32 1 2013 1 FENXI CESHI XUEBAO Journal of Instrumental Analysis Vol. 32 No. 1 9 ~ 22-290 1 2 1* 2 2 2 2* 1. 710021 2. 100123 290 QuEChERS N- PSA Thermo Accucore aq 100 mm 2. 1 mm 2. 6 μm MRM 290 1. 0 ~ 200 μg L - 1 0. 99 3 MRL 2MRL 4MRL 290 67% ~ 119% LOQ S /N 10 10. 0 μg kg - 1 - QuEChERS O657. 63 TQ460. 72 doi 10. 3969 /j. issn. 1004-4957. 2013. 01. 002 A 1004-4957 2013 01-0009 - 14 Determination of 290 Pesticide Residues in Tea by High Performance Liquid Chromatography - Tandem Mass Spectrometry JIA Wei 1 2 HUANG Jun-rong 1* LING Yun 2 FENG Feng 2 ZHENG Yue-ming 2 CHU Xiao-gang 2* 1. College of Life Science and Engineering Shaanxi University of Science and Technology Xi'an 710021 China 2. Chinese Academy of Inspection and Quarantine Beijing 100123 China Abstract A simple and rapid method was developed for the simultaneous determination of 290 pesticide residues in tea. The sample was prepared by the modified QuEChERS quick easy cheap effective rugged and safe method extracted with acetonitrile followed by liquid - liquid partitioning formed by adding sodium chloride and anhydrous magnesium sulfate. The extract was separated on a Thermo Accucore aq 100 mm 2. 1 mm 2. 6 μm column detected by high performance liquid chromatography - tandem mass spectrometry under multiple reaction monitoring mode and quantified by the external standard method. The calibration curves of 290 pesticide residues were linear in the range of 1. 0-200 μg L - 1 with correlation coefficients more than 0. 99. The recoveries for all compounds in tea at the fortified levels of 1MRL 2MRL and 4MRL were 67% - 119%. The limits of quantitation LOQs S /N 10 for 290 pesticides were less than 10. 0 μg kg - 1. The established method was successfully used for the screening and determination of real samples such as green tea black tea oolong tea and pu er tea bought at supermarket. The method was simple rapid and reliable and could meet the requirement for simultaneous determination of 290 pesticide residues in tea. Key words high performance liquid chromatography - tandem mass spectrometry QuEChERS pesticide residues tea CAC 2012-09 - 04 2012-10 - 04 2011BAK10B04 201310167-2 * Tel 010-85778904 E - mail xgangchu@ 163. com Tel 029-86168663 E - mail huangjunrong2000@ 163. com
10 32 MRL 0. 10 ~ 50. 0 0. 01 ~ 30. 0 0. 01 ~ 30. 0 mg /kg 0. 01 mg /kg 1 ELISA 2 GC 3-4 - GC - MS 5-7 HPLC 8 - LC - MS 9-10 - LC - MS /MS 11-14 ELISA GC HPLC GC - MS LC - MS - LC - MS /MS LC - MS /MS 200 3 QuEChERS 15-2003 Oringinal AOAC 2007. 12008 CEN 15662 17-3 QuECh- ERS QuEChERS 290 1 1. 1 TSQ Quantum Ultra - Thermo Fisher Scientific Avnti J - 26 PI Beckman Coulter Vortex. Genie2T Scientific Industries Yamata SA31 0. 20 μm Pall Caliper HPLC Thermo Fisher Scientific C 18 N- PSA 40 ~ 60 μm 100 GCB 40 ~ 120 μm Supelco 500 4 h Sigma Sigma Milli-Q 290 Dr. Ehrenstorfer 1 000. 0 mg /L - 24 1 1 10 5 ml 15 ml 1 000 μg /L 10 20 50 100 200 500 1 000 2 000 4 000 5 000 μl 5 ml 5 8 mmol /L 1. 0 2. 0 5. 0 10 20 50 100 200 400 500 μg /L 1. 2 1. 2. 1 Accucore aq 100 mm 2. 1 mm 2. 6 μm Accucore C 18 10 mm 2. 1 mm 2. 6 μm Thermo Fisher Scientific 35 A 0. 1% - 4 mmol /L B 0. 1% - 4 mmol /L 0 ~ 1 min 100% A 1 ~ 35 min 100% ~ 0% A 35 ~ 40 min 0% A 40 ~ 40. 1 min 0% ~ 100% A 40. 1 ~ 45 min
1-290 11 100% A 300 μl /min 99. 999% 0. 2 Pa 10 μl 1. 2. 2 275 kpa 3 L / min 3 000 V 2 500 V Tube lens 152 V Skimmer 20 V 350 295 0. 2 s EZ MRM 1 1. 3 0. 3 mm 10 g 0. 01 g 50 ml 20 ml 30 min 20 ml 1% - 2. 0 g 30 s 6. 0 g 1. 5 g 30 s 5 min 10 000 r / min 5 min 10 ml 75 mg GCB 400 mg PSA 1. 2 g 30 s 0. 7 ml 30 s 10 000 r /min 5 min 0. 20 μm 200 μl 300 μl 500 μl 8 mmol /L - 2 2. 1 1 400 DMSA 90 70% 130% 10 290 2. 2 ESI + ESI - 290 2 MRM 1 1 2. 3 2. 3. 1 Thermo Scientific Accucore 2. 6 μm Accucore RP - MS C 18 aq 3 HPLC 100 mm 2. 1 mm 2. 6 μm 290 Accucore aq 2. 3. 2 - - 290 Parathion Fenitrothion Dimethoate Schradan Dioxacarb Mefenacet - 1 6 - Fig. 1 Chromatographic response of 6 pesticides in different mobile phases
12 32 1 0. 1% - 4 mmol /L 0. 1% - 4 mmol /L 2 1. 3 2 290 20 μg /L Fig. 2 Total ion current chromatograms of 290 pesticides standard at 20 μg / L prepared in oolong tea A. standard solution prepared with the solvent B. matrix-matched standard solution 2. 4 2. 4. 1 30 min 1. 3 6. 0 g 6. 0 g 10 μg /L Mefenacet Ethoprophos Fenamidone Cumyluron Dipropetryn Azoxystrobin 6 3
1-290 13 PSA 18 ph 2003 Oringinal AOAC 2007. 01 CEN 151662 1. 5 g 3 2 QuEChERS 10 μg /L 1% AOAC 2007. 01 n = 7 0. 5 g 1. 0 g Fig. 3 Comparison of recoveries of two versions of QuEChERS sample preparation method for oolong tea CEN 151662 Oringinal 10 μg /L samples spiked with 10 μg /L pesticides n = 7 Para- thion Fenitrothion Dimethoate Schradan Dioxacarb Carbendazim 6 4 ph 5. 0 ~ 5. 5 4 3 QuEChERS 10 μg /L ph n = 7 5. 0 ~ 5. 5 4. 8 6 Fig. 4 Comparison of recoveries of three versions of QuEChERS sample preparation method for oolong tea samples spiked with 10 μg /L pesticides n = 7 2. 4. 2 Oringinal AOAC 2007. 01 CEN 151662 C 18 GCB C 18 C 18 500 mg C 18 C 18 10 μg /L Mefenacet Ethoprophos Fenamidone Cumyluron Dipropetryn Azoxystrobin 6 5 2 QuEChERS 10 μg /L 5 n = 7 Fig. 5 Comparison of recoveries of two versions of C 18 QuEChERS sample preparation method for oolong tea samples spiked with 10 μg /L pesticides n = 7 CEN 151662
14 32 GCB GCB PSA GCB 10 ml 40 45 50 55 60 65 70 75 80 85 mg GCB 30 s 10 000 r /min 5 min 75 mg GCB GCB 6 6 GCB Fig. 6 Influence of toluene volume used in purification on recoveries of 8 pesticides Ethoprophos Azaconazole Fenbuconazole Tebufenpyrad Carbofuran Pyrimethanil GCB 75 mg GCB 10 μg /L 6 6 0. 7 ml GCB Dichlorvos Fenuron 10 ml 75 mg GCB 400 mg PSA 1. 2 g 30 s 0. 7 ml 2003 Oringinal AOAC 2007. 01 CEN 151662 PSA QuEChERS 1. 3 2. 4. 3 2 = 1 - / 100% 19 290 19. 2% 2. 5% 79. 3% 20 μg /L 7 1. 2 s 1 ~ 9 María 20 2. 5 2. 5. 1 290 1. 0 2. 0 5. 0 10 20 50 100 200 μg /L y x μg /L r 2 0. 99 1. 0 ~ 200 μg /L S /N 10 290 0. 01 mg /kg 2. 5. 2 CAC MRL 0. 01 mg /kg 1 2 4 61% ~ 119% 7
1-290 15 12. 4% MRL 0. 01 mg /kg 1 1 290 r 2 n = 7 Table 1 Retention times mass spectrometric parameters correlation coefficients r 2 recoveries and precisions of 290 pesticides n = 7 No. Pesticide Linear range Spiked t R Transition Recovery RSD CE /ev ρ / μg r 2 w / mg /min m /z R 珔 /% s L - 1 kg - 1 r /% 1 Aldicarb sulfoxide 0. 86 207. 0 /132. 0 * 207. 0 /89. 0 16 10 10 ~ 200 0. 998 7 0. 10 84 6. 5 2 Methamidophos 0. 86 142. 0 /94. 0 * 142. 0 /125. 0 20 10 5 ~ 200 0. 995 7 0. 10 94 5. 6 3 Omethoate 0. 86 214. 1 /183. 0 * 214. 1 /155. 0 18 13 15 ~ 200 0. 990 6 0. 05 75 5. 3 4 Pymetrozine 0. 86 218. 0 /105. 0 * 218. 0 /79. 0 30 25 5 ~ 200 0. 994 8 0. 01 102 5. 7 5 Acephate 0. 87 184. 1 /143. 1 * 184. 1 /95. 2 25 10 5 ~ 200 0. 999 0 0. 01 91 4. 2 6 Cyromazine 0. 87 167. 1 /85. 2 * 167. 1 /68. 2 28 26 19 5 ~ 200 0. 990 7 0. 01 96 5. 7 7 Fonophos 0. 88 247. 0 /109. 1 * 247. 0 /137. 1 23 12 5 ~ 200 0. 995 5 0. 01 95 4. 3 8 Dinotefuran 0. 89 203. 0 /129. 0 * 203. 0 /114. 0 15 10 5 ~ 200 0. 995 3 0. 01 96 5. 1 9 Aminocarb 2. 25 209. 1 /137. 1 * 209. 1 /152. 1 25 15 5 ~ 200 0. 997 6 0. 01 97 4. 8 10 Propamocarb 2. 91 189. 1 /102. 1 * 189. 1 /144. 1 19 14 5 ~ 200 0. 996 9 0. 01 85 3. 7 11 Methomyl 4. 27 272. 2 /198. 0 * 272. 2 /240. 0 10 10 5 ~ 200 0. 997 1 0. 01 99 4. 7 12 Carbendazim 4. 52 192. 1 /160. 1 * 192. 1 /132. 1 33 20 5 ~ 200 0. 999 2 0. 01 97 3. 8 13 Nitenpyram 5. 64 271. 2 /225. 0 * 271. 2 /237. 0 12 20 5 ~ 200 0. 998 9 0. 01 111 3. 8 14 Thiabendazole 5. 76 202. 0 /175. 1 * 202. 0 /131. 1 35 28 5 ~ 200 0. 999 9 0. 10 96 4. 3 15 Thiamethoxam 6. 02 292. 2 /211. 1 * 292. 2 /132. 1 24 14 5 ~ 200 0. 992 7 0. 01 97 5. 6 16 Mexacarbate 6. 24 224. 1 /193. 1 * 224. 1 /127. 1 26 16 5 ~ 200 0. 998 0 0. 01 98 6. 1 17 Dicrotophos 6. 38 238. 1 /193. 1 * 238. 1 /112. 1 14 10 5 ~ 200 0. 997 2 0. 01 95 5. 0 18 Dichlorvos 6. 39 238. 0 /127. 0 * 238. 0 / 109. 0 238. 0 /221. 0 24 24 18 10 ~ 200 0. 993 8 0. 10 97 5. 6 19 Fuberidazole 6. 42 185. 1 /157. 0 * 185. 1 / 130. 2 185. 1 /156. 0 23 29 23 10 ~ 200 0. 999 5 0. 10 100 4. 1 20 Fenuron 7. 01 165. 0 /72. 1 * 165. 0 /46. 3 18 17 5 ~ 200 0. 998 9 0. 01 89 4. 9 21 Clothianidin 7. 25 250. 1 /169. 1 * 250. 1 /132. 1 18 14 5 ~ 200 0. 991 5 0. 01 99 6. 0 22 Diamidafos 7. 56 201. 1 /107. 2 * 201. 1 /95. 2 * 28 29 10 ~ 200 0. 991 4 0. 1 98 3. 9 23 Vamidothion 7. 58 288. 1 /146. 1 * 288. 1 /118. 1 27 14 5 ~ 200 0. 997 3 0. 01 82 4. 6 24 Ethidimuron 7. 66 265. 1 /208. 2 * 265. 1 /114. 2 20 16 5 ~ 200 0. 997 3 0. 02 96 6. 4 25 Mevinphos 7. 69 225. 1 /127. 1 * 225. 1 /192. 8 15 8 5 ~ 200 0. 991 3 0. 01 88 6. 2 26 Carbofuran-3-hydroxy 7. 72 238. 1 /181. 1 * 238. 1 /220. 1 11 9 5 ~ 200 0. 998 9 0. 01 85 7. 0 3-27 Phorate 7. 75 261. 0 /75. 1 * 261. 0 /142. 9 14 19 5 ~ 200 0. 991 7 0. 01 90 3. 9 28 Imidacloprid 7. 79 256. 1 /209. 1 * 256. 1 /175. 1 20 18 1 ~ 200 0. 995 8 0. 01 107 5. 6 29 Bendiocarb 7. 97 224. 2 /167. 1 * 224. 2 /109. 1 20 10 5 ~ 200 0. 992 8 0. 01 73 5. 5 30 Dioxacarb 7. 97 224. 1 /167. 1 * 224. 1 /123. 1 18 10 5 ~ 200 0. 996 9 0. 02 81 4. 7 31 Dimethoate 7. 99 230. 1 /199. 1 * 230. 1 /125. 1 23 12 5 ~ 200 0. 997 7 0. 01 106 6. 5 32 Schradan 8. 12 287. 1 /242. 0 * 287. 1 / 40 26 14 5 ~ 200 0. 990 8 0. 01 95 5. 5 92. 2 287. 1 /135. 1 33 Dimetilan 8. 58 241. 1 /72. 2 * 241. 1 /171. 2 21 13 5 ~ 200 0. 996 5 0. 01 83 5. 5 34 Butoxycarboxin 8. 65 223. 1 /86. 2 * 223. 1 /106. 1 20 10 20 ~ 200 0. 991 1 0. 10 96 4. 8 35 Pirimicarb 8. 70 239. 1 /182. 0 * 239. 1 /72. 0 21 16 20 ~ 200 0. 998 2 0. 10 79 6. 4 36 Monocrotophos 8. 72 224. 1 /127. 1 * 224. 1 /193. 1 28 19 5 ~ 200 0. 998 5 0. 01 99 7. 0 37 Acetamiprid 8. 74 223. 1 /126. 1 * 223. 1 /90. 2 36 22 10 ~ 200 0. 998 6 0. 05 97 6. 3 38 Acibenzolar-S-methyl 8. 97 211. 1 /140. 0 * 32 24 1 ~ 200 0. 999 3 0. 01 95 -S- 211. 1 /136. 0 4. 7 39 Ethirimol 8. 97 210. 2 /140. 1 * 210. 2 /98. 1 28 23 5 ~ 200 0. 999 3 0. 01 90 7. 6 40 Tricyclazole 9. 36 190. 1 /163. 1 * 190. 1 /136. 1 30 24 5 ~ 200 0. 999 3 0. 01 78 4. 5 41 Thiacloprid 10. 27 253. 1 /126. 1 * 253. 1 /90. 2 37 22 5 ~ 200 0. 999 6 0. 01 78 6. 3 42 Matoxuron 10. 38 229. 0 /72. 2 * 229. 0 /156. 0 24 25 10 ~ 200 0. 994 8 0. 10 86 7. 3 43 Allidochlor 10. 56 174. 1 /98. 2 * 174. 1 / 39. 4 174. 1 /41. 4 45 23 12 5 ~ 200 0. 997 8 0. 01 98 6. 6 44 Pyroquilon 10. 56 174. 1 /132. 1 * 174. 1 / 31 38 23 5 ~ 200 0. 998 1 0. 01 107 2. 5 117. 2 174. 1 /130. 1 45 Tebuthiuron 10. 56 229. 2 /172. 1 * 229. 2 /116. 1 28 18 5 ~ 200 0. 997 8 0. 01 105 6. 7
16 32 1 No. Pesticide Linear range Spiked t R Transition Recovery RSD CE /ev ρ / μg r 2 w / mg /min m /z R 珔 /% s L - 1 kg - 1 r /% 46 Carbetamide 10. 62 237. 1 /192. 1 * 237. 1 /118. 1 15 10 5 ~ 200 0. 994 4 0. 01 79 6. 9 47 Oxamyl 10. 62 237. 1 /72. 1 * 237. 1 /90. 1 15 10 5 ~ 200 0. 991 4 0. 01 98 4. 4 48 Fenpiclonil 10. 75 254. 1 /172. 0 * 254. 1 /202. 0 17 13 5 ~ 200 0. 996 5 0. 01 77 3. 5 49 Hexazinone 10. 75 253. 1 /171. 0 * 253. 1 / 30 29 17 1 ~ 200 0. 998 9 0. 01 88 4. 1 71. 3 253. 1 /85. 2 50 Simazine 10. 99 202. 1 /132. 0 * 202. 1 /104. 0 27 20 5 ~ 200 0. 999 1 0. 01 106 7. 2 51 Chlorpropham 11. 07 214. 0 /172. 0 * 214. 0 /154. 0 19 12 5 ~ 200 0. 996 2 0. 01 98 4. 9 52 Desmetryn 11. 07 214. 1 /172. 1 * 214. 1 / 33 30 18 5 ~ 200 0. 997 9 0. 01 95 7. 8 57. 3 214. 1 /82. 2 53 Simetryne 11. 09 214. 1 /124. 0 * 214. 1 /96. 0 26 20 25 ~ 200 0. 998 0 0. 05 92 6. 0 54 Octhilinone 11. 10 214. 1 /102. 1 * 214. 1 / 17 16 14 5 ~ 200 0. 991 9 0. 01 99 6. 3 172. 1 214. 1 /57. 4 55 Flucarbazone 11. 12 397. 1 /129. 9 * 397. 1 /115. 0 48 21 5 ~ 200 0. 990 1 0. 01 107 4. 5 56 Thidiazuron 11. 22 221. 1 /102. 1 * 221. 1 /94. 2 14 16 5 ~ 200 0. 998 1 0. 05 102 5. 9 57 Metribuzin 11. 24 225. 1 /127. 1 * 225. 1 /192. 8 17 17 5 ~ 200 0. 998 2 0. 01 107 6. 4 58 Mephospholan 11. 31 270. 0 /140. 0 * 270. 0 / 25 17 14 5 ~ 200 0. 996 7 0. 01 103 6. 3 168. 0 270. 0 /196. 0 59 Oxadixyl 11. 40 279. 0 /219. 0 * 279. 0 /132. 0 25 15 5 ~ 200 0. 992 8 0. 01 100 5. 8 60 Ancymidol 11. 45 257. 1 /135. 0 * 257. 1 / 45 26 26 5 ~ 200 0. 992 7 0. 01 98 6. 1 77. 2 257. 1 /81. 2 61 Cyanazine 11. 67 241. 1 /214. 0 * 241. 1 /226. 0 17 12 45 ~ 200 0. 997 1 0. 1 91 3. 8 62 Imazaquin 11. 67 312. 0 /199. 0 * 312. 0 / 252. 0 312. 0 /267. 0 30 27 22 1 ~ 200 0. 997 6 0. 01 109 7. 6 63 Azamethiphos 11. 92 325. 0 /182. 9 * 325. 0 / 112. 0 325. 0 /139. 0 36 23 17 25 ~ 200 0. 991 9 0. 05 97 5. 0 64 Prometon 12. 21 226. 2 /141. 9 * 226. 2 /184. 0 24 21 5 ~ 200 0. 997 6 0. 01 85 4. 7 65 Secbumeton 12. 21 226. 2 /169. 9 * 226. 2 /99. 9 33 19 5 ~ 200 0. 998 5 0. 01 71 6. 0 66 Bentazone 12. 22 239. 1 /197. 0 * 239. 1 /132. 0 28 22 30 ~ 200 0. 993 7 0. 1 91 6. 0 67 Thiophanate methyl 12. 28 343. 2 /151. 1 * 343. 2 /311. 2 24 12 5 ~ 200 0. 996 1 0. 01 96 6. 2 68 Propoxur 12. 31 210. 1 /111. 1 * 210. 1 /168. 1 16 10 5 ~ 200 0. 995 2 0. 01 92 5. 7 69 Diphenylamine 12. 57 170. 1 /114. 1 * 170. 1 / 26 22 17 5 ~ 200 0. 993 8 0. 01 98 4. 1 69. 2 170. 1 /100. 1 70 Terbumeton 12. 57 226. 2 /169. 9 * 226. 2 /113. 9 25 20 5 ~ 200 0. 998 4 0. 01 92 5. 9 71 Bufencarb 12. 59 222. 1 /77. 2 * 222. 1 /95. 2 43 34 5 ~ 200 0. 995 2 0. 01 81 6. 7 72 Carbofuran 12. 59 222. 1 /165. 1 * 222. 1 /123. 1 25 14 5 ~ 200 0. 993 3 0. 05 86 7. 4 73 Methabenzhiazuron 12. 59 222. 1 /165. 0 * 222. 1 /137. 0 17 20 5 ~ 200 0. 995 8 0. 01 95 6. 0 74 Pyracarbolid 12. 84 218. 2 /124. 9 * 218. 2 /96. 9 31 21 5 ~ 200 0. 996 6 0. 01 88 7. 7 75 Florasulam 12. 87 360. 0 /129. 0 * 360. 0 /192. 0 26 18 5 ~ 200 0. 990 4 0. 01 105 6. 0 76 Imazapyr 12. 90 262. 1 /217. 0 * 262. 1 /202. 0 27 19 5 ~ 200 0. 998 7 0. 01 100 4. 8 77 Zoxamide 13. 02 336. 2 /187. 0 * 336. 2 /159. 0 38 23 5 ~ 200 0. 996 6 0. 01 83 4. 1 78 Flumetsulam 13. 05 326. 0 /109. 0 * 326. 0 /109. 0 53 53 5 ~ 200 0. 992 8 0. 01 95 6. 8 79 Fenthion sulfone 13. 11 328. 1 /311. 0 * 328. 1 /109. 1 37 9 5 ~ 200 0. 990 6 0. 01 106 5. 0 80 Mefluidide 13. 12 328. 1 /311. 0 * 328. 1 / 41 30 14 10 ~ 200 0. 990 6 0. 05 104 8. 8 121. 1 328. 1 /135. 1 81 Pyrosulam 13. 20 434. 9 /194. 1 * 434. 9 /174. 1 39 43 5 ~ 200 0. 990 2 0. 01 93 4. 9 82 Fenthion sulfoxide 13. 33 294. 9 /108. 9 * 294. 9 /114. 9 32 27 5 ~ 200 0. 994 1 0. 01 95 5. 2 83 Chlortoluron 13. 34 213. 1 /140. 0 * 213. 1 /168. 0 22 20 15 ~ 200 0. 995 4 0. 10 96 6. 5 84 Ametryn 13. 51 228. 2 /185. 9 * 228. 2 /96. 0 26 19 5 ~ 200 0. 996 2 0. 01 96 6. 4 85 Methoprotryne 13. 56 259. 1 /170. 0 * 259. 1 /148. 0 15 10 5 ~ 200 0. 994 9 0. 01 82 5. 4 86 Fluometuron 13. 68 233. 1 /72. 1 * 233. 1 /46. 3 17 18 5 ~ 200 0. 993 3 0. 01 85 5. 4 87 Cycluron 13. 75 199. 1 /89. 1 * 199. 1 /72. 2 24 16 5 ~ 200 0. 997 4 0. 01 104 7. 2 88 Ethiofencarb 13. 87 226. 1 /107. 0 * 226. 1 /169. 0 16 9 5 ~ 200 0. 995 4 0. 01 119 5. 3 89 Forchlorfenuron 13. 94 248. 1 /129. 0 * 248. 1 /93. 0 36 18 5 ~ 200 0. 992 3 0. 01 114 6. 4 90 Pyrimethanil 14. 01 200. 1 /107. 0 * 200. 1 /82. 0 30 26 5 ~ 200 0. 998 5 0. 01 83 5. 2 91 Ethaboxam 14. 10 321. 0 /183. 1 * 321. 0 /200. 1 24 28 5 ~ 200 0. 995 2 0. 01 88 4. 7 93 Flutriafol 14. 13 302. 2 /70. 1 * 302. 2 /123. 0 19 33 5 ~ 200 0. 991 1 0. 01 92 6. 5
1-290 17 1 No. Pesticide Linear range Spiked t R Transition Recovery RSD CE /ev ρ / μg r w / mg /min m /z R /% s L - 1 kg - 1 r /% 94 Isoproturon 14. 25 207. 1 /72. 0 * 207. 1 /165. 2 19 14 5 ~ 200 0. 999 8 0. 01 102 6. 3 95 Metalaxyl 14. 29 280. 1 /220. 1 * 280. 1 /192. 1 16 16 5 ~ 200 0. 998 1 0. 01 95 7. 0 96 Diuron 14. 37 233. 1 /72. 0 * 233. 1 /46. 3 35 20 1 ~ 400 0. 992 7 0. 01 105 7. 8 97 Azaconazole 14. 45 300. 0 /158. 9 * 300. 0 / 123. 0 300. 0 /230. 9 51 27 17 5 ~ 200 0. 998 7 0. 01 83 6. 5 98 Diazinon oxon 14. 55 289. 0 /233. 0 * 289. 0 /274. 0 20 12 10 ~ 200 0. 991 0 0. 10 95 5. 4 99 Metosulam 14. 56 215. 1 /131. 0 * 215. 1 /187. 1 45 27 24 5 ~ 200 0. 993 2 0. 01 92 6. 5 100 Isoprocarb 14. 71 194. 1 /137. 0 * 194. 1 /95. 0 16 11 5 ~ 200 0. 996 0 0. 01 100 5. 1 101 Norflurazon 14. 98 304. 1 /284. 0 * 304. 1 /88. 0 39 25 5 ~ 200 0. 999 3 0. 01 96 5. 4 102 Imazamox 14. 99 306. 1 /193. 1 * 306. 1 /261. 1 27 23 5 ~ 200 0. 994 4 0. 01 101 6. 7 103 Atrazine 15. 08 216. 0 /174. 0 * 216. 0 /201. 0 16 12 5 ~ 200 0. 997 1 0. 05 103 7. 4 104 Azafenidrin 15. 08 338. 1 /264. 0 * 338. 1 / 299. 0 338. 1 /302. 1 30 20 17 25 ~ 200 0. 994 2 0. 05 105 5. 2 105 Terbufos sulfone 15. 08 338. 1 /115. 0 * 338. 1 / 42 31 16 5 ~ 200 0. 994 4 0. 01 102 97. 1 338. 1 /171. 0 4. 9 106 Propachlor 15. 11 212. 1 /170. 0 * 212. 1 / 41 25 15 5 ~ 200 0. 990 3 0. 01 102 4. 6 77. 2 212. 1 /94. 1 107 Metazachlor 15. 30 278. 0 /134. 1 * 278. 0 /105. 1 41 24 5 ~ 200 0. 999 6 0. 01 103 3. 7 108 Demeton-O 15. 37 259. 0 /89. 1 * 259. 0 /61. 2 29 11 5 ~ 200 0. 999 6 0. 5 109 7. 3 109 Demeton-S 15. 37 259. 0 /89. 3 * 259. 0 /61. 2 47 9 5 ~ 200 0. 995 5 0. 01 101 5. 5 110 Pyrifenox 15. 55 295. 0 /93. 1 * 295. 0 / 67. 2 295. 0 /92. 1 50 52 26 25 ~ 200 0. 994 4 0. 10 94 7. 8 111 Flonicamid 15. 78 230. 1 /174. 1 * 230. 1 /135. 1 18 20 5 ~ 200 0. 999 0 0. 01 81 7. 5 112 Prothoate 15. 79 286. 0 /97. 0 * 286. 0 /116. 0 35 29 5 ~ 200 0. 992 2 0. 01 97 7. 1 113 Carbary 15. 80 202. 1 /145. 0 * 202. 1 /127. 0 30 12 5 ~ 200 0. 990 1 0. 01 76 6. 0 114 Ethoxyquin 15. 80 218. 0 /174. 0 * 218. 0 /160. 0 34 34 5 ~ 200 0. 997 1 0. 01 107 5. 0 115 Diphenamid 15. 85 240. 1 /134. 1 * 240. 1 / 165. 1 240. 1 /167. 1 21 48 24 5 ~ 200 0. 998 2 0. 01 89 7. 7 116 Nuarimol 15. 85 315. 1 /251. 9 * 315. 1 /81. 0 36 26 5 ~ 200 0. 994 4 0. 01 104 3. 1 117 Amicarbazone 15. 97 242. 2 /85. 2 * 242. 2 /143. 1 32 12 25 ~ 200 0. 998 0 0. 10 99 5. 7 118 Prometryn 15. 97 242. 2 /157. 9 * 242. 2 /199. 9 24 20 5 ~ 200 0. 997 6 0. 01 98 6. 0 119 Penoxsulam 16. 05 484. 1 /195. 2 * 484. 1 /194. 7 36 29 5 ~ 200 0. 995 8 0. 01 118 6. 2 120 Propanil 16. 16 216. 0 /160. 0 * 216. 0 /64. 0 21 30 5 ~ 200 0. 995 3 0. 01 96 6. 8 121 Imazalil 16. 23 297. 2 /159. 0 * 297. 2 /201. 0 24 18 5 ~ 200 0. 998 3 0. 01 102 8. 0 122 Chlorantraniliprole 16. 24 482. 1 /283. 8 * 482. 1 /450. 9 19 21 5 ~ 200 0. 995 5 0. 01 97 7. 3 123 Terbutryn 16. 26 242. 2 /185. 9 * 242. 2 /91. 0 28 20 5 ~ 200 0. 996 6 0. 10 105 5. 2 124 Coumaphos oxon 16. 36 347. 0 /290. 9 * 347. 0 / 210. 9 347. 0 /318. 9 28 18 14 5 ~ 200 0. 998 2 0. 01 99 4. 0 125 Siduron 16. 55 233. 1 /137. 0 * 233. 1 /94. 0 38 20 5 ~ 200 0. 997 8 0. 01 80 5. 6 126 Paclobutrazole 16. 74 294. 1 /70. 0 * 294. 1 /125. 0 20 35 5 ~ 200 0. 995 8 0. 01 75 7. 4 127 Triadimenol 16. 74 296. 1 /70. 0 * 296. 1 /113. 0 15 12 5 ~ 200 0. 992 0 0. 01 96 6. 9 128 Fensulfothion 16. 84 309. 2 /163. 0 * 309. 2 /251. 0 18 21 5 ~ 200 0. 993 8 0. 01 112 5. 3 129 Clofentezine 17. 08 303. 1 /102. 0 * 303. 1 /138. 0 36 18 5 ~ 200 0. 999 7 0. 01 97 6. 3 130 Furalaxyl 17. 11 302. 1 /95. 0 * 302. 1 /242. 1 35 17 5 ~ 200 0. 993 3 0. 01 71 6. 4 131 Cyproconazole 17. 14 292. 1 /125. 0 * 292. 1 /267. 0 32 26 5 ~ 200 0. 992 3 0. 01 107 6. 6 132 Fenitrothion 17. 16 277. 9 /246. 0 * 277. 9 /125. 1 21 17 5 ~ 200 0. 990 9 0. 01 85 6. 7 133 Triticonazole 17. 16 318. 1 /70. 0 * 318. 1 /125. 0 25 30 5 ~ 200 0. 996 2 0. 01 107 5. 9 134 Desmedipham 17. 19 318. 2 /136. 0 * 318. 2 /182. 0 28 15 50 ~ 200 0. 995 0 0. 10 92 6. 3 135 Phenmedipham 17. 19 301. 2 /136. 0 * 301. 2 /168. 0 22 10 5 ~ 200 0. 993 0 0. 01 104 6. 7 136 Benthiavalicarb 17. 22 382. 1 /180. 0 * 382. 1 /116. 0 23 33 5 ~ 200 0. 999 7 0. 01 76 6. 7 137 Butocarboxin 17. 45 208. 1 /91. 4 * 208. 1 /109. 2 39 15 5 ~ 200 0. 994 6 0. 01 100 6. 7 138 Promecarb 17. 45 208. 1 /109. 0 208. 1 /151. 0 * 17 10 5 ~ 200 0. 999 5 0. 01 110 5. 2 139 Isofenfos O-analog 17. 46 330. 2 /121. 1 * 330. 2 /111. 1 43 45 5 ~ 200 0. 996 6 0. 01 103 6. 4 140 Spirotetramat 17. 65 374. 2 /302. 2 * 374. 2 /330. 2 19 17 20 ~ 200 0. 999 7 0. 10 98 6. 2 141 Carpropamid 17. 68 334. 0 /103. 0 * 334. 0 / 139. 0 334. 0 /196. 0 38 22 14 5 ~ 200 0. 995 0 0. 01 117 5. 5
18 32 1 No. Pesticide t R /min Transition m /z 142 Fludioxonil 17. 74 247. 0 /180. 0 * 247. 0 / 126. 2 247. 0 /169. 1 143 Halofenozide 17. 84 329. 1 /121. 1 * 329. 1 / 77. 3 329. 1 /155. 1 144 Dimethametryn 17. 9 256. 1 /186. 1 * Linear range Spiked Recovery RSD CE /ev ρ / μg r w / mg R /% s L - 1 kg - 1 r /% 34 32 34 5 ~ 200 0. 995 3 0. 01 99 5. 3 37 22 29 5 ~ 200 0. 993 7 0. 01 85 6. 3 256. 1 /213. 1 22 11 5 ~ 200 0. 997 4 0. 01 99 4. 0 145 Iprovalicarb 18. 00 321. 2 /119. 0 * 321. 2 /203. 0 20 10 5 ~ 200 0. 994 6 0. 01 92 5. 4 146 Diclobutrazol 18. 03 328. 1 /159. 0 * 328. 1 /70. 2 25 35 5 ~ 200 0. 993 1 0. 01 100 3. 1 147 Etaconazole 18. 03 328. 2 /159. 0 * 328. 2 /123. 0 58 32 20 ~ 200 0. 997 7 0. 10 101 5. 6 148 Fenamiphos 18. 04 304. 0 /217. 0 * 304. 0 /234. 0 24 8 5 ~ 200 0. 995 2 0. 01 107 5. 3 149 Uniconazole 18. 09 292. 1 /70. 2 * 292. 1 /125. 0 25 32 5 ~ 200 0. 990 4 0. 01 103 5. 9 150 Parathion 18. 14 292. 0 /236. 0 * 292. 0 /97. 0 30 15 5 ~ 200 0. 998 5 0. 01 106 5. 1 151 Mefenacet 18. 15 299. 2 /148. 0 * 299. 2 /120. 1 31 14 5 ~ 200 0. 994 6 0. 01 101 6. 2 152 Ethoprophos 18. 19 243. 1 /97. 1 * 243. 1 /131. 1 40 30 5 ~ 200 0. 997 8 0. 01 108 4. 3 153 Fenamidone 18. 2 312. 2 /236. 2 * 312. 2 /264. 2 16 12 5 ~ 200 0. 995 2 0. 01 96 5. 9 154 Cumyluron 18. 22 303. 0 /185. 0 * 303. 0 / 34 22 14 25 ~ 200 0. 999 0 0. 10 101 6. 4 125. 0 303. 0 /119. 0 155 Dipropetryn 18. 25 256. 2 /144. 1 * 256. 2 / 29 21 19 5 ~ 200 0. 998 2 0. 01 72 8. 5 172. 0 256. 2 /214. 1 156 Azoxystrobin 18. 27 404. 1 /372. 1 * 404. 1 /329. 1 14 32 50 ~ 200 0. 995 3 0. 10 98 7. 6 157 Profenophos 18. 27 372. 9 /128. 0 * 372. 9 / 143. 9 372. 9 /302. 8 40 36 19 5 ~ 200 0. 992 6 0. 01 92 6. 5 158 Salflufenacil 18. 27 518. 2 /348. 9 * 518. 2 /459. 0 30 16 5 ~ 200 0. 997 9 0. 01 101 6. 9 159 Tepraloxydim 18. 29 340. 0 /248. 0 * 340. 0 /220. 0 34 18 5 ~ 200 0. 994 0 0. 10 100 7. 3 160 Epoxiconazole 18. 32 330. 2 /121. 0 * 330. 2 /123. 0 21 20 5 ~ 200 0. 992 1 0. 01 101 6. 0 161 Triadimefon 18. 34 294. 2 /197. 1 * 294. 2 /225. 1 16 16 5 ~ 200 0. 995 2 0. 01 113 7. 0 162 Daimuron 18. 46 269. 0 /151. 0 * 269. 0 / 45 25 14 5 ~ 200 0. 991 6 0. 01 94 4. 2 91. 0 269. 0 /119. 0 163 Di-allate 18. 46 270. 0 /109. 0 * 270. 0 / 17 30 20 5 ~ 200 0. 992 3 0. 01 87 5. 7 86. 2 270. 0 /143. 0 164 Propazine 18. 52 230. 0 /124. 0 * 230. 0 /215. 0 17 10 5 ~ 200 0. 997 9 0. 01 86 3. 8 165 Bromuconazole 18. 61 377. 9 /158. 9 * 377. 9 / 55 28 28 5 ~ 200 0. 991 1 0. 02 93 6. 4 123. 0 377. 9 /160. 9 166 Mepanipyrim 18. 72 224. 1 /106. 0 * 224. 1 /77. 0 40 27 5 ~ 200 0. 998 2 0. 01 98 8. 2 167 Pyridaphenthion 18. 76 340. 9 /189. 1 * 340. 9 /205. 0 23 22 5 ~ 200 0. 991 9 0. 01 99 8. 3 168 Napropamide 18. 77 272. 1 /171. 1 * 272. 1 /129. 2 22 16 20 5 ~ 200 0. 996 9 0. 01 108 6. 7 169 Fenamiphos sulfone 18. 84 336. 1 /279. 9 * 336. 1 /200. 0 28 17 25 ~ 200 0. 995 6 0. 10 97 8. 0 170 Tebuconazole 18. 89 308. 2 /70. 2 * 308. 2 /125. 0 21 34 5 ~ 200 0. 993 4 0. 01 97 4. 9 171 Asulam 18. 91 231. 0 /156. 0 * 231. 0 /92. 0 25 12 5 ~ 200 0. 999 5 0. 01 98 6. 9 172 Mandipropamid 19. 05 412. 1 /327. 9 * 412. 1 /355. 9 15 11 5 ~ 200 0. 993 6 0. 01 91 6. 2 173 Bupirimate 19. 06 317. 3 /166. 1 * 317. 3 /108. 1 27 25 50 ~ 200 0. 992 9 0. 10 85 8. 2 174 Tebupirimfos 19. 06 319. 1 /210. 2 * 319. 1 /235. 2 22 20 25 ~ 200 0. 991 1 0. 10 76 7. 5 175 Tetraconazole 19. 1 372. 2 /159. 0 * 372. 2 /70. 0 24 39 50 ~ 200 0. 999 5 0. 10 97 5. 8 176 Ethalfluralin 19. 12 334. 2 /166. 2 * 334. 2 /165. 2 20 21 5 ~ 200 0. 998 3 0. 01 98 3. 5 177 Isoxaben 19. 12 333. 1 /165. 0 * 333. 1 /107. 0 61 20 5 ~ 200 0. 992 5 0. 01 106 4. 8 178 Dodemorph 19. 16 282. 2 /116. 2 * 282. 2 / 69. 3 282. 2 /98. 2 31 25 20 5 ~ 200 0. 998 6 0. 01 101 7. 6 179 Demeton S methyl 19. 2 231. 0 /61. 3 * 231. 0 /89. 2 32 10 5 ~ 200 0. 997 4 0. 01 73 7. 3 180 Isoprothiolane 19. 21 291. 0 /231. 0 * 291. 0 /189. 0 22 12 5 ~ 200 0. 991 3 0. 01 106 6. 3 181 Mepronil 19. 23 270. 2 /228. 0 * 270. 2 /119. 0 21 16 5 ~ 200 0. 994 8 0. 01 98 2. 9 182 Metolachlor 19. 26 418. 0 /140. 0 * 418. 0 / 24 17 5 ~ 200 0. 992 3 0. 01 85 8. 1 174. 9 418. 0 /189. 7 183 Phorate sulfone 19. 29 276. 1 /94. 1 * 276. 1 /174. 0 35 21 10 ~ 200 0. 999 4 0. 10 102 5. 7 184 Metobromuron 19. 31 284. 1 /252. 1 * 284. 1 /148. 2 25 20 5 ~ 200 0. 998 8 0. 01 102 5. 1 185 Bifenazate 19. 32 301. 2 /170. 0 * 301. 2 /152. 0 40 20 5 ~ 200 0. 993 4 0. 01 98 5. 8 186 Penconazole 19. 34 284. 1 /159. 0 * 284. 1 /70. 1 17 35 5 ~ 200 0. 994 8 0. 01 101 7. 5 187 Flusiazole 19. 42 316. 2 /247. 1 * 316. 2 /165. 0 34 19 5 ~ 200 0. 993 5 0. 01 70 3. 8 188 Prothioconazole 19. 43 342. 0 /306. 0 * 342. 0 /100. 0 30 16 5 ~ 200 0. 996 4 0. 01 97 6. 6 189 Nitrothal isopropyl 19. 45 313. 0 /148. 9 * 313. 0 /91. 1 41 15 5 ~ 200 0. 996 1 0. 01 103 4. 3
1-290 19 1 No. Pesticide Linear range Spiked t R Transition Recovery RSD CE /ev ρ / μg r w / mg /min m /z R /% s L - 1 kg - 1 r /% 190 Fenbuconazole 19. 48 337. 0 /125. 1 * 337. 0 /70. 4 27 35 5 ~ 200 0. 994 4 0. 01 83 5. 4 191 Metconazole 19. 65 320. 2 /70. 1 * 320. 2 /124. 9 22 41 5 ~ 200 0. 992 8 0. 01 101 6. 7 192 Isoxathion 19. 75 314. 0 /286. 0 * 314. 0 / 18 12 10 5 ~ 200 0. 998 3 0. 01 105 5. 5 105. 0 314. 0 /258. 0 193 Isozophos 19. 75 314. 0 /97. 0 * 314. 0 /123. 0 34 28 5 ~ 200 0. 990 7 0. 01 100 6. 4 194 Triazophos 19. 76 314. 0 /162. 1 * 314. 0 /119. 2 36 21 5 ~ 200 0. 997 8 0. 01 92 2. 7 195 Prochloraz 19. 79 376. 2 /308. 0 * 376. 2 /266. 0 18 14 15 ~ 200 0. 996 6 0. 10 75 5. 4 196 Propiconazole 19. 92 342. 2 /159. 0 * 342. 2 /69. 2 21 29 5 ~ 200 0. 995 7 0. 01 100 5. 5 197 Flutolanil 19. 93 324. 2 /242. 0 * 324. 2 /262. 0 26 18 5 ~ 200 0. 994 5 0. 01 103 5. 2 198 Benodanil 19. 94 324. 0 /242. 0 * 324. 0 / 19 25 18 5 ~ 200 0. 998 9 0. 01 102 5. 7 132. 0 324. 0 /262. 0 199 EPTC 19. 96 190. 1 /128. 2 * 190. 1 /86. 2 14 13 1 ~ 200 0. 997 6 0. 01 96 6. 0 200 Rotenone 19. 98 395. 3 /213. 2 * 395. 3 /192. 1 26 23 20 ~ 200 0. 990 1 0. 10 99 8. 8 201 Dimoxystrobin 20. 01 327. 1 /205. 0 * 327. 1 /116. 0 25 12 30 ~ 200 0. 999 0 0. 10 106 5. 9 202 Pinoxaden 20. 01 401. 2 /317. 0 * 401. 2 /57. 1 34 23 5 ~ 200 0. 997 4 0. 01 97 4. 7 203 Phosmet 20. 02 317. 9 /133. 1 * 317. 9 /160. 1 39 15 5 ~ 200 0. 991 5 0. 01 77 4. 4 204 Neburon 20. 11 275. 1 /57. 2 * 275. 1 /88. 0 35 30 5 ~ 200 0. 996 9 0. 01 94 5. 4 205 Ethion monoxon 20. 18 368. 9 /142. 9 * 368. 9 /199. 2 27 13 5 ~ 200 0. 993 7 0. 01 116 5. 7 206 Ditalimfos 20. 27 300. 1 /145. 3 * 300. 1 /144. 2 21 22 20 ~ 200 0. 996 4 0. 10 100 5. 4 207 Fluoxastrobin 20. 3 459. 2 /427. 1 * 459. 2 /188. 0 37 18 5 ~ 200 0. 999 2 0. 01 100 5. 0 208 Fenpropimorph 20. 35 304. 4 /147. 1 * 304. 4 /130. 1 26 31 5 ~ 200 0. 997 8 0. 01 104 6. 4 209 Spiroxamine 20. 55 298. 2 /144. 0 * 298. 2 /100. 0 35 21 5 ~ 200 0. 999 1 0. 01 105 5. 0 210 Benalaxyl 20. 76 326. 2 /148. 0 * 326. 2 /208. 0 22 15 5 ~ 200 0. 998 7 0. 01 82 6. 2 211 Diniconazole 20. 76 326. 2 /148. 2 * 326. 2 /70. 2 35 27 5 ~ 200 0. 999 6 0. 01 99 4. 2 212 Propetamphos 20. 81 282. 0 /138. 1 * 282. 0 /156. 0 18 10 5 ~ 200 0. 996 3 0. 01 103 6. 8 213 Fluquinconazole 20. 83 376. 2 /307. 0 * 376. 2 /349. 2 20 21 5 ~ 200 0. 993 4 0. 01 95 7. 0 214 Quinalphos 20. 84 299. 0 /163. 0 * 299. 0 / 38 24 23 5 ~ 200 0. 992 7 0. 01 109 6. 1 119. 1 299. 0 /147. 1 215 Tebufenozide 20. 86 353. 1 /133. 0 * 353. 1 /297. 0 19 10 5 ~ 200 0. 993 2 0. 05 93 6. 6 216 Ipconazole 21. 12 334. 1 /70. 2 * 334. 1 /125. 0 22 42 5 ~ 200 0. 994 6 0. 01 104 7. 9 217 Difenoconazole 21. 29 406. 2 /251. 0 * 406. 2 /111. 0 55 25 5 ~ 1600 0. 997 2 0. 1 81 5. 5 218 Etrimfos 21. 40 293. 1 /265. 0 * 293. 1 /278. 0 17 11 1 ~ 200 0. 995 2 0. 01 109 7. 1 219 Chlorbromuron 21. 41 292. 9 /124. 9 * 292. 9 / 33 19 20 5 ~ 200 0. 997 6 0. 01 73 6. 8 182. 0 292. 9 /203. 9 220 Cadusafos 21. 42 271. 0 /158. 9 * 271. 0 /97. 0 36 16 5 ~ 200 0. 994 5 0. 01 103 5. 4 221 Flubendiamide 21. 48 681. 0 /253. 9 * 681. 0 / 271. 9 681. 0 /273. 9 29 19 19 5 ~ 200 0. 999 0 0. 01 103 5. 9 222 Pyraclofos 21. 55 361. 1 /257. 0 * 374. 0 / 194. 0 374. 0 /222. 1 23 36 22 5 ~ 200 0. 998 3 0. 01 99 6. 0 223 Naphthol 21. 64 145. 1 /127. 1 * 272. 1 /114. 2 22 18 19 5 ~ 200 0. 997 4 0. 01 96 4. 7 224 Anilofos 21. 67 368. 0 /199. 0 * 368. 0 / 34 23 16 5 ~ 200 0. 997 5 0. 01 90 4. 3 125. 0 368. 0 /171. 0 225 Orbencarb 21. 72 258. 1 /125. 1 * 258. 1 / 89. 1 258. 1 /100. 2 43 13 28 5 ~ 200 0. 998 4 0. 01 95 6. 2 226 Methacrifos 21. 73 258. 1 /79. 2 * 258. 1 /125. 0 32 25 12 258. 1 /209. 0 5 ~ 200 0. 997 1 0. 01 118 4. 9 227 Triflumizole 21. 75 346. 2 /278. 1 * 346. 2 /73. 0 18 12 50 ~ 200 0. 990 8 0. 10 99 7. 0 228 Diazinon 21. 80 305. 0 /169. 1 * 305. 0 /153. 1 23 25 5 ~ 200 0. 993 3 0. 01 115 7. 1 229 Isocarbophos 21. 80 307. 1 /171. 1 * 307. 1 /230. 9 22 17 50 ~ 200 0. 994 1 0. 10 101 6. 5 230 Vernolate 22. 19 204. 2 /128. 2 * 204. 2 / 43. 5 204. 2 /86. 2 19 13 11 5 ~ 200 0. 999 9 0. 01 99 6. 5 231 Pirimiphos methyl 22. 42 306. 0 /164. 1 * 306. 0 /108. 2 34 24 25 ~ 200 0. 992 6 0. 10 69 6. 1 232 Thiazopyr 22. 43 397. 0 /377. 0 * 397. 0 /335. 0 26 22 5 ~ 200 0. 997 5 0. 01 97 7. 2 233 Crotoxyphos 22. 66 332. 1 /127. 0 * 332. 1 /99. 0 27 23 5 ~ 200 0. 992 8 0. 01 93 5. 7 234 Tetramethrin 22. 66 332. 1 /127. 0 * 332. 1 / 174. 0 332. 1 /226. 9 28 19 18 5 ~ 200 0. 990 4 0. 01 74 6. 1 235 Dimethylvinphos 22. 67 331. 0 /99. 1 * 331. 0 /127. 0 26 13 5 ~ 200 0. 997 3 0. 01 95 3. 8
20 32 1 No. Pesticide Linear range Spiked t R Transition Recovery RSD CE /ev ρ / μg r w / mg /min m /z R /% s L - 1 kg - 1 r /% 236 Pencycuron 22. 67 329. 0 /125. 0 * 329. 0 /218. 0 30 16 20 ~ 200 0. 995 2 0. 10 67 5. 1 237 Dimepiperate 22. 74 264. 1 /146. 1 * 264. 1 / 35 17 11 5 ~ 200 0. 999 3 0. 01 101 6. 9 91. 2 264. 1 /119. 1 238 Isofenfos 22. 88 346. 0 /216. 9 * 346. 0 /245. 0 23 12 5 ~ 200 0. 997 8 0. 01 100 8. 0 239 Teflubenzuron 22. 93 379. 2 /339. 0 * 379. 2 /196. 0 22 13 5 ~ 200 0. 993 0 0. 01 82 7. 3 240 Pretilachlor 22. 96 312. 2 /252. 0 * 312. 2 /263. 0 17 12 5 ~ 200 0. 992 2 0. 01 90 7. 0 241 Flumioxazin 23. 11 355. 1 /170. 8 * 355. 1 / 24 17 29 5 ~ 200 0. 992 8 0. 01 69 212. 8 355. 1 /142. 9 6. 0 242 Piperophos 23. 11 354. 1 /170. 9 * 354. 1 /142. 9 32 22 16 25 ~ 200 0. 995 7 0. 10 103 7. 4 354. 1 /212. 8 243 Hexaflumuron 23. 23 458. 9 /439. 0 * 458. 9 /175. 0 39 12 5 ~ 200 0. 990 7 0. 05 98 4. 9 244 Buprofezin 23. 28 306. 2 /201. 0 * 306. 2 /116. 0 18 12 5 ~ 200 0. 997 0 0. 01 116 5. 7 245 Haloxyfop methyl 23. 33 376. 0 /316. 0 * 376. 0 / 31 25 17 5 ~ 200 0. 999 7 0. 01 73 8. 3 91. 1 376. 0 /288. 0 246 Imibenconazole 23. 44 411. 0 /125. 0 * 411. 0 /171. 0 36 21 5 ~ 200 0. 994 6 0. 01 76 4. 6 247 Tebufenpyrad 23. 47 334. 2 /117. 0 * 334. 2 /145. 2 36 28 5 ~ 200 0. 993 4 0. 01 101 6. 1 248 Ethofumesate 23. 57 287. 0 /120. 9 * 287. 0 /258. 9 20 11 5 ~ 200 0. 997 5 0. 01 97 7. 6 249 Bromadiolone 23. 59 525. 1 /250. 0 * 525. 1 / 50 37 40 5 ~ 200 0. 993 2 0. 01 94 6. 6 218. 9 525. 1 /263. 3 250 Spinosyn A 23. 61 732. 5 /142. 0 * 732. 5 /98. 0 47 35 5 ~ 200 0. 999 1 0. 01 102 6. 0 251 Quinoxyfen 23. 83 307. 9 /196. 8 * 307. 9 /161. 9 47 33 5 ~ 200 0. 999 0 0. 01 104 6. 2 252 Clethodim 23. 90 360. 2 /164. 0 * 360. 2 /268. 0 20 14 5 ~ 200 0. 994 7 0. 01 88 6. 2 253 Isocarbamid 23. 93 186. 1 /145. 1 * 186. 1 /131. 1 22 24 5 ~ 200 0. 998 4 0. 01 71 5. 3 254 Tolfenpyrad 23. 93 384. 1 /196. 9 * 384. 1 /181. 7 30 29 5 ~ 200 0. 999 5 0. 01 74 3. 5 255 Trifloxystrobin 23. 93 409. 3 /186. 0 * 409. 3 /206. 1 21 16 5 ~ 200 0. 996 1 0. 01 81 7. 0 256 Novaluron 24. 03 491. 2 /471. 0 * 491. 2 /305. 0 19 15 50 ~ 200 0. 995 0 0. 10 75 5. 1 257 Piperonyl butoxide 24. 10 356. 2 /177. 0 * 356. 2 /119. 0 33 13 5 ~ 200 0. 991 5 0. 01 112 3. 5 258 Sethoxydim 24. 20 328. 0 /178. 0 * 328. 0 /128. 0 20 26 5 ~ 200 0. 999 3 0. 01 79 4. 6 259 Esprocarb 24. 41 266. 2 /91. 0 * 266. 2 /71. 1 17 24 5 ~ 200 0. 997 7 0. 01 109 6. 0 260 Alachlor 24. 49 270. 1 /162. 0 * 270. 1 /189. 0 19 16 5 ~ 200 0. 997 6 0. 01 91 5. 3 261 Furathiocarb 24. 50 383. 2 /195. 0 * 383. 2 /252. 0 20 14 5 ~ 200 0. 997 8 0. 01 103 7. 0 262 Tralkoxydim 24. 90 330. 0 /284. 0 * 330. 0 /138. 0 22 13 5 ~ 200 0. 999 2 0. 01 104 5. 2 263 Pyriproxyfen 25. 02 322. 2 /96. 0 * 322. 2 /185. 3 16 27 5 ~ 200 0. 995 6 0. 01 113 7. 2 264 Spinosyn D 25. 11 746. 5 /142. 0 * 746. 5 /98. 0 47 34 5 ~ 200 0. 991 3 0. 01 96 7. 3 265 Linuron 25. 12 249. 1 /160. 0 * 249. 1 /182. 0 17 18 5 ~ 200 0. 996 1 0. 01 102 7. 3 266 Lufenuron 25. 12 509. 2 /326. 0 * 509. 2 /175. 0 37 18 5 ~ 200 0. 996 1 0. 01 102 6. 1 267 Emamectin B1b 25. 18 872. 4 /158. 2 * 872. 4 /302. 3 33 20 5 ~ 200 0. 997 3 0. 01 94 5. 7 B1b 268 Phorate oxon sulfone 25. 18 277. 0 /97. 0 * 277. 0 /142. 9 36 22 16 5 ~ 200 0. 995 7 0. 01 72 6. 3 277. 0 /153. 0 269 Tridemorph 25. 33 298. 0 /130. 0 * 298. 0 /98. 0 32 28 5 ~ 8000 0. 998 4 0. 01 103 5. 4 270 Pirimiphos ethyl 25. 34 334. 1 /198. 1 * 334. 1 /182. 1 26 24 5 ~ 200 0. 997 1 0. 10 92 5. 5 271 Metaflumizone 25. 36 505. 2 /302. 0 * 505. 2 / 52 22 34 5 ~ 200 0. 990 9 0. 01 101 6. 4 285. 1 505. 2 /117. 1 272 Fluazinam 25. 39 463. 2 /416. 0 * 463. 2 /398. 0 17 20 5 ~ 200 0. 996 2 0. 01 104 6. 5 273 Noviflumuron 25. 46 527. 0 /193. 0 * 527. 0 /344. 0 35 15 5 ~ 200 0. 994 9 0. 01 106 9. 4 274 Fenazaquin 25. 68 307. 2 /57. 2 * 307. 2 /160. 9 23 18 5 ~ 200 0. 997 1 0. 01 94 5. 7 275 Warfarin 25. 68 307. 0 /160. 9 * 307. 0 /265. 9 20 13 1 ~ 200 0. 994 6 0. 01 104 3. 7 276 Fenpyroximate 25. 89 422. 2 /366. 0 * 422. 2 /214. 0 34 15 1 ~ 200 0. 996 7 0. 01 94 5. 7 277 Etoxazole 26. 13 360. 2 /177. 1 * 360. 2 /143. 1 22 30 51 ~ 200 0. 994 4 0. 01 92 8. 5 278 Emamectin 26. 44 886. 7 /158. 0 * 886. 7 /302. 0 33 20 5 ~ 200 0. 997 3 0. 20 92 5. 3 279 Eprinomectin B1a 26. 64 936. 5 /352. 1 * 936. 5 /490. 2 57 52 5 ~ 200 0. 997 2 0. 20 106 4. 9 B1a 280 Sulfuramid 27. 15 526. 0 /168. 9 * 526. 0 / 27 26 23 5 ~ 200 0. 996 5 0. 05 94 5. 9 219. 0 526. 0 /269. 1
1-290 21 1 No. Pesticide t R /min Transition m /z 281 Spinetoram 27. 23 760. 2 /141. 9 * 748. 3 / 98. 0 748. 3 /141. 9 282 Pyridaben 27. 42 365. 2 /147. 0 * 283 DEF 27. 43 315. 0 /169. 0 * 284 Dichlorfenthion 27. 44 315. 0 /258. 8 * Linear range Spiked Recovery RSD CE /ev ρ / μg r 2 w / mg R 珔 /% s L - 1 kg - 1 r /% 37 30 31 5 ~ 200 0. 998 7 0. 01 96 7. 6 365. 2 /309. 1 23 13 10 ~ 200 0. 990 6 20 80 3. 8 315. 0 /259. 1 17 13 5 ~ 200 0. 990 7 0. 05 94 7. 7 315. 0 /258. 8 16 13 5 ~ 200 0. 996 9 0. 01 98 6. 2 285 Hexaconazole 27. 65 314. 1 /159. 0 * 314. 1 /70. 2 20 29 5 ~ 200 0. 998 9 0. 01 105 6. 1 286 Brodifacoum 28. 16 522. 9 /335. 0 * 522. 9 /178. 2 35 23 5 ~ 200 0. 991 8 0. 01 105 4. 3 287 Phenothrin 28. 54 368. 2 /183. 0 * 368. 2 / 165. 0 368. 2 /237. 0 42 24 12 5 ~ 200 0. 990 8 0. 01 98 8. 6 288 Ivermectin B1a B1a 28. 97 892. 5 /307. 0 * 892. 5 /569. 0 28 17 5 ~ 200 0. 994 1 0. 01 95 6. 1 289 Pyridate 29. 63 379. 2 /207. 0 * 379. 2 /109. 0 19 23 5 ~ 200 0. 991 5 0. 01 96 6. 2 290 Allethrin 78. 22 303. 2 /91. 2 * 303. 2 / 33 18 13 5 ~ 200 0. 991 0 0. 05 103 6. 0 123. 1 303. 2 /135. 0 * quantitation ion **represents the analytes were detected under the negative electrospray ionization ESI - mode rest of analytes were detected under the positive electrospray ionization ESI + mode 2. 6 10 290 1 Acetamiprid Methamidophos 28 μg /kg 37 μg /kg 1 Imidacloprid Thiamethoxam 12 μg /kg 19 μg /kg 1 Acephate Dimethoate Omethoate Triazophos Phosmet Triadimefon Buprofezin Isocarbophos Quinalphos Pyridaben Imidacloprid 18 26 39 43 29 68 82 29 46 25 14 μg / kg 290 3 - HPLC - MS /MS QuEChERS 290 Thermo Fisher Scientific James Chang Jia Wang 1 General Administration of Quality Supervision Inspection and Quarantine of the People s Republic of China. Pesticide Residue Limits.. 2012-06 - 17. http / /www. tbtsps. com / FOODSAFE /XLBZ /Pages /pesticide. aspx. 2 Nuria S Bego a V Berta B Marco M. Talanta 2012 89 30 310-316. 3 Flaviane A S Anna I G C Maria E L R Q Reinaldo F T Ant nio A N Gevany P P. Food Chem. 2012 135 1 179-185. 4 Liu D Min S G. J. Chromatogr. A 2012 1235 27 166-173. 5 Chen L ShangGuan L M Wu Y Y Xu L J Fu F F. Food Control 2012 25 2 433-440. 6 Li B Zeng F G Dong Q C Cao Y Fan H T Deng C F. Phys. Procedia 2012 25 3 1776-1780. 7 Milagros M Angeles M Amadeo R. J. Chromatogr. 2012 1100 3 605-619. 8 Virginia P Elena D Bezhan C Antonio L Maria G Maria L M. J. Chromatogr. A 2012 1234 20 22-31. 9 Claudia O Wolfgang S. J. Chromatogr. A 2011 1218 37 6540-6547. 10 Emilia F Anna S. J. Chromatogr. B 2012 901 15 107-114. 11 Oscar N Héctor G Imma F Encarnación M Maria T G. J. Chromatogr. A 2012 1249 3 164-180. 12 László P Juan F G R Péter F Attila G Mihály D László A Bienvenida G Antonio M. J. Chromatogr. A 2012 1249 3 83-91.
22 32 13 Zhu W X Yang J Z Liu Y F Wei W. J. Instrum. Anal.. 2010 29 11 1109-1113. 14 Xu J Chen J Ye H Y Wang L Sun L H Lai Z F. J. Instrum. Anal.. 2011 30 9 990-995. 15 Anastassiades M Lehotay S J Stajnbaher D Schenck F J. J. AOAC Int. 2003 86 2 412-431. 16 Lehotay S J Kateřina M Alan R L. J. AOAC Int. 2005 88 2 615-629. 17 Anastassiades M. pren 15662. Determination of Pesticide Residues Using GC - MS and /or LC - MS /MS Following Acetonitrile Extraction / Ppartitioning and Ccleanup by Dispersive SPE - QuEChERS Method. European Commitee for Standardization. 18 Lehotay S J. J. AOAC Int. 2007 90 2 485-520. 19 Anastasios E Helen B Spyros A Despina T. J. Chromatogr. A 2009 1216 31 5856-5867. 20 María L G P Patricia P B Roberto R G José L M V Antonia G F. J. Chromatogr. A 2012 1248 27 130-138. 櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏櫏 CN 44-1318 /TH CODEN FCEXES BM 6013 ISSN 1004-4957 46-104 440000100186 2011 5 30% 70% CA 94% 2006 CA 38 AA 2011 9 2012 8000 500 CAJCED CJFD 16 12. 00 / 144 100 510070 020 87684776 37656606 http / /www. fxcsxb. com E - mail fxcsxb @ china. com