Citation: MA Lin, CHEN Jianbo, ZHAO Li, ZHAN Xiuping. Determination of six amide pesticide residues in vegetables and fruits by solid phase extraction-ultra high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2015, 33(10): 1019-1025. doi: 10.3724/SP.J.1123.2015.05013 shu

Determination of six amide pesticide residues in vegetables and fruits by solid phase extraction-ultra high performance liquid chromatography-tandem mass spectrometry

1.
Shanghai Agriculture Technology Extension & Service Centre, Pesticide Quality Supervision and Inspection Testing Centre (Shanghai), Ministry of Agriculture, Shanghai 201103, China

Corresponding author: ZHAO Li,
Received Date: 21 May 2015

Fund Project: 上海市农委科技攻关项目(沪农科攻字(2015)第4-6号). (沪农科攻字(2015)第4-6号)

A solid phase extraction coupled with ultra high performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS) method was developed for simultaneous determination of six amide pesticides, cyantraniliprole, mandipropamid, boscalid, fluopicolide, thifluzamide and flubendiamide, in vegetables and fruits. After extraction with acetonitrile, purification with Florisil SPE cartridges and dissolution with methanol, the targets in the sample solutions were analyzed by UPLC-MS/MS on an Agilent Proshell 120 EC-C18 column with a mixture of 0.1% formic acid solution and methanol as the mobile phases under gradient elution conditions. The mass spectrometer operated in multiple reaction monitoring (MRM) mode with the negative and positive modes. Good linearity was obtained for the six amide pesticides at the mass concentrations of 0.0005-1.00mg/L with the correlation coefficients more than 0.999. The fortified recoveries were in the range of 72.4%-119.4% with the concentration levels at 0.01, 0.1 and 1.0 mg/kg for cyantraniliprole, mandipropamid, boscalid, fluopicolide, thifluzamide, and 0.001, 0.01 and 0.1 mg/kg for flubendiamide. The relative standard deviations (RSDs) were less than 15% and the limits of quantification were 0.01 mg/kg for cyantraniliprole, mandipropamid, boscalid, fluopicolide, thifluzamide, and 0.001 mg/kg for flubendiamide. All the above observations indicate that the established analytical method is simple, efficient and sensitive, and suitable for the determination of the six amide pesticides in vegetables and fruits.
- ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS),
- solid phase extraction (SPE),
- amide pesticides,
- residues,
- vegetables,
- fruits
1. [1]
  [1] Yang G Q, Huang Q, Chen L, et al. World Pesticides (杨桂秋, 黄琦, 陈霖, 等. 世界农药), 2012, 34(6): 19
2. [2]
  [2] Kato K, Kiyonaka S, Sawaguchi Y, et al. Biochemistry, 2009, 48(43): 10342
3. [3]
  [3] Singh G, Sahoo S K, Takkar R, et al. Chemosphere, 2011, 84(10): 1416
4. [4]
  [4] Liu C Y, Hao Y J, Wang J, et al. China Vegetables (刘春艳, 郝永娟, 王勇, 等. 中国蔬菜), 2008(1): 26
5. [5]
  [5] Chi H W, Diao J, Nie K S, et al. Agrochemicals (迟会伟, 刁杰, 聂开晟, 等. 农药), 2007, 46(1): 52
6. [6]
  [6] Cui G W, Lu H T, Yu L X, et al. World Pesticides (崔国葳, 鲁洪涛, 于乐祥, 等. 世界农药), 2010, 32(2): 25
7. [7]
  [7] Yan F Y, Liu D Q, Sima L F, et al. Agrochemicals (颜范勇, 刘冬青, 司马利锋, 等. 农药), 2008, 47(2): 132
8. [8]
  [8] Zhu W G, Hu W Q, Chen J. China Rice (朱卫刚, 胡伟群, 陈杰. 中国稻米), 2011, 17(2): 54
9. [9]
  [9] Codex Alimentarius Commission. Pesticide Residues in Food-FAO/WHO Food Standards. (2015-07-08)[2015-07-19]. http://www.codexalimentarius.net/pestres/data/index.html?language=EN&version=ext&hasbulk=0
10. [10]
  [10] European Union. Commission Regulation. (2015-07-07) [2015-07-19]. http://ec.europa.eu/food/plant/pesticides/eu-pesticides-database/public/?event=pesticide.residue.selection&language=EN
11. [11]
  [11] The Japan Food Chemical Research Foundation. Maximum Residue Limits (MRLs) List of Agricultural Chemicals in Foods. (2015-05-13) [2015-07-19]. http://www.m5.ws001.squarestart.ne.jp/foundation/search.html
12. [12]
  [12] Fan X Q, Zhan X P, Ma L. Modern Agrochemicals (樊晓青, 占绣萍, 马琳. 现代农药), 2014, 13(1): 41
13. [13]
  [13] Wei L N, Zhang J J, Wang F R, et al. Chinese Journal of Pesticide Science (韦利娜, 张静静, 汪芙蓉, 等. 农药学学报), 2013, 15(3): 311
14. [14]
  [14] Wang D D, Chen Y, Song N H, et al. Journal of Instrumental Analysis (王点点, 陈源, 宋宁慧, 等. 分析测试学报), 2013, 32(1): 138
15. [15]
  [15] Zhang Y T, Guo Y Z, Liu L, et al. Agrochemicals (张玉婷, 郭永泽, 刘磊, 等. 农药), 2011, 50(7): 518
16. [16]
  [16] Watanabe E, Kobara Y, Baba K, et al. Food Chem, 2014, 154: 7
17. [17]
  [17] Duan T T, Zhang Y, Wei J, et al. Journal of Instrumental Analysis (段婷婷, 张盈, 魏进, 等. 分析测试学报), 2014, 33(5): 598
18. [18]
  [18] Chen X L, Li Z X, Cao Z Y, et al. Chinese Journal of Chromatography (陈小龙, 李正翔, 曹赵云, 等. 色谱), 2013, 31(10): 954
19. [19]
  [19] Rajski Ł, Lozano A, Uclés A, et al. J Chromatogr A, 2013, 1304(7): 109
20. [20]
  [20] Qian C, Wu Q, Lü D Z, et al. Chinese Journal of Pesticide Science (钱程, 吴琼, 吕岱竹, 等. 农药学学报), 2014, 16(5): 594
21. [21]
  [21] Wang C B, Huang X G, Fan X Q, et al. Acta Agriculturae Shanghai (汪传炳, 黄秀根, 樊晓青, 等. 上海农业学报), 2013, 29(4): 36
22. [22]
  [22] European Union. Commission Regulation. (2012-08-12) [2015-08-31]. http://eur-lex.europa.eu/legal-content/EN/ALL/?uri=CELEX: 32002D0657
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