☆H23 13－農薬一斉分析（大垣）.doc
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1 Examination of Determination of Residual Pesticides in Agricultural Products Yuki OHGAKI, Katsuhiro HAYASHI, Hiroyuki KAWAI, and Kyoko SHIMURA GC/MS 92 LC/MS/MS n- 5 GC/MS % LC/MS/MS % 117 LC/MS/MS 5 PL GPC 15) GPC 6) 6) GC/MSLC/MS/MS PL-2-1
2 2µg/mL n- LC/MS PL-3-1-BHC - GC/NH 2 GL SciencesInert Sep GC/NH 2 (500mg/500mg/6mL) PL-7-2GC/MS GC/MS-QP2010 B1a RESTEK Rtx-5MS 0.25mm i.d.30m, 0.25µm 501min25min125 10min30010min MS 230 1µLSplitless He EI PL S- 70eV SIM 1 LC/MS/MS A D HPLC ProminenceUFLC MSAB SCIEX API3200QTRAP GL Science Inertsil ODS-SP 2.1mm i.d. 150mm, 3µm mL/min 3µL A 5mM PL-1-1PL-2-1 PL-3-1 B 5mM 1µg/mL 0 A:B=85: A:B=60:40 6 A:B=50:50 8 A:B=45: A:B=5:95 PL-7-2 PL-14-1
3 No. m/z (min) (µg/ml) (µg/ml) (ppm) ß ß
4 No. m/z (min) (µg/ml) (µg/ml) (ppm) ESI(+) MRM 2 GPC 6) 6) 25g PL-1-1 PL-2-1 PL-3-1 1µg/mL 2.5mL 0.1µg/g
5 2 LC/MS/MS No. DP CE DP CE (min) m/z V V m/z V V > > > > (PAC) > > > > > > > > > > > > > > > > (E) > > (Z) > > > > > > > > > > > > > > > > > > > > > > > > > > > > > > > > > > B1a > > > > > > > > > > > > > > > > > > > > > > S > > > > > > > > > > > > > > > > > > > > > > > > > > > > > > > > > > > > A > > D > > > >
6 GC/MS mL 1.0µg/mL GC/NH 2 1 n- (1:1) 20mL S/N µg/mL 25g 0.01ppm 1mL 5mL PL-7-2 PL-14-1 GC/MS LC/MS/MS LC/MS/MS ng/mL 1 3 PL-7-2 PL g 2µg/mL 1mL 0.01ppm 0.08µg/g 0.02ppm 0.01ppm 0.05ppm 6) GPC B1a 60130mL D GPC 1mL GPC PL-7-2 n- (1:1) 1mL PL µg/mL 4mL n- (1:1) mL 5mL 10mL GC/NH 2 LC/MS/MS (500mg/500mg/6mL) 4 n- (1:1) 20mL 100% B1a A 1mL GC/MS D 5055mL 65mL 5mL 0.2µmPTFE LC/MS/MS 3 1 LC/MS/MS GPC 60130mL 60130mL 3 70% PL-1-1PL-2-1 PL-3-1 GC/MS 25g PL-1-1 PL-2-1 PL µg/mL 2.5mL 0.1ppm
7 3 3 5 No. (ng/ml) (ng/ml) (ppm) %7-3 (PAC) FPD(P)-GC LC/MS/MS 7-11 (E) (Z) % GC/NH % % C.V.20% 7-29 B1a PL-7-2 PL µg/mL 1mL 0.08ppm 5 6 LC/MS/MS 2 LC/MS/MS S A D
8 4 GPC LC/MS/MS No. 5mL (PAC) (E) (Z) B1a S A D
9 No. 5 GC/MS n=3 C.V. C.V. C.V. C.V. C.V. (%) (%) (%) (%) (%) (%) (%) (%) (%) (%) ß
10 5 No. C.V. C.V. C.V. C.V. C.V. (%) (%) (%) (%) (%) (%) (%) (%) (%) (%) ß
11 No. 5 C.V. C.V. C.V. C.V. C.V. (%) (%) (%) (%) (%) (%) (%) (%) (%) (%) B1a 50 D ng/mL 25g 0.01ppm LC/MS/MS 60 GPC GC/MS B1a 100 A D 57 LC/MS/MS 60130mL 5 GC/MS % LC/MS/MS % ) 1) GPC GC/MS 92 LC/MS/MS 60 No (1995) 2) GC/MS GPC GC/MS-SIM µg/mL No.42 25g 0.01ppm 83-94(1996) LC/MS/MS
12 6 LC/MS/MS n=5 No. C.V. C.V. C.V. C.V. C.V. (%) (%) (%) (%) (%) (%) (%) (%) (%) (%) (PAC) (PAC) (E) (E) (Z) (Z)
13 6 No. C.V. C.V. C.V. C.V. C.V. (%) (%) (%) (%) (%) (%) (%) (%) (%) (%) B1a B1a S S
14 6 No. C.V. C.V. C.V. C.V. C.V. (%) (%) (%) (%) (%) (%) (%) (%) (%) (%) A A D D
15 7 (%) (PAC) (PAC) (E) (E) (Z) (Z) B1a B1a
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3--2-3-Iodo-2-propynyl butylcarbamate (IPBC) Carbamic acid, butyl-, 3-iodo-2-propynyl ester Iodocarb CAS 55406-53-6 C 8 H 12 NO 2 I C (g/cm 3 ) (mmhg) log P ow 281.09 (280.9910) 64 68 1.51 1.57 (20 C)
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2,2-2,2 -Iminodiethanol Diethanol amine CAS 111-42-2 C 4 H 11 NO 2 105.1356-105.0790-28 C 1) 1.0881 g/cm 3 1)
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2,2-2,2 -Iminodiethanol Diethanol amine CAS 111-42-2 C 4 H 11 NO 2 105.1356-105.0790-28 C 1) 1.0881 g/cm 3 1)
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N,N- N,N-Dimethylacetamide Acethyldimethylamine CAS 127-19-5 C 4 H 9 NO 87.12 ~ 87.14 87.68413 163-165 C 1) - 18.59 C 2) 1 mg/l 25 C 3) 3.3 hpa 2 C 4) log P ow -.77 2).9429 2/4 C 1) 3.1 4) 1.31E - 8 atm-m
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(PCB) 1 ng/l (µg/kg, wet) (µg/kg) 10 (0.01) 1 (0.001) 1 (0.001) 10 (0.01) 1 (0.001) 1 (0.001) 10 (0.01) 1 (0.001) 1 (0.001) 10 (0.01) 1 (0.001) 1 (0.001) 10 (0.01) 1 (0.001) 1 (0.001) 10 (0.01) 1 (0.001)
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PBDEs TriBDE DeBDE 1 TriBDE 8 TeBDE 6 PeBDE 8 HxBDE 7 HpBDE 5 OcBDE 3 NoBDE 2 DeBDE 40 GC/MS 1 1 1 ng/l µg/kg, dry µg/kg TriBDE 0.1 0.01 0.01 TeBDE 0.1 0.01 0.01 PeBDE 0.1 0.01 0.01 HxBDE 0.1 0.01 0.01
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