Determination of fipronil and its metabolites in feeds by stable isotope dilution ultra high performance liquid chromatography-tandem mass spectrometry

doi:10.3724/SP.J.1123.2018.01049

Abstract

Abstract:

A method based on ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was established for the determination of fipronil and its metabolites in feeds. Sodium chloride was added to the samples after the ultrasonic extraction of pure water and acetonitrile, and then cleaned up by the QuEChERS method. The target analytes were separated on a Waters HSS T3 C₁₈ column using methanol and water as mobile phases with gradient elution, and detected by a MS/MS system under negative electro-spry ionization (ESI^-) and the multiple reaction monitoring (MRM) mode. The limits of detection (LODs) were 0.05 μg/kg, and the limits of quantification (LOQs) were 0.2 μg/kg. The linear correlation coefficients were more than 0.9998. The average recoveries ranged from 92.3% to 105.4% with RSDs no more than 2.3%. This method is suitable for the identification of fipronil and its metabolites in feeds because of its simplicity and high sensitivity.

Key words: feeds, fipronil and its metabolites, isotope dilution, QuEChERS, ultra high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)

CLC Number:

O658

ZHOU Peng, HUANG Qian, OUYANG Liqun, WANG Zheng, MENG Peng, DAI Ming, WANG Ying. Determination of fipronil and its metabolites in feeds by stable isotope dilution ultra high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2018, 36(7): 629-633.

References

[1] Bonmatin J M, Giorio C, Girolami V, et al. Environ Sci Pollut Res, 2015, 22(1):35
[2] Pisa L W, Amaral-Rogers V, Belzunces L P, et al. Environ Sci Pollut Res, 2015, 22(1):68
[3] Simon-Delso N, Amaral-Rogers V, Belzunces L P, et al. Environ Sci Pollut Res, 2015, 22(1):5
[4] Ministry of Agriculture. No. 1157 Bulletin of the Ministry of Agriculture of the People's Republic of China. (2009-02-25)[2018-01-05]. http://www.moa.gov.cn/zwllm/tzgg/gg/200902/t20090227_1226994.htm 农业部. 中华人民共和国农业部公告第1157号. (2009-02-25)[2018-01-05]. http://www.moa.gov.cn/zwllm/tzgg/gg/200902/t20090227_1226994.htm
[5] GB 2763-2016
[6] Ye Q, Deng Y C, Lu D H, et al. Agrochemicals, 2016, 55(1):51 叶倩, 邓义才, 路大海, 等. 农药, 2016, 55(1):51
[7] Lü L, He L, Gan J H, et al. Chinese Journal of Analysis Laboratory, 2015, 34(7):847 吕磊, 何力, 甘金华, 等. 分析试验室, 2015, 34(7):847
[8] Zhao L, Hong X H, Rong G Q, et al. Journal of Food Safety and Quality, 2017, 8(10):3921 赵丽, 洪雪花, 荣国琼, 等. 食品安全质量检测学报, 2017, 8(10):3921
[9] Wang J L, Yan H P. Journal of Agriculture, 2016, 6(1):83 王洁莲, 阎会平. 农学学报, 2016, 6(1):83.
[10] Shen W J, Liu H, Zhang R, et al. Chinese Journal of Chromatography, 2017, 35(12):1224 沈伟健, 柳菡, 张睿, 等. 色谱, 2017, 35(12):1224
[11] Kaur R, Mandal K, Kumar R, et al. J AOAC Int, 2015, 98(2):464
[12] Hu Gui X, Xia X, Zhu H F. Chemical Reagent, 2017, 39(5):509 胡贵祥, 夏祥, 朱慧芳. 化学试剂, 2017, 39(5):509
[13] Qin L, Wang S, Cai Y Q. Chinese Journal of Health Laboratory Technology, 2017, 27(9):1247 覃玲, 王生, 蔡亚清. 中国卫生检验杂志, 2017, 27(9):1247
[14] Zhou H X, Bi L F, Zang R Y, et al. Food Research and Development, 2017, 38(19):166 周宏霞, 毕乐飞, 臧汝瑛, 等. 食品研究与开发, 2017, 38(19):166
[15] Li J, Zheng X, Wang H Q, et al. Chinese Journal of Chromatography, 2017, 35(12):1211 励炯, 郑锌, 王红青, 等. 色谱, 2017, 35(12):1211
[16] Guo D H, Shi Y Y, Li Y, et al. Chinese Journal of Chromatography, 2017, 35(12):1216 郭德华, 时逸吟, 李优, 等. 色谱, 2017, 35(12):1216
[17] Li M H, Li P Y, Wang L, et al. J Agric Food Chem, 2015, 63(18):4435
[18] Lü B, Yin S X, Chen D W, et al. Journal of Instrumental Analysis, 2017, 36(12):1424 吕冰, 尹帅星, 陈达炜. 分析测试学报, 2017, 36(12):1424