51 1.05 AFG2 / / / 0.06 / 1.95 1.56 / 1.52 / T-2 / / / / / / / / / / HT-2 / / / / / / / / / / Verrulogen / / / / / / / / / / Sterigmatocystin / / / / / 0.42 0.21 / 7.26 / Citrinin / / / / / / / / 4.53 / TA / / / / / / / / / / FX / / / / / / / / / / 3-ADN / / / / / / / / / / 15-ADN / / / / / / / / / / NIV / / / / / / / / / / ZN / / / / / / / / / / DN / / / / / / / / / / 16
VERR TA T-2 FX HT-2 AFG2 AFM1 AFG SMC 3-ADN 15-ADN ZAN - ( IS) ZAN + ( IS) ZN AFB2 NIV AFB1 CTN DN 12 MRM 5 VERR TA T-2 FX HT-2 AFG2 3-ADN AFM1 15-ADN AFG1 SMC ZAN - ( IS) ZAN + ( IS) ZN AFB2 AFB1 CTN NIV DN 13 MRM 5 17
µg/kg µg/kg 18
19