Agilent サンプリークQuEChERS AOACキットをmakeuseしたLC/MS/MS 検出によるホウレン草中の残留農薬 analysis Manual
Contents
1. 120 1 mL 8 mL SPE 1 mL 8 mL 100 80 60 3 40 20 0 NK L lt NK 3 1 K H w h Xx ll h A h xX BN R v Nn Xx lt IN H mn 7 N KN 4 1mL SPE 8mL SPE Agilent QuEChERS AUAC SPE SPE SPE2. IS TPP 2 SPE A SPE B LC MS MS LC MS MS 3 SPE A SPE B 50 ng g LC MS MS 1 2 3 4 5 6 7 8 9 10 11 12 13 IS TPP L00
3. Agilent Technologies Inc 2009 Published in Japan August 6 2009 5990 4248JAJP Agilent Technologies
4. SPE 4 SPE GCB 13 Agilent AOAC 5982 5755 QuEChERS AOAC SPE 5982 5222 5982 5258 SPE
5. PSA SPE GCB C18 GCB SPE ACN 1 mL 50 mg GCB 50 mg PSA 150 mg GCB GCB
6. 2 3 IS SPE SPE LC MS MS 50 ng g LC MS MS 4 SPE 4 20 40 60 100 2 3 RSD 15 5
7. LC ESI MS MS SPE SPE 5 ng g LOO Limit of quantitation MRL Maximum residue limits 10 50 200 ng g 64 108 91 9 RSD 10 3 3 Agilent Technologies QuEChERS AOAC USDA 1 3 SPE 2 ACN MgS0
8. 200 pL 800 pL LC MS MS 1 SPE SPE 15 g 0 1 g 50 mL y mw L IS 0C 1 1 HAc 15 mL ACN AOAC QuEChERS Y 1 4000 rpm 5 1 mL ACN 1 mL ACN SPE 2 mL SPE 2 mL 325 pL 30 Y 13 000 rpm 2 13 000
9. 15mL 1 HOAc ACN Agilent QuEChERS AOAC 5982 5755 1 4000 rpm 5 ACN SPE SPE 2 SPE 2 mL SPE ACN 14 ml SPE SPE 15 mL 1 14 mL ACN SPE 1
10. 5 250 ng g 5 10 50 100 200 250 ng TPP 100 ng g IS IS S 5 ng g LO00 5 ppb MRL 3 1 mL 8 mL SPE R2 3 1 mL SPE 8 mL SPE
11. HAc pH 5 4 C 200 mL 800 mL 0 5 mL 1M NH 0Ac pH 5 5 mM NH 0Ac pH 5 20 80 H 0 5 mL 1 M NH 0Ac pH 5 1L ACN 5 5 mM NH 0Ac ACN 10 mL HAc 1L ACN 1 HAc ACN IS 0 5 mg mL 2 0 mg mL 0 1 ACN DMSO0 20 C 1 5 7 5 30 ug mL 3 0C 1 1 ACN H 0 0 1 0 1 1 1 ACN H 0 10 ng mL 1 1 ACN H 0 0 1 15 ng mL TPP IS
12. 6 1 mL 8 mL SPE RSD 4 5 9 1 mL 97 8 8 10 mL 103 4 1 mL RSD 3 6 8 mL RSD 4 3 4 1 mL 78 5 8 mL 69 7 1 mL RSD 2 7 8 mL RSD 3 3 4 4 2mL SPE 5982 5222 1 mL 10 ng g QC RSD 50 ng g 0C RSD 200 ng g 0
13. 1 5 7 Log P pKa MRL ng g 0 89 8 35 0 20 P SN S H 2 36 10 4 NH 50 SS 1 48 4 2 0 100 N ocn NH N 4 4 44 H 500 N 3 82 6 53 20 CI CH 0 CI il N 0 57 NA vy No 000 N ee NH 2 CI 0 79 NA 0 10 DN SCH 3 72 1 51 50 N J 1 5 7 Log P pKa MRL ng g 0 14 NA 2000 0 H Ps 0 0 19 4 06 600 NN N NH CT gt 0 N 2 39 4 73 50 12 00 lt 0 N 2 99 NA 1 5 Ne Re 0 HaC 3 4 NA cH 50 0 CH 0 OCH N 0
14. 1 142 0 gt 94 0 60 8 2 54 2 142 0 gt 124 9 8 1 218 1 gt 105 0 115 20 2 97 2 218 1 gt 78 0 50 1 192 1 gt 160 0 95 18 5 07 2 192 1 gt 105 0 40 1 256 1 gt 209 1 60 12 5 53 2 256 1 gt 175 0 18 1 202 1 gt 175 0 110 27 5 65 2 202 1 gt 131 0 38 1 210 1 gt 111 0 50 12 6 89 2 210 1 gt 92 9 15 1 202 0 gt 145 0 50 3 7 30 2 202 0 gt 115 0 40 1 243 1 gt 130 9 80 15 8 50 2 243 1 gt 172 9 15 1 297 1 gt 158 9 80 22 8 52 2 297 1 gt 200 9 15 1 284 1 gt 158 9 80 32 8 95 2 284 1 gt 172 9 32 1 226 1 gt 93 0 120 35 9 23 2 226 1 gt 108 0 35 1 314 0 gt 222 1 70 10 9 44 2 314 0 gt 235 0 10 TPP IS 1 327 1 gt 77 0 70 45 9 49 2 327 1 gt 151 9 45 1 2 15 mL 4 000 rpm 5 825 nL N 0 1 600 HL ACN
15. MRL Agilent 1200 HPLC Agilent Technologies Inc Agilent 6410 LC MS Agilent Technologies Inc Agilent QuEChERS AOAC 5982 5755 Agilent QuEChERS AOAC SPE 5982 5222 5982 5258 Agilent Technologies Inc CentraCL3R Thermo IEC VWR Eppendorf Brinkmann Instruments LC MS MS 8 HPLC Agilent Z0RBAX Eclipse Plus 3 0 x 150 mm 3 5 nm 959963 312 0 3 mL min 30 C 10 umL A 20 80 H 0 5 mM NH4OAc pH 5 0 B ACN 5 mM NH 0Ac pH 5 0
16. 1 HPLC Honeywell ACN DMSO0 HAc Sigma Aldrich NH40Ac Fisher Chemicals FA Fluka Sleinheim TPP Sigma Aldrich ChemService Ultra AlfaAesar 19 27 g NH OAc 250 mL 0 1M NH 0Ac pH 5 pH
17. R2 R2 Y 0 2358X 0 0008 0 9976 Y 0 2164X 0 0014 0 9983 Y 0 0862X 0 0003 0 9975 Y 0 0804X 0 0006 0 9942 Y 0 2073X 0 0002 0 9995 Y 0 2034X 0 0013 0 9978 Y 0 8375X 0 0032 0 9915 Y 0 8383X 0 0002 0 9982 Y 0 0652X 0 0007 0 9905 Y 0 0620X 0 0011 0 9742 Y 0 4081X 0 0008 0 9995 Y 0 4102X 0 0011 0 9975 Y 1 9253X 0 0042 0 9995 Y 1 8253X 0 0037 0 9996 Y 0 4243X 0 0013 0 9979 Y 0 3993X 0 0019 0 9946 Y 0 7859X 0 0012 0 9983 Y 0 7420X 0 0012 0 9985 Y 0 4586X 0 0002 0 9954 Y 0 4229X 0 0005 0 9903 Y 0 1643X 0 0014 0 9923 Y 0 1468X 0 0003 0 9944 Y 0 3274X 0 0024 0 9904 Y 0 3067X 0 0013 0 9978 Y 0 1809X 0 0015 0 9975 Y 0 1659X 0 0008 0 9928 SPE 10 50 200 ng g 3 0C
18. 1 1 1 1 ACN IPA H 0 0 2 B mL min 0 20 0 3 0 5 20 0 3 8 0 100 0 3 10 0 100 0 3 10 01 20 0 5 13 0 STOP 4 17 MS 350 C 10 L min 40 psi 4000 V 2 SPE 8 SPE 15 g 0 1 g 50 mL 0C 100 pL 100 uL IS 15 hug mL TPP 30
19. Limian Zhao Joan Stevens Agilent Technologies Inc 2850 Centerville Road Wilmington DE 19809 1610 USA Agilent QuEChERS AOAC LC MS MS AOAC 0uEChERS quick easy cheap effective rugged safe 13 AOAC SPE SPE GCB W MRM
20. GCB Agilent QuEChERS AOAC SPE 1 M Anastassiades S J Lehotay Fast and Easy Multiresidue Method Employment Acetonitrile Extraction Partitioning and Dispersive Solid Phase Extraction for the Determination of Pesticide Residues in Produce J AOAC Int 2003 86 412 431 2 S J Lehotay et al Use of Buffering and Other Means to Improve Results of Problematic Pesticides in a Fast and Easy Method for Residue Analysis of Fruits and Vegetables J AOAC Int 2005 88 615 629 3 S J Lehotay et al De
21. 1 mL Agilent QuEChERS SPE 2 mL 5982 5222 8 mL Agilent QuEChERS SPE 15 mL 5982 5258 2 mL 50 mg PSA 50 mg GCB 150 mg 15 mL 400 mg PSA 400 mg GCB 1200 mg 375 pL 2 mL 3 mL 15 mL 1 2 mL 13 000 rpm 2 2 LC MS MS 13 MRM m z V CE V RT 1 184 0 gt 94 9 60 3 2 55 2 184 0 gt 111 0 15
22. rpm 2 825 pL ACN Y Y 0 1 600 pL ACN Y LC MS MS GC MS 30 LC MS MS GC MS 2 mL SPE SPE QuEChERS AOAC 1 0uEChERS SPE GCB 4 LC MS MS
23. 7 58 0 3 5 62 1 3 3 66 8 2 8 104 9 1 4 103 3 3 7 99 0 3 3 116 9 2 2 114 6 2 4 110 8 2 1 105 3 2 5 105 7 2 8 103 0 2 3 86 3 3 9 94 9 4 3 93 9 3 4 103 5 10 4 106 9 3 6 99 2 6 4 63 1 2 8 60 6 4 8 62 7 2 9 111 2 4 5 106 6 3 2 112 0 3 0 SPE 11 4 1mL 8mL SPE 3 2 SPE 8 mL SPE 2 2 1 mL SPE 1
24. C RSD n 6 n 6 n 6 91 8 4 2 93 3 3 7 93 8 5 7 93 4 3 3 91 3 5 6 101 9 7 8 74 0 2 9 71 1 3 2 70 3 2 9 105 3 4 0 109 1 2 5 88 9 1 7 98 2 4 5 100 4 3 7 100 0 2 7 79 0 2 7 76 6 2 3 75 5 1 8 100 0 1 7 98 1 3 5 93 0 4 0 110 8 3 2 108 1 1 0 105 1 3 2 98 8 1 6 98 2 3 3 95 1 3 1 84 0 3 8 89 6 2 5 89 8 1 7 103 1 5 4 98 4 3 5 97 2 1 9 69 1 4 7 62 0 2 9 61 3 1 1 104 4 4 8 101 2 5 0 102 6 3 0 SPE 5 15 mL SPE 5982 5258 8 mL 10 ng g OC RSD 50 ng g OC RSD 200 ng g QC RSD n 6 n 6 n 6 98 6 3 8 94 2 7 1 97 8 2 9 95 5 8 9 91 5 6 3 105 6 5 7 62 4 4 3 53 9 3 4 59 3 5 4 95 7 1 6 98 6 1 9 93 3 2 9 112 7 4 2 107 6 7 7 110 4 3
25. termination of Pesticide Residues in Foods by Acetonitrile Extraction and Partitioning with Magnesium Sulfate Collaborative Study J AOAC Int 2007 90 485 520 4 L Zhao J Stevens Agilent QuEChERS AUAC 5990 4247 JAJP 5 http sitem herts ac uk aeru footprint en index htm 6 http www m5 ws001 squarestart ne jp foundation search html 7 http Wwww mrldatabase com selectvetdrug 0 8 L Zhao D Schultz J Stevens Evaluation of the OuEChERS AOAC Sample Preparation Kit for the Analysis of Pesticide Residues in Apples with LC MS MS Detection Agilent Technologies publication 5990 3937EN www agilent com chem jp www adilent com chem jp
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