Chinese Journal of Chromatography

Chinese Journal of Chromatography ›› 2017, Vol. 35 ›› Issue (12): 1216-1223.DOI: 10.3724/SP.J.1123.2017.09026

Previous Articles     Next Articles

Rapid screening of fipronil and its metabolites in egg and egg products by solid phase extraction-liquid chromatography-quadrupole time-of-flight mass spectrometry

GUO Dehua1, SHI Yiyin1, LI You1, YI Xionghai1, DENG Xiaojun1, XIAO Wenqing1, WANG Jian1, LI Xiao1, LIU Han2, SHEN Weijian2   

  1. 1. Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China;
    2. Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China
  • Received:2017-09-14 Online:2017-12-08 Published:2017-12-15
  • Supported by:

    Project of Shanghai Science and Technology Commission 2015 Annual Field of Scientific Instruments (No. 15142201700).

PDF

232

Abstract:

A method for rapid screening of fipronil and its metabolites in egg and egg products was developed by liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (LC-QTOF MS). The samples were extracted by acid-acetonitrile, cleaned up by PRiME HLB SPE. The separation was performed on a Poroshell 120 EC C18 column (150 mm×3 mm, 2.7 μm) with gradient elution using water and acetonitrile as mobile phases. The target compounds were monitored under negative ionization mode with electrospray ionization (ESI) source and two databases of accurate mass and fragment ions were created. The matrix effects in four kinds of egg and egg products were considered and the quantification was carried out by internal standard method. The results demonstrated that the linear ranges were from 0.1 to 5 μg/L with good correlation coefficients (r2>0.99). The limits of detection (LODs, S/N>3) and limits of quantitation (LOQs, S/N>10) were 0.2 μg/kg and 1 μg/kg, respectively. The recoveries of fipronil and its metabolites in different matrixes spiked with 1, 2 and 5 μg/kg varied from 82.6%-98.1%, and the relative standard deviations (RSDs) were between 3.8%-9.9% (n=6). The method can effectively correct the ionization suppression. It is sensitive, accurate and suitable for the rapid screening of fipronil, fipronil sulfide, fipronil sulfone and fipronil desulfinyl in egg, egg noodle, cake and mayonnaise.

Key words: egg and egg products, fipronil and its metabolites, liquid chromatography-quadrupole time-of-flight mass spectrometry (LC-QTOF MS), screening, solid phase extraction (SPE)

CLC Number: