4 1 Vol. 4 No. 1 2013 2 Journal of Food Safety and Quality Feb., 2013 70 周 * 昱, 刘艳英, 庄丽丽, 张志刚, 郑向华, 徐敦明 (, 361026) 摘要 : 目的 70 SPE- 方法, Envi-Carb II/PSA( / -N- ), GC-MS 结果 0.01~1.0 mg/kg 60%~119%, (RSD) 1.5%~17.8% 68 0.01 mg/kg, 0.005 mg/kg 结论,, 关键词 : ; ; ; ; Determination of 70 organophosphorous pesticides in complex matrix of natural resources of plants ZHOU Yu, LIU Yan-Ying, ZHUANG Li-Li, ZHANG Zhi-Gang, ZHENG Xiang-Hua, XU Dun-Ming * (Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361026, China) ABSTRACT: Objective To establish a method for the detection of 70 organophosphorous pesticides in multi-matrix such as fresh mushroom, welsh onion, chinese chive, ginger by solid phase extraction(spe)-gas chromatography-tandem mass spectrometry. Methods The samples were extracted with acetonitrile and then purified by an Envi-Carb/PSA-solid phase extraction(spe)column. The analytes were determined by gas chromatography-mass spectrometry. Results The recoveries were 60%~119% at the spiked levels of 0.01 (0.005)~1.0 mg/kg and the relative standard deviations(rsds)were in the range of 1.5%~17.8%. The limits of quantitations (LOQs) of ethoprophos and terbufos were 0.005 mg/kg and others were 0.01 mg/kg. Conclusion The method can meet the pesticide residue limit requirements for all countries. This method has an important significance for ensuring food safety and stimulating food export. KEY WORDS: solid phase extraction (SPE); gas chromatography-tandem mass spectrometry; pesticide residue; organophosphorous; complex matrix,, 70% [1,2],, ( ), ( ) ( ),,,, 基金项目 : (3502Z20092009 3502Z20102013) (2010IK192) Fund: Supported by the Xiamen City Science and Technology Project (3502Z20092009, 3502Z20102013) and the State Quality Inspection Administration of Science and Technology Plan Project (2010IK192) * 通讯作者 :,,, E-mail: xudm@xmciq.gov.cn *Corresponding author: XU Dun-Ming, Senior Engineer, Technical Center of Xiamen Entry-Exit Inspection and Quarantine Bureau, No. 2165, Haicang Jiangang Road, Xiamen 361026, China. E-mail: xudm@xmciq.gov.cn
72 4,,, [3-6] [7-11] [12] [13] [14] [15] [16], 50,,,,,,,,,,, 1 材料与方法 1.1 试剂 ;, ; - (65 : 35, v/v); : 550 4 h,, ; : 140 4 h,, 70, 1, Dr. : 10.0 mg( 100%), 100 ml,,,, 100 mg/ml 0 ~4, : 70 4, 1,,,,, 4 : 1.2 仪器与设备 TQD - ( Thermo ); DB-5MS(30 m 0.25 mm, 0.25 µm)( Thermo ); ; T18 Basic ( IKA ); HGC-24 ( ); ENVI-Carb (0.5 g, 3 ml, Supelco ); Envi-Carb/PSA (500 mg/500 mg/6 ml, Sigma-Aldrich/ Supelco ); Anke TVL-40B ( ); PP (50 ml, ) 1.3 样品制备与保存 500 g,,,,,, 18, 1.4 样品处理 1.4.1 提取 10 g( 0.01 g), 50 ml, 10 ml, 2 min, 4 g 1 g, 2 min, 4000 r/min 5 min, 50 ml, 10 ml,, 1 ml(45 ), 1.4.2 净化 ENVI-Carb/PSA, 5 ml -, 1 ml/min, 10 ml -, 10 ml, 40 0.5 ml, 1.0 ml, GC-MS 1.5 分析条件 GC-MS : DB-5MS(30 m 0.25 mm, 0.25 µm) ; : 100 0.5 min, 15 /min 250, 20 min; :, 99.999%,
1, : 70 73, 1.0 ml/min; : 200 ; : 2 µl, ; : 250 ; : 250 ; EI, 70 ev 70 1 表 1 70 种有机磷农药的保留时间 定量离子 定性离子及离子丰度比 Table 1 Retention time, quantitative ions, qualitative ions and ions abundance ratios of 70 organophosphorous pesticides (min) (m/z) GroupI 1 dichlorvos( ) 9.63 109* 185 220 100: 19: 4 2 acephate( ) 12.64 136* 94 142 100: 45: 10 3 cadusafos( ) 15.36 159* 127 270 100: 65: 9 4 dicrotophos( ) 15.15 127* 193 237 100: 10: 7 5 disulfoton( ) 16.77 88* 89 142 100: 35: 8 6 dimethoate( ) 16.05 87* 93 125 100: 65: 50 7 parathion-methyl( ) 17.75 109* 125 263 100: 82: 30 8 chloropyriphos( ) 18.51 97* 199 314 100: 45: 20 9 pirimiphos-ethyl( ) 18.88 168* 318 333 100: 40: 35 10 fenthion ( ) 18.63 125* 109 278 100: 95: 70 11 propaphos( ) 19.83 220* 304 262 100: 70: 35 12 phoxim( ) 8.67 103* 130 77 100: 50: 42 13 ditalimfos( ) 20.19 130* 148 299 100: 40: 18 14 carbofenothion( ) 21.48 157* 342 199 100: 49: 28 15 triazophos( ) 22.08 161* 162 172 100: 55: 40 16 pyridaphenthion( ) 24.11 97* 199 340 100: 38: 25 17 phosmet( ) 24.17 160* 161-100: 18 GroupII 18 trichlorphon( ) 13.15 79* 109 145 100: 80: 25 19 ethoprophos ( ) 14.81 158* 139 200 100: 55: 40 20 phorate( ) 15.52 75* 121 260 100: 25: 5 21 omethoate ( ) 14.47 110* 156 79 100: 80: 79 22 demeton( ) 14.52/15.91 88* 89 171 100: 70: 30 23 diazinon( ) 16.52 137* 179 304 100: 95: 30 24 dyfonate( ) 16.56 109* 137 246 100: 75: 50 25 iprobenfos( ) 17.13 91* 204 288 100: 45: 7 26 isazofos( ) 16.83 161* 119 257 100: 87: 25 27 chlorpyrifos methyl( ) 17.62 125* 286 288 100: 86: 75 28 paraoxon( ) 18.04 109* 81 275 100: 63: 22 29 fenitrothion( ) 18.29 125* 109 277 100: 87: 55 30 bromophos methyl( ) 19.04 125* 329 331 100: 67: 90 31 bromophos ethyl( ) 19.85 97* 302 358 100: 98: 66 32 fosthiazate( ) 19.09 195* 97 283 100: 80: 25 33 profenofos( ) 10.66 156* 97 208 100: 95: 15 34 ethion( ) 21.62 231* 97 153 100: 99: 92 35 edifenphos( ) 22.57 109* 172 309 100: 85: 75 36 pyraclofos( ) 27.92 138* 194 360 100: 80: 55 37 coumaphos( ) 28.73 109* 226 362 100: 60: 45
74 4 ( 续表 1) (min) (m/z) GroupIII 38 methamidophos( ) 9.95 94* 95 141 100: 68: 58 39 sulfotep( ) 15.19 97* 202 322 100: 90: 80 40 terbufos( ) 16.40 57* 231-100: 40 41 monocrotophos( ) 15.61 127* 67 192 100: 23: 13 42 dichlofenthion( ) 17.42 223* 279 97 100: 88: 87 43 fenchlorphos( ) 17.93 285* 125 287 100: 60: 50 44 pirimiphos-methyl( ) 18.08 276* 305 290 100: 64: 53 45 parathion( ) 18.72 97* 109 291 100: 80: 30 46 dimethylvinphos( ) 18.57 109* 295 297 100: 55: 35 47 isophenphos( ) 19.34 58* 121 213 100: 35: 35 48 phenthoate( ) 19.47 121* 125 274 100: 92: 70 49 methidathion( ) 19.86 145* 85-100: 98 50 phosfolan methyl( ) 19.55 196* 140 106 100: 85: 69 51 famphur( ) 22.28 218* 125 93 100: 45: 39 52 phosalone( ) 26.17 182* 121 367 100: 54: 12 53 azinphos methyl( ) 26.72 77* 132 160 100: 82: 78 GroupIV 54 dibrom( ) 15.07 109* 145 301 100: 55: 10 55 phosdrin( ) 12.20 127* 109 192 100: 30: 30 56 thiometon( ) 15.78 88* 125 93 100: 35: 20 57 propetamphos( ) 16.85 138* 194 236 100: 45: 25 58 etrimfos( ) 16.88 181* 153 292 100: 92: 63 59 phosphamidon( ) 16.55/17.35 127* 72 264 100: 55: 25 60 trichloronate( ) 18.88 109* 268 296 100: 75: 55 61 malathion( ) 18.34 125* 173 93 100: 98: 81 62 isofenphos-methyl( ) 19.07 58* 199 121 100: 45: 35 63 isocarbophos ( ) 18.86 136* 121 230 100: 75: 15 64 quinalphos( ) 19.56 146* 157 298 100: 87: 13 65 tetrachlorvinphose( ) 19.92 109* 329 331 100: 35: 30 66 iodofenphos( ) 20.37 376* 125 378 100: 55: 35 67 phosfolan( ) 19.54 92* 140 196 100: 75: 45 68 triamiphos( ) 21.72 160* 135 294 100: 35: 15 69 EPN( ) 24.57 157* 169 185 100: 50: 30 70 azinphos ethyl ( ) 27.56 132* 160 77 100: 78: 50 : *
1, : 70 75 1.6 定量测定 1.5 -, (±0.5%),,,,, ( 1) 1.7 添加回收实验 10.0 g, 0.01~1.0 mg/kg, 5 1.4~1.6,, 2 结果与分析 2.1 样品前处理方法的选择, : (1:1, v/v ) [6] [5] - (4:3, v/v) [11] [17], - - :,, 70,,, FPD,,,,, [18] -,,,,,,,,,,, ENVI-Carb ENVI- Carb/ PSA,, ENVI-Carb/PSA,,, ENVI- Carb/PSA 2.2 仪器方法的建立 DB-5MS(30 m 0.25 mm 0.1 μm),, / (GC-MSD/SIM), (GC-MSD/SCAN) (TIC), GC-MSD-SIM,, 1 2-1, 2.3 方法检测限,, 3 (LOD), 10 (LOQ), 68 LOQ 0.01 mg/kg, LOQ 0.005 mg/kg 2.4 回收率与精密度 70, 0.01(0.005)~1.0 mg/kg, 5, 3 60%~119%; 1.5%~17.8% SN/T 0001-1995 [19], 1 µg/kg, 50%~120%; 1~10 µg/kg, 70%~110%; 10 µg/kg, 80%~110%,, SN/T 0001-1995 [19], 1 µg/kg, <45%; 1~10 µg/kg, 32%, 10~100 µg/kg, <23%, 1000 µg/kg, <16%,, 2.5 实际样品分析,
76 4, (, ),, 0.01 mg/kg, 0.23 mg/kg 表 2 检测离子的开始时间和驻留时间 Table 2 The start time and scan time of ions /min (m/z) /s GroupI 1 7.00 77 103 130 0.36 2 9.00 109 185 220 0.36 3 10.00 94 136 142 0.36 4 13.00 127 159 193 237 270 0.59 5 15.80 87 88 89 93 237 270 0.70 6 17.00 109 125 263 0.36 7 18.00 97 109 125 168 199 278 314 318 333 1.05 8 19.30 130 148 220 262 299 304 0.70 9 21.00 77 157 199 161 162 172 342 0.82 10 23.00 97 160 161 199 340 0.59 GroupII 1 9.00 79 97 109 145 156 208 0.70 2 13.50 79 88 89 109 110 139 156 158 170 200 1.16 3 15.10 75 88 89 121 170 260 0.70 4 16.20 109 119 137 152 161 179 246 257 304 1.05 5 16.95 91 125 204 286 288 0.59 6 17.85 81 109 125 275 277 0.59 7 18.60 97 125 195 283 302 329 331 358 0.93 8 20.00 109 172 309 0.36 9 21.00 97 153 231 0.36 10 22.00 109 138 194 226 360 362 0.70 GroupIII 1 8.00 94 95 141 0.24 2 11.00 67 97 127 192 202 322 0.70 3 16.00 57 231 0.24 4 17.00 97 125 223 276 279 285 287 290 305 1.05 5 18.30 97 109 291 295 297 0.59 6 19.00 58 85 106 121 125 140 145 196 213 274 1.16 7 21.00 93 125 128 0.36 8 23.00 77 121 132 160 182 367 0.70 GroupIV 1 11.00 109 127 192 0.36 2 13.00 88 93 109 125 145 301 0.70 3 16.00 72 127 138 153 181 194 236 264 292 1.05
1, : 70 77 ( )
78 4 Fig. 1 1 SIM SIM chromatotrams of 70 organophosphorous pesticides Table 3 表 3 鲜香菇 大葱 生姜 韭菜 70 种农药不同添加水平回收率数据 (n=5) Recoveries and RSDsof oganophosphorous pesticides in fresh mushroom, green Chinese onion, ginger and leek(n=5) (mg/kg) Recovery/% RSD/% Recovery/% RSD/% Recovery/% RSD/% Recovery/% RSD/% 1 0.01 0.1 60 81 3.4 12.6 72 82 5.4 12.5 62 75 4.2 11.7 98 108 4.5 11.3 2 0.01 0.1 67 78 6.0 13.6 68 83 6.6 14.4 65 77 5.1 12.3 62 77 5.3 12.4 3 0.01 0.1 60 86 3.2 11.6 70 76 3.7 10.6 66 88 4.2 9.6 82 97 3.8 11.1 4 0.01 0.1 65 87 4.5 12.1 70 86 5.5 12.7 64 89 4.8 11.7 84 90 5.0 11.7 5 0.01 0.1 75 92 5.9 13.3 78 83 5.2 13.6 65 97 4.9 12.1 77 92 4.9 12.0 6 0.01 0.1 60 89 5.7 12.9 80 85 5.9 14.9 63 96 5.4 13.1 75 86 5.4 12.2 7 0.01 0.1 62 81 4.7 11.8 75 79 5.7 12.4 69 86 6.1 12.8 74 85 4.5 10.9 8 0.01 0.1 63 82 6.3 13.8 88 99 5.3 12.7 69 92 6.5 13.2 71 84 5.8 12.5 9 0.01 0.1 60 95 6.5 13.5 67 87 6.1 13.1 67 104 7.0 14.0 72 83 5.2 11.7 10 0.01 0.1 65 84 5.1 12.2 76 88 5.4 12.8 66 119 6.1 13.3 71 82 5.9 12.1 11 0.01 0.1 70 82 7.5 14.2 75 85 6.5 13.2 73 112 7.5 14.7 75 87 6.5 13.1 12 0.01 0.1 64 96 5.3 11.6 76 87 6.9 12.7 62 81 6.4 12.5 74 85 6.2 12.4 13 0.01 0.1 64 95 6.3 12.4 80 97 7.3 12.9 63 99 7.3 14.4 75 88 6.1 11.3 14 0.01 0.1 67 94 6.3 12.5 84 89 5.3 12.8 60 76 7.0 13.5 77 89 5.3 11.0 15 0.01 0.1 69 94 6.6 13.1 76 90 6.4 12.1 77 94 7.6 14.4 76 90 5.9 12.9 16 0.01 0.1 68 96 6.5 13.6 90 110 5.5 12.6 63 102 5.5 12.8 83 95 5.1 12.5 17 0.01 0.1 70 85 4.8 10.8 67 89 4.1 10.2 74 97 5.7 12.9 73 81 5.5 11.8 18 0.01 0.1 80 96 8.8 15.5 77 90 8.3 16.5 88 104 7.8 15.8 80 87 6.8 13.1 19 0.005 0.1 60 84 7.1 14.3 78 97 6.1 12.4 84 118 6.1 13.1 85 91 6.1 13.3 20 0.01 0.1 65 87 6.3 12.7 69 98 7.3 13.9 81 94 5.8 11.8 85 93 6.8 13.7 21 0.01 0.1 75 82 5.9 12.2 66 89 6.8 13.2 88 101 6.6 13.3 83 90 6.6 13.9 22 0.01 0.1 65 76 6.6 13.7 69 89 6.4 13.0 82 89 7.2 14.4 88 93 6.7 13.0 23 0.01 0.1 65 86 6.0 13.3 78 89 6.2 13.5 76 109 7.0 14.2 65 78 7.0 14.3 24 0.01 0.1 60 74 7.1 14.4 79 87 8.1 14.9 81 103 7.5 13.7 66 82 7.7 14.8
1, : 70 79 ( 续表 3) (mg/kg) Recovery/% RSD/% Recovery/% RSD/% Recovery/% RSD/% Recovery/% RSD/% 25 0.01 0.1 83 90 7.9 14.5 70 75 6.9 13.5 77 98 6.9 13.5 70 85 7.4 14.4 26 0.01 0.1 60 76 8.3 15.6 75 87 7.3 14.5 70 89 7.2 14.4 68 81 8.1 15.5 27 0.01 0.1 62 74 11.0 17.8 69 80 2.1 16.8 71 91 10.0 16.8 69 85 9.9 16.1 28 0.01 0.1 87 98 10.7 17.0 65 90 9.6 16.0 70 93 11.1 17.4 71 89 7.7 15.5 29 0.01 0.1 78 90 9.1 16.8 74 89 8.5 17.2 79 95 8.8 15.7 66 81 8.1 15.8 30 0.01 0.1 74 93 6.0 13.5 67 91 7.1 15.5 71 93 7.5 14.6 67 82 7.2 14.1 31 0.01 0.1 78 97 7.6 14.9 61 76 7.3 14.2 73 94 6.4 13.4 70 85 7.3 13.9 32 0.01 0.1 94 106 5.7 12.5 80 90 6.2 12.1 63 86 6.8 13.7 71 90 6.7 13.3 33 0.01 0.1 93 102 2.8 15.8 67 79 8.4 16.8 79 96 7.4 15.2 70 83 7.8 14.9 34 0.01 0.1 97 108 5.2 12.3 67 90 6.3 13.1 60 73 6.2 13.4 68 79 6.2 13.2 35 0.01 0.1 95 108 6.0 13.4 78 90 5.9 12.5 61 75 7.1 14.5 69 85 7.3 14.4 36 0.01 0.1 90 93 5.8 12.6 90 98 6.3 13.4 66 77 6.7 13.1 73 97 6.8 13.1 37 0.01 0.1 65 90 6.5 13.7 67 89 6.5 13.7 67 81 7.3 14.2 75 101 7.6 14.1 38 0.01 0.1 73 82 7.1 15.6 67 90 7.8 16.6 63 78 6.1 12.6 72 93 7.4 14.3 39 0.01 0.1 63 80 8.3 17.6 77 80 9.0 17.2 68 79 7.3 15.6 80 92 8.3 15.6 40 0.005 0.1 60 81 5.8 12.8 85 90 6.2 13.7 74 91 9.7 16.5 66 78 7.6 13.8 41 0.01 0.1 109 119 6.2 14.7 67 92 7.1 15.1 67 79 8.2 15.7 85 97 7.2 14.5 42 0.01 0.1 70 74 5.6 12.8 68 89 6.2 13.7 65 80 6.5 13.8 71 88 6.5 13.3 43 0.01 0.1 72 76 5.9 13.1 65 78 6.1 13.0 82 93 6.7 14.0 73 89 6.9 13.7 44 0.01 0.1 70 79 7.4 16.8 78 90 8.4 17.8 72 81 7.1 15.5 75 98 7.2 15.5 45 0.01 0.1 80 89 7.1 16.2 65 78 7.6 15.2 76 83 7.3 15.4 78 101 7.0 14.3 46 0.01 0.1 87 112 8.6 17.7 80 98 6.8 15.7 70 81 8.1 16.8 82 95 7.6 14.7 47 0.01 0.1 86 95 8.1 17.8 77 87 6.0 14.8 75 90 8.8 17.4 75 93 7.8 15.8 48 0.01 0.1 71 83 5.8 12.9 67 90 5.1 12.3 72 96 7.8 16.1 85 110 6.9 12.3 49 0.01 0.1 84 99 7.8 16.6 89 97 7.5 15.7 71 99 7.2 15.7 82 112 7.7 15.0 50 0.01 0.1 90 102 5.6 13.2 70 90 6.3 14.2 78 91 6.7 14.1 82 101 6.4 12.2 51 0.01 0.1 96 100 6.0 13.5 66 88 6.5 13.2 75 105 6.4 13.7 83 98 6.7 13.7 52 0.01 0.1 101 111 5.9 13.5 69 97 5.5 13.2 79 90 6.9 13.4 79 95 5.9 12.5 53 0.01 0.1 96 107 6.4 13.8 87 98 7.4 16.8 69 85 7.2 14.2 78 98 6.6 12.8 54 0.01 0.1 87 97 7.1 17.5 78 94 7.0 16.2 70 89 7.7 15.1 75 93 6.9 13.5 55 0.01 0.1 81 86 8.0 17.6 78 89 8.4 17.1 71 91 8.3 16.9 82 98 1.5 15.6 56 0.01 0.1 70 85 9.0 17.4 68 88 8.5 17.5 70 93 8.2 16.4 63 77 8.2 16.4 57 0.01 0.1 91 98 8.5 16.4 64 88 8.3 17.1 79 95 8.8 16.7 80 91 7.5 15.4 58 0.01 0.1 73 85 7.3 17.6 65 78 7.7 16.7 71 93 7.7 15.5 88 93 8.3 16.1 59 0.01 0.1 98 112 6.8 16.5 63 70 7.8 16.9 73 94 7.8 16.1 73 90 7.8 15.1 60 0.01 0.1 83 96 5.4 14.2 79 100 6.4 14.5 63 86 6.4 13.2 88 101 6.7 13.7 61 0.01 0.1 93 103 6.2 14.5 69 89 7.2 15.4 79 96 6.6 13.7 80 99 6.8 14.0 62 0.01 0.1 97 110 8.7 17.1 79 97 7.9 16.2 60 73 7.7 15.1 79 102 7.5 15.1 63 0.01 0.1 103 113 5.9 13.8 69 90 6.8 12.8 61 75 6.9 14.0 80 98 6.9 13.7 64 0.01 0.1 91 99 6.0 15.2 75 87 7.0 15.8 68 88 6.2 13.3 86 103 6.1 13.4 65 0.01 0.1 106 111 5.6 12.1 70 89 6.6 13.2 64 88 5.9 12.4 92 115 5.5 12.0 66 0.01 0.1 103 113 7.1 17.1 67 89 7.3 15.2 65 78 6.1 16.6 84 103 6.1 13.1 67 0.01 0.1 91 98 3.8 17.9 90 98 7.9 16.9 63 70 7.8 16.9 83 98 7.8 14.9 68 0.01 0.1 106 122 8.2 17.5 80 85 8.5 16.5 79 100 8.2 16.1 81 95 7.2 14.7 69 0.01 0.1 96 107 7.6 16.4 67 79 7.2 15.3 69 89 6.6 15.3 90 104 3.0 16.2 70 0.01 0.1 107 114 6.1 14.2 69 80 6.9 13.7 79 97 7.0 14.5 95 112 6.8 14.4
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