气相色谱-串联质谱法测定鱼肉中毒死蜱及其代谢产物3,5,6,-三氯-2-羟基吡啶的残留量
GC-MS/MS Determination of Residual Amounts of Residual Amounts of Chlorpyrifos and Its Metabolite-3,5,6-Trichloro-2-Pyridinol in Fish
摘 要
采用气相色谱-串联质谱法(GC-MS/MS)测定鱼肉中毒死蜱及其代谢产物3,5,6,-三氯-2-羟基吡啶(TCP)残留量。样品经1 mol·L-1盐酸-乙腈(1+99)混合液提取,提取液于-20 ℃冷冻去除脂肪,浓缩近干,残渣用乙酸乙酯溶解后与N-甲基-N-叔丁基二甲基硅基三氟乙酰胺进行衍生反应,产物经净化后采用GC-MS/MS测定。毒死蜱和TCP的线性范围分别为2.0~2 000,1.0~1 000 μg·L。鱼肉中毒死蜱和TCP的检出限(3S/N)分别为0.5,0.3 μg·kg-1,测定下限(10S/N)分别为1.7,1.0 μg·kg-1。加标回收率分别为84.6%~95.6%,73.8%~82.7%,测定值的相对标准偏差(n=6)分别小于10%,13%。
毒死蜱
3,5,6,-三氯-2-羟基吡啶
鱼肉
GC-MS/MS
Chlorpyrifos
3,5,6-Trichloro-2-pyridinol
Fish
Abstract
GC-MS/MS was applied to the simultaneous determination of residual amounts of chlorpyrifos (CP) and its metabolite 3,5,6-trichloro-2-pyridinol (TCP) in fish. The sample was extracted with a mixture of 1 mol·L-1 HCl solution and acetone (1+99). The extract was defatted by frozen at -20 ℃. After removing the fat separated, the extract was evaporated and the residue was dissolved with ethyl acetate and derivatized by reacting with N-(tert-Butyldimethylsilyl)-N-Methyltrifluoroacetamide. The derivative was purified and then analyzed by GC-MS/MS. The linearity ranges of CP and TCP were between 2.0-2 000, 1.0-1 000 μg·L-1, with the detection limits (3S/N) of 0.5, 0.3 μg·kg-1, and lower limits of determination (10S/N) of 1.7, 1.0 μg·kg-1, respectively. Values of recovery found by standard addition method were 84.6%-95.6%, 73.8%-82.7%, respectively, and RSD′s (n=6) were less than 10%, 13%, respectively.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201509009
所属栏目 工作简报
基金项目 西南民族大学中央高校基本科研业务费青年教师基 金项目(11NZYQN06)
收稿日期 2014/9/3
修改稿日期
网络出版日期
作者单位点击查看
联系人作者贺亮(microvet@163.com)
备注郝力力(1980-)男,山西长治人,博士,主要从事寄 生虫学及药物残留分析。
引用该论文: HAO Li-li,LI Rui,HE Liang. GC-MS/MS Determination of Residual Amounts of Residual Amounts of Chlorpyrifos and Its Metabolite-3,5,6-Trichloro-2-Pyridinol in Fish[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(9): 1247～1251
郝力力,李锐,贺亮. 气相色谱-串联质谱法测定鱼肉中毒死蜱及其代谢产物3,5,6,-三氯-2-羟基吡啶的残留量[J]. 理化检验－化学分册, 2015, 51(9): 1247～1251
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参考文献
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【2】张文童,李锐,章虎,等.毒死蜱在大田作物-饲料-畜禽产品食物链中残留行为及其风险评估［J］.浙江农业科学, 2012,1(6):885-890.
【3】SOGORB M A, VILANOV E, CARRER V . Future applications of phosphotriesterases in the prophylaxis and treatment of organophosporus insecticide and nerve agent poisonings［J］. Toxicology Letter, 2004,151(1):219-233.
【4】TIMCHALK C, BUSBY A, CAMPBELL J, et al. Comparative pharmacokinetics of the organophosphorus insecticide chlorpyrifos and its major metabolites diethylphosphate, diethylthiophosphate and 3,5,6-trichloro-2-pyridinol in the rat［J］. Toxicology, 2007,237:145-157.
【5】CACERES T, HE Wen-xiang, NAIDU R, et al. Toxicity of chlorpyrifos and TCP alone and in combination to daphnia carinata: the influence of microbial degradation in natural water［J］. Water Research, 2007,41:4497-4503.
【6】BICKER W, LAMMERHOFERA M, GENSER D, et al. A case study of acute chlorpyrifos poisoning; novel aspects on metabolism and toxicokinetics derived from liquid chromatography tandem mass spectrometry analysis of urine samples［J］. Toxicology Letters, 2005,159(3):235-251.
【7】SCHARBERG D M, RICHARDSON D L. Multiresidue screen for organophosphorus insecticides using gel permeation chromatography-silica gel cleanup［J］. Journal of the Association of Official Analytical Chemists, 1991,74:394-399.
【8】FRENICH A G, BOLANOS P P, VIDAL J L. Multiresidue analysis of pesticides in animal liver bygas chromatography using triple quadrupole tandem mass spectrometry［J］. Chromatography A, 2007,1153(1/2):194-202.
【9】MOL H G, PLAZ-BOLANOS P, ZOMER P, et al. Toward a generic extraction method for simultaneous determination of pesticides, mycotoxins, plant toxins, and veterinary drugs in feed and food matrixes［J］. Analytical Chemistry, 2008,80(24):9450-9459.
【10】INMAN R D, KIIGEMAGI U, DEINZER M L. Determination of chlorpyrifos and 3,5,6-trichloro-2-pyridinol residues in peppermint hay and peppermint oil［J］. Agricutural Food Chemistry ,1981,29(2):321-323.
【11】张文童,李锐,章虎,等.气相色谱-串联质谱法测定稻米中毒死蜱及其代谢产物［J］.理化检验-化学分册, 2012,48(6):667-670.
【12】LIANG Bin, YANG Cheng-li, GONG Ming-bo, et al. Adsorption and degradation of triazophos, chlorpyrifos and their main hydrolytic metabolites in paddy soil from Chaohu Lake, China［J］. Environment Manage, 2011,92(9):2229-2234.
【13】DISHBURGER H J, MCKELLAR R L, PENNINGTON J Y, et al. Determination of residues of chlorpyrifos, its oxygen analogue, and 3,5,6-trichloro-2-pyridinol in tissues of cattle fed chlorpyrifos［J］. Agricural Food Chemistry, 1977,25(6):1325-1329.
【14】BARTLETT M G. Determination of chlorpyrifos and its metabolites in rat brain tissue using coupled-column liquid chromatography/electrospray ionization tandem mass spectrometry［J］. Rapid Communications in Mass Spectrometry, 2006,20(18):2689-2695.
【15】SCHENCK F J, HOBBS J E. Evaluation of the quick, easy, cheap, effective, rugged, and safe (QuEChERS) approach to pesticide residue analysis［J］. Bulletin of Environmental Contamination and Toxicology, 2004,73(1):24-30.
【16】JUHLER R K. Optimized method for the determination of organophosphorus pesticides in meat and fatty matrices［J］. Chromatograph A, 1997,786(1):145-153.
【17】KUHLER R K. Optimized method for the determination of organophosphorus pesticides in meat and fatty matrices［J］. Chromatograph A, 1997,786(1):145-153.
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