Multiresidue Determination of Organophosphorus Pesticides in Fruits and Vegetables by Gas Chromatography-Negative Chemical Ionization-Mass Spectrometry

Abstract

Abstract: A gas chromatography-negative chemical ionization-mass spectrometry (GC-NCI-MS) method was established to simultaneously determine 9 organophosphorus pesticide residues in fruits and vegetables. Samples were extracted with ethyl acetate and cleaned up on a Florisil column before GC-NCI-MS analysis in a selective ion-monitoring (SIM) mode. The internal standard used was ethion. The presented method was rapid, simple, sensitive and selective. The detection limits of this method for 9 organophosphorus pesticides were in the range of 0.12－1.21 μg/kg. The average recovery rates of 9 organophosphorus pesticides varied from 76.5% to 112% with a relative standard deviation of 1.45%－11.0%.

Key words: gas chromatography-negative chemical ionization-mass spectrometry (GC-NCI-MS), organophosphorus pesticides, pesticide residues, fruits, vegetables

CLC Number:

TS207.3

References

参考文献：
[1] 葛晓光,张智敏. 绿色蔬菜生产[M]. 北京:中国农业出版社,1997.
[2] 汪雅谷,张四荣. 无污染蔬菜生产的理论与实践[M]. 北京:中国农业出社,2001.
[3] Silvia Lacorte and Míriam Guillamo. Validation of a pressurized solvent extraction and GC–NCI–MS method for the low level determination of 40 polybrominated diphenyl ethers in mothers’ milk[J].Chemosphere, 2008, 73(1): 70-75.
[4] 马玉，林竹光. 气相色谱-负离子化学源/质谱法（GC-NCI/MS）分析鱼类和贝类样品中多溴联苯醚和多溴联苯[J]. 分析试验室，2011, 30(4):99-103.
[5] Jianzhong Shen, Xi Xia, Haiyang Jiang and Cun Li, et al. Determination of chloramphenicol, thiamphenicol, florfenicol, and florfenicol amine in poultry and porcine muscle and liver by gas chromatography-negative chemical ionization mass spectrometry[J]. Journal of Chromatography B, 2009, 877(14-15):1523-1529.
[6] 沈伟健，徐锦忠，赵增运等. 气相色谱负化学源质谱法测定蔬菜中11种醚类除草剂残留[J]. 分析化学 ( FENX I HUAXUE)研究报告，2008, 36(5):663-667.
[7] Laura B. Rivera-Rodríguez and Ricardo Rodríguez-Estrella, et, al. Quantification of low levels of organochlorine pesticides using small volumes (≤100 μl) of plasma of wild birds through gas chromatography negative chemical ionization mass spectrometry [J]. Environmental Pollution, 2007, 148(2): 654-662.
[8] 王英，元学奎，马召辉等. 气相色谱/负化学电离源质谱法测定底泥中的有机氯农药[J]. 化学通报，2011, 74(3):264-269.
[9] 胡贝贞，沈国军和邵铁峰等. 加速溶剂萃取-气相色谱-负化学离子源质谱法测定茶叶中有机氯和拟除虫菊酯类农药残留量[J]. 分析试验室，2009, 28(1):80-83.
[10] M.L.Feo, E.Eljarrat, D.Barceló. A rapid and sensitive analytical method for the determination of 14 pyrethroids in water samples [J]. Journal of Chromatography A, 2010, 1217(15): 2248-2253.
[11] Mario Vincenzo Russo, Luigi Campanella, Pasquale Avino. Determination of organophosphorus pesticide residues in human tissues by capillary gas chromatography-negative chemical ionization mass spectrometry analysis[J]. Journal of Chromatography B, 2002, 780(2):431-441.
[12] Luca Amendola, Francesco Botrè, et, al. Analysis of organophosphorus pesticides by gas chromatography–mass spectrometry with negative chemical ionization: a study on the ionization conditions[J]. Analytica Chimica Acta, 2002, 461(1):97-108.
[13] 郑向华，方恩华和吴敏等. 气相色谱-负化学离子源质谱联用法测定植物性产品中多组分农药残留量[J]. 分析试验室，2009, 28(9):99-102.
[14] Liliane Martins, Michel Yegles, et, al. Simultaneous enantioselective determination of amphetamine and congeners in hair specimens by negative chemical ionization gas chromatography–mass spectrometry[J]. Journal of Chromatography B, 2005, 825(1):57-62.
[15] Budzikiewicz H. Negative chemical ionization (NCI) of organic compounds [J]. Mass Spectrometry Reviews, 1986, 5 (6): 345-380.