Agilent サンプリークQuEChERSAOAC キットをmakeuseしたGC/MS によるホウレン草中の残留農薬 analysis Manual
Contents
1. Agilent Technologies Inc 2009 Published in Japan July 16 2009 5990 4305JAJP2. 2 3 IS SPE SPE 50 ng g GC MS GC MS 4000 A 3500 4 00 6 00 8 00 10 00 12 00 14 00 16 00 18 00 20 00 4000 B 3500 IS 3000 2500 2000 1500 1000 500 03 a 4 00 6 00 8 00 10 00 12 00 14 00 16 00 18 00 20 00 Ne 2 SPE A SPE B GC MS IS TPP 4 00 8 00 8 00 12 00 12 00 EE A
3. GCB C18 GCB SPE GCB GCB SPE
4. LOO Limit of quantitation 10 ng g LOQ 50 ng g QuEChERS MRL Maximum residue limits 10 50 200 ng g Agilent Technologies QuEChERS AUAC USDA 1 3 1 HAc MgS0 PSA SPE
5. 14 1 mL 88 8 8 mL 86 3 1 mL RSD 5 4 8 mL RSD 4 8 4 1 mL 75 3 1 mL RSD 6 1 41 7 RSD 14 9 4 L00 50 ng g 4 AOAC 1 mL 2 mL LC MS MS QC 10 ng g 0C 50 ng g QC 200 ng g RSD RSD RSD 94 0 30 91
6. 4 LC MS MS LC MS MS GC MS SIM LC MS MS MRM GC MS o LOQ 10 ng g oc 20 GC MS
7. 0C 100 pL 100 uL IS 15 ug mL TPP 30 15 mL 1 HAc 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
8. 6 n 6 1 mL 8 mL SPE RSD 4 5 SPE 1 mL 8 mL 8 mL SPE GC 18 4 SPE GCB 50 200 SPE 14 SPE 4
9. SPE 4 SPE AOAC AOAC SPE LC 5 AOAC 5982 5755 AOAC SPE 5982 5222 5982 5258 GC MS 0C 0P 0N GC
10. N 0 1 600 pL ACN GC MS SPE 1 ACN 1 SPE SPE 2 mL 15 g 0 1 g 50 mL TPP 100 uL 0C 1 1 HAc 15 mL ACN AOAC QuEChERS 4 1 4000 rpm 5
11. 17 1 HPLC Me0H Honeywell ACN HAc Sigma Aldrich FA Fluka Sleinheim TPP Sigma Aldrich Chem Service Ultra Scientific 5 10 mL 1L ACN ACN 1 IS 2 mg mL 20 C 1 5 7 5
12. 6 1 NA 50 LA 1 S 0 CI 0 0 3 86 NA 100 Cl MRL GC MS 10 GC Aux EPC Aux EPC MS 5188 5398 19 6 psi 1 0 psi 250 C 1 0 0 75 30 mL min 70 C 1 50 C min 150 C 0
13. 1 mL ACN 1 mL ACN SPE 2 mL SPE 2 mL Y 325 pL 30 30 13 000 rpm 2 13 000 rpm 2 Y 825 pL ACN 600pL 0 1 ACN Y GC MS GC MS QuEChERS AOAC 2 mL SPE SPE 0uEChERS SPE GCB
14. GCB Agilent QuEChERS AOAC SPE i 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 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 S J Lehotay et al Determination of Pesticide Residues in Foods by Acetonit
15. 30 ng mL 3 0C 1 1 ACN H 0 0 1 ACN 0 1 2 5 pg mL 1 1 ACN H 0 0 1 15 ng mL TPP IS Agilent Agilent Technologies Inc Agilent 5975C Agilent Technologies Inc QuEChERS AOAC 5982 5755 Agilent Technologies Inc QuEChERS AOAC SPE 5982 5222 5982 5258 Agilent Technologies Inc CentraCL3R Thermo IEC VWR Eppendorf Brinkmann Instruments 1 6 9 Log P pKa MRL ng g 3 18 9 4 gt OH 2000 1 9 NA 0 10 I 32
16. 1 mL SPE 8 mL SPE RF RF 5 55e 001 9 1 4 71e 001 6 8 oc 2 93e 000 7 9 2 30e 000 9 3 8 34e 001 9 5 6 98e 001 8 1 1 03e 000 8 7 9 25e 001 11 2 7 67e 001 14 2 7 83e 001 13 7 1 26e 000 12 5 1 20e 000 10 3 3 03e 000 9 8 2 61e 000 12 2 6 46e 001 6 9 5 99e 001 11 5 4 36e 002 10 2 3 33e 002 11 4 y 1 73e 001 6 2 1 38e 001 6 4 DDE 2 98e 000 7 4 2 49e 000 6 2 w 1 37e 001 8 1 1 07e 001 8 1 3 41e 001 5 1 2 92e 001 10 6 1 07e 000 15 6 1 42e 000 12 2 3 06e 001 4 6 2 42e 001 4 2 1 14e 000 6 4 1 22e 000 9 7 3 45e 001 6 4 2 64e 001 11 3 SPE 50 400 ng g 10 50 200 ng g 3 0C
17. 6 C min 200 C 0 16 C min 280 C 6 3 Purged Ultimate Union G3186B Purged Ultimate Union 4 0 psi 80 0 psi Agilent J amp W HP 5MS 15 mx 0 25 mm x 0 25 um 19091S 431UI Purged Ultimate Union G3186B 65 cm x 0 15 mm 0 15 um DB 5MS Purged Ultimate Union MSD Atune u SIM 2 230 C 150 C 280 C 2 30 SPE 8 SPE 15 g 0 1 g 50 mL
18. Limian Zhao Joan Stevens Agilent Technologies Inc 2850 Centerville Road Wilmington DE 19809 USA Agilent QuEChERS AO0AC GC MS QuEChERS quick easy cheap effective rugged safe A0AC GC 18 SPE SPE GCB SIM GC MS
19. SPE SPE 8 mL 1 2 GC MS 18 SIM RT 1 184 9 2 3 4 0 2 88 2 oc 170 1 169 1 40 5 0 4 35 3 180 9 182 9 5 0 6 9 6 67 4 137 1 179 1 6 9 7 7 7 19 5 265 8 263 8 6 9 7 7 7 34 6 285 9 287 9 7 7 8 6 8 25 7 250 0 139 0 8 6 10 0 9 55 8 196 8 198 8 8 6 10 0 9 57 9 352 8 354 8 10 0 10 4 10 31 10 259 9 261 9 10 4 10 85 10 75 11 y 372 8 374 8 10 85 11 6 10 97 12 DDE 245 9 317 9 10 85 11 6 11 21 13 wc 372 8 374 8 10 85 11 6 11 50 14 262 9 264 9 11 0 12 3 11 89 15 230 9 12 3 13 6 12 97 16 273 8 12 3 13 6 13 35 TPP IS 325 1 3
20. 0 CI 3 69 NA CI 10 TT Cl lt Cl Cl 3 69 2 6 100 N N 2 IM 2 94 NA N 4000 CI CI CI SS NN CI 4 00 NA CI 30 N Cl Cl 4 44 NA 500 4 7 NA CI x CI 10 Cl N 0 0 P 0 Hc S 1 6 9 Log P pKa MRL ng g a CI CI 5 83 NA 30 CI CI CI CI CI 0 3 02 NA 0 2000 N S CI Cl 0 Cl 2 78 NA CI CI 20 CI CI Cl Cl Cl Cl DDE 6 55 NA Cl CI 50 CI 0 8 CI 3 7 NA CI CI 10 CI CI 0 Cl Cl 5 07 NA 300 2 ss Ss OS S 1 0 1 6 9 Log P pKa MRL ng g 3 13 NA 50 CI CI CI CI Cl ci 0 0
21. 400 ng 9 10 20 50 100 250 400 ng TPP 100 ng g IS IS S 10 ng g LO0 10 ppb 50 ng g LO0 50 ppb MRL 3 1 mL 8 mL SPE RSD 3 17
22. 26 1 13 6 15 0 13 84 17 183 1 15 0 23 0 15 69 15 79 18 362 0 225 9 15 0 23 0 15 83 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 15 mL 4 000 rpm 5 825 uL
23. 7 1055 80 9 46 o 95 0 2 2 92 0 7 9 78 7 3 8 83 7 3 1 93 9 12 2 91 8 3 3 97 3 43 95 6 9 9 91 8 3 3 47 5 6 8 44 9 6 6 49 4 43 74 1 46 717 45 72 2 5 8 97 5 7 6 66 8 3 9 68 8 6 8 88 3 3 0 79 6 35 77 0 35 74 9 19 81 6 117 78 2 3 9 NA NA 98 8 60 77 7 6 7 1060 49 112 2 3 3 93 6 5 3 DDE 80 3 22 86 8 96 754 35 a 107 6 42 108 4 35 91 6 37 99 7 2 6 93 7 96 78 9 34 91 4 34 1000 50 107 4 7 6 93 7 48 97 3 88 89 8 43 84 7 5 7 74 8 9 9 84 6 6 0 98 4 55 84 2 95 81 2 3 2 SPE 12 5 AOAC 8 mL 15 mL GC MS QC 10 ng g 0C 50 ng g QC 200 ng g RSD RSD RSD 93 7 2 6 92 5 4 2 66 2 5 9 o 87 9 5 1 92 5 6 6 95 2 6 3 83 1 5 1 85 4 2 9 64 5 5 2
24. 85 8 6 9 85 2 2 9 87 3 5 5 21 1 49 7 23 6 14 3 23 2 14 0 76 4 2 4 73 9 2 7 73 8 3 6 93 3 4 1 56 6 2 0 61 4 4 5 77 8 3 6 70 2 4 6 69 0 3 1 78 6 4 6 79 6 2 6 85 3 5 1 NA NA 60 3 17 4 53 7 10 7 yy 106 8 5 7 110 7 3 5 100 4 4 9 DDE 80 8 4 2 81 8 2 6 81 3 4 9 ga 104 2 6 2 103 6 3 3 95 8 5 3 96 4 6 2 93 0 1 2 79 3 5 3 83 8 4 0 82 8 2 3 85 3 4 9 90 5 8 8 87 5 7 3 84 5 6 4 84 0 4 9 78 4 6 8 79 5 10 7 61 2 22 2 42 6 28 8 35 3 20 6 SPE GCB SPE Agilent QuEChERS AUAC SPE SPE SPE
25. OAC AOAC 50 ng g GC MS 16 00 18 00 20 00 14 00 16 00 18 00 20 00 3 SPE A SPE B 50 ng g GC MS 1 2 oc 3 4 5 6 7 8 9 10 11 12 DDE 13 oc 14 15 16 17 18 IS TPP L00 10 400 ng g 50
26. rile Extraction and Partitioning with Maqnesium Sulfate Collaborative Study J AOAC Int 2007 90 485 520 L Zhao J Stevens Agilent AOAC QuEChERS 5990 4247JAJP L Zhao J Stevens Agilent QuEChERS AO0AC LC MS MS 5990 4248JAJP http sitem herts ac uk aeru footprint en index htm http www m5 ws001 squarestartne jp foundation search html http Wwww mrldatabase com selectvetdrug 0 Agilent Technologies 9 http Wwww ams usda gov AMSv1 0 getfile dDoc Name PDP1995Summary 10 P L Wylie C K Meng A Method for the Trace Analysis of 175 Pesticides Using the Agilent Triple Quadrupole GC MS MS Agilent Technologies publication 5990 3578EN www agilent com chem jp www agilent com chem jp
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