DOI: 10.3724/SP.J.1123.2017.03033

Chinese Journal of Chromatography (色谱) 2017/35:8 PP.860-866

Determination of pyrethroid pesticides in tea by series two-solid phase extraction-columns cleanup and gas chromatography-tandem mass spectrometry

A rapid determination method of three pyrethroid pesticides (cyfluthrin, cypermethrin and fenvalerate) in tea was developed by series two-solid phase extraction-column cleanup and external standard method coupled with gas chromatography-tandem mass spectrometry (GC-MS/MS) in 30 min. The pesticide residues in tea were extracted with acetonitrile, and cleaned up by Carb/NH2 and SLH solid-phase extraction columns. After filtration, the target compounds were analyzed by GC-MS and quantified by the external standard method. Under the optimized conditions, good linear ranges of 0.05-2.00 mg/kg were obtained. The limits of detection varied from 0.3 to 1.0 μ g/kg. The linear correlation coefficients were greater than 0.999. At three spiked levels (0.10, 0.50 and 2.00 mg/L), the average recoveries were determined between 80.6% and 116.3% in the four matrices. The inter-day relative standard deviations were between 1.3%-12.6%, and the intra-day relative standard deviations were between 2.7% and 12.1%. This method is simple, fast, and has a good reproducibility, which can meet the requirements of the rapid detection of pyrethroid pesticides in tea.

Key words:gas chromatography-tandem mass spectrometry (GC-MS/MS),pyrethroid pesticides,tea

ReleaseDate:2017-11-03 11:22:02

[1] Zortéa T, Baretta D, Maccari A P, et al. Chemosphere, 2015(122):94

[2] Bing X, Ru S G. China Environmental Science, 2009, 29(2):152邴欣, 汝少国. 中国环境科学, 2009, 29(2):152

[3] Farag A T, Goda N F, Shaaban N A, et al. Reprod Toxicol, 2007, 23(4):560

[4] Rodriguez H, Tamayo C, Inostroza J, et al. Ecotox Environ Safe, 2009, 72(2):658

[5] Babina K, Dollard M, Pilotto L, et al. Environ Int, 2012, 48:109

[6] European Commission. EU Pesticides Database.[2017-03-20].

[7] GB 2763-2016

[8] Ye J L, Jin G E, Wu Y H, et al. Food Science, 2013, 34(12):265叶江雷, 金贵娥, 吴云辉, 等. 食品科学, 2013, 34(12):265

[9] Rong J F, Wei H, Li Y J, et al. Chinese Journal of Chromatography, 2016, 32(4):194荣杰峰, 韦航, 李亦军, 等. 色谱, 2016, 32(4):194

[10] Li H S, Huang C Q, Jiang Q T, et al. Chinese Journal of Chromatography, 2016, 32(3):263李慧思, 黄超群, 蒋沁婷, 等. 色谱, 2016, 32(3):263

[11] Yu L, Song W, Lü Y N, et al. Chinese Journal of Chromatography, 2015, 33(6):597余璐, 宋伟, 吕亚宁, 等. 色谱, 2015, 33(6):597

[12] Liu S N, Zhao X Y, Dong X Q, et al. Chinese Journal of Chromatography, 2015, 33(11):1205刘松南, 赵新颖, 董晓倩, 等. 色谱, 2015, 33(11):1205

[13] Zhao C L, Ding R Y, Huo L G, et al. J AOAC Int, 2014, 97(4):1001

[14] Hou X, Lei S R, Qiu S T, et al. Food Chem, 2014, 153(15):121

[15] Liu T F, Yang D F, Dong M H, et al. Chinese Journal of Pesticide Science, 2015, 17(5):571刘腾飞, 杨代凤, 董明辉, 等. 农药学学报, 2015, 17(5):571

[16] Li Y, Guo M J, Yuan T. Chinese Journal of Health Laboratory Technology, 2016, 26(11):1579李晔, 郭蒙京, 袁佗. 中国卫生检验杂志, 2016, 26(11):1579

[17] Kuang H, Miao H, Hou X I, et al. J Chromatogr Sci, 2010, 48(9):771

[18] Li J M, Zhong D B, Wang Y Q, et al. Chinese Journal of Chromatography, 2010, 28(9):840李军明, 钟读波, 王亚琴, 等. 色谱, 2010, 28(9):840

[19] Ding H Y, Xie W, Jiang X Y, et al. Chinese Journal of Analysis Laboratory, 2009, 28(5):14丁慧瑛, 谢文, 蒋晓英, 等. 分析试验室, 2009, 28(5):14

[20] Hu B Z, Song W H, Xie L P, et al. Chinese Journal of Chromatography, 2008, 26(1):22胡贝贞, 宋伟华, 谢丽萍, 等. 色谱, 2008, 26(1):22

[21] Su J F, Zhong M S, Chen J, et al. Journal of Instrumental Analysis, 2015, 34(6):625苏建峰, 钟茂生, 陈晶, 等. 分析测试学报, 2015, 34(6):625

[22] Agilent Technologies. Use Methylbenzene and Graphite Carbon Black Agilent Bond Elut QuEChERS AOAC Kit to Optimize the Recovery of Flat Structure Pesticide in Spinach. (2009-08-03)[2017-03-20].

[23] Pan Y C, Yi X H, Deng X J, et al. Chinese Journal of Chromatography, 2012, 30(11):1159潘煜辰, 伊雄海, 邓晓军, 等. 色谱, 2012, 30(11):1159

[24] Chen H P, Liu X, Wang Q H, et al. Chinese Journal of Chromatography, 2011, 29(5):409陈红平, 刘新, 汪庆华, 等. 色谱, 2011, 29(5):409

[25] Cao X Y, Pang G F, Jin L H, et al. Chinese Journal of Chromatography, 2015, 33(4):389曹新悦, 庞国芳, 金铃和, 等. 色谱, 2015, 33(4):389

[26] Lin Z G, Jin Z, Liu Y, et al. Chemical Journal of Chinese University, 2005, 26(12):2218林竹光, 金珍, 刘勇, 等. 高等学校化学学报, 2005, 26(12):2218