Determination of fipronil and its metabolites in eggs by UPLC-QqLIT-MS/MS with multistage mass spectrometry mode. Issue 9 (28th May 2018)

• Record Type: Journal Article
• Authors: Wang, Ni; Wang, Chenchen; Li, Huidong; Fang, Liping; Ding, Ruiyan; Mao, Jiangsheng; Chen, Zilei; Yang, Guosheng; Aboul-Enein, Hassan Y.
• Is Part Of: Journal of liquid chromatography & related technologies. Volume 41:Issue 9(2018)
• Page Start: 544
• Page End: 551
• Publication Date: 2018-05-28
• Subjects: Eggs -- Fipronil -- Metabolites -- Multistage mass spectrometry -- Ultra-performance liquid chromatography-quadrupole-linear ion trap mass spectrometry; Liquid chromatography -- Periodicals; Chromatographic analysis -- Periodicals; Separation (Technology) -- Periodicals; Biotechnology -- Periodicals; Chromatography, Liquid -- Periodicals; 543.8405
• DOI: 10.1080/10826076.2018.1485041
• Languages: English
• ISSNs: 1082-6076

Abstract

Abstract: A fast, sensitive, and reliable method for the determination of fipronil and its metabolites (fipronil-sulfone, fipronil sulfide, and fipronil-desulfynil) in eggs was developed by a modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) pretreatment method and ultra-performance liquid chromatography-quadrupole-linear ion trap mass spectrometry (UPLC-QqLIT-MS/MS). The proposed multistage mass spectrometry (MS 3 ) method provides sufficient sensitivity and excellent reproducibility. The four analytes were separated by a Waters ACQUITY UPLC ® BEH C18 column and detected by AB Sciex QTRAP ® 5500. The mean recoveries for the four analytes ranged from 90.7% to 105% with relative standard deviations (RSDs) of 0.7% to 4.9%. The calibration curve showed a good linearity within the concentration range of 0.05 to 20 ng/mL. The correlation coefficients (R 2 ) were higher than 0.999. The limits of detection (LODs) obtained from the experimental results for fipronil, fipronil-sulfone, fipronil-sulfide, and fipronil-desulfinyl were 0.06, 0.02, 0.05, and 0.04 µg/kg, respectively. The MS 3 method was successfully applied to detect fipronil and its metabolites in 60 egg samples purchased from Chinese supermarkets, and wholesale markets. Graphical Abstract: