Determination of 135 pesticides and their metabolites in Angelica sinensis by ultra-fast liquid chromatography-tandem mass spectrometry coupled with solid-phase extraction

doi:10.3724/SP.J.1123.2015.09014

Abstract

Abstract:

A method using solid-phase extraction (SPE) followed by ultra-fast liquid chromatography-tandem mass spectrometry (UFLC-MS/MS) has been established for simultaneously quantitative determination of 135 pesticides and their metabolites (organophosphorus pesticides, pyrethroid pesticides and carbamate pesticides, etc.) in Angelica sinensis. The pesticide residues were extracted from the samples by acetonitrile, cleaned-up with a primary secondary amine (PSA) column and then analyzed using UFLC-MS/MS in multiple reaction monitoring (MRM) mode with positive electrospray ionization. The pesticide residues were quantified by matrix matched standard solution-internal standard method. All of the pesticides had good linear responses with r>0.99. The average recoveries of the pesticides at the spiked levels of 10, 50, 100 μg/kg ranged from 71.3%-119.7% with the RSDs of 1.0%-19.9%, except for clethodim (62.0%-68.2%). The limits of quantification of the 135 pesticides and their metabolites were 1.0-10.0 μg/kg. The results demonstrated that the method is simple, fast, sensitive and can be used for the analysis of the multiclass of pesticide residues in Angelica sinensis.

Key words: Angelica sinensis, multiclass of pesticide residues and metabolites, solid-phase extraction (SPE), ultra-fast liquid chromatography-tandem mass spectrometry (UFLC-MS/MS)

CLC Number:

O658

LIU Jie, TONG Ling, MENG Wenting, ZHAO Yunli, YU Zhiguo. Determination of 135 pesticides and their metabolites in Angelica sinensis by ultra-fast liquid chromatography-tandem mass spectrometry coupled with solid-phase extraction[J]. Chinese Journal of Chromatography, 2015, 33(12): 1257-1268.

References

[1] Bian J, Chen T X, Chen X R, et al. Acta Prataculturae Sinica (卞静, 陈泰祥, 陈秀蓉, 等. 草业学报), 2014, 23(6): 266
[2] Kong J, Li J G, Wang J, et al. Journal of Northwest Normal University (孔杰, 李建刚, 王剑, 等. 西北师范学院学报), 1988(3): 50
[3] Cui J J, Song X B, Ma X J, et al. Modern Chinese Medicine (崔建军, 宋学斌, 马晓嘉, 等. 中国现代中药), 2012, 14(6): 28
[4] Wang L. [MS Dissertation]. Yanji: Yanbian University (王亮. [硕士学位论文]. 延吉: 延边大学), 2007
[5] Zhuang W J. The Global Regulations on Maximum Residue Limits (MRLs) for Pesticides in Foodstuffs and Feedstuffs: Volumes Ⅰ-Ⅳ. Beijing: Chemical Industry Press (庄无忌. 国际食品饲料中农药残留限量法规: Ⅰ-Ⅳ卷. 北京: 化学工业出版社), 2010
[6] GB 2763-2014
[7] Lin W X. The Compilation of Residue Limit Standards for Pesticides and Veterinary Drugs in Foodstuffs in the World. Dalian: Dalian Maritime University Press (林维宣. 各国食品中农药兽药残留限量规定. 大连: 大连海事大学出版社), 2002
[8] Zhang Y, Zhang Q, Wang X Q. Chinese Journal of Pharmaceutical Analysis (张园, 张琦, 王贤亲. 药物分析杂志), 2012, 32(1): 95
[9] Ding M, Zhong D L, Tang F B, et al. Chinese Journal of Chromatography (丁明, 钟冬莲, 汤富彬, 等. 色谱), 2013, 31(2): 117
[10] Li N, Shao H, Liu L, et al. Chinese Journal of Pharmaceutical Analysis (李娜, 邵辉, 刘磊, 等. 药物分析杂志), 2012, 32(5): 852
[11] Cheng Z, Zhang R, Liu W H, et al. Chinese Journal of Chromatography (程志, 张蓉, 刘韦华, 等. 色谱), 2014, 32(1): 57
[12] Wang F, Li T, Ma C. Chinese Journal of Chromatography (王菲, 李彤, 马辰. 色谱), 2013, 31(3): 191
[13] Wang L Z, Zhou Y, Huang X Y, et al. Chinese Journal of Chromatography (王连珠, 周昱, 黄小燕, 等. 色谱), 2013, 31(12): 1167
[14] European Pharmacopeial Convention. European Pharmacopoeia 7.0. (2012-06-01). http://db.yaozh.com/foreign/EP7.0/20813E.PDF
[15] The United Stated Pharmacopeial Convention. United States Pharmacopeia 34. (2011-04-24). http://ishare.iask.sina.com.cn/f/14853792.html
[16] European Commission Decision 2002/657/EC
[17] Mei T, Wu R S, Wei B. China Fruit Vegetable (梅婷, 吴荣顺, 魏波. 中国果菜), 2014, 34(2): 62
[18] Wang Y J, Huang H L, Zhuo H H, et al. Journal of Inspection and Quarantine (王玉健, 黄惠玲, 卓海华, 等. 检验检疫学刊), 2009, 19(2): 74
[19] Jin C L. [MS Dissertation]. Baoding: Hebei University (金春丽. [硕士学位论文]. 保定: 河北大学), 2012
[20] Yu H J, Cai Y Q, Li Q, et al. Chinese Journal of Chromatography (于惠娟, 蔡友琼, 李庆, 等. 色谱), 2006, 24(1): 23
[21] Wang J H, Xu W Y, Sun L, et al. Chinese Journal of Pharmaceutical Analysis (王京辉, 许玮仪, 孙磊, 等. 药物分析杂志), 2012, 32(9): 1704