Determination of zearalanol and related mycotoxins in pork by solid-phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry

doi:10.3724/SP.J.1123.2012.12033

Abstract

Abstract:

A method was established for the determination of six compounds of zearalanol and related mycotoxins in pork and its products. After hydrolysis of the target compounds in the pork by β-glucosidase/sulfatase, they were extracted with methanol aqueous solution and further purified by an HLB column. The separation was performed on a BEH C18 column with gradient elution using acetonitrile-water as mobile phases. The analytes were determined by mass spectrometry using electrospray ionization (ESI) in negative scan mode and multiple reaction monitoring (MRM) mode. α-Zearalenol-D7 and β-zearalenol-D7 were used as internal standards. The good linearities (r >0.999) were achieved for the six compounds over the range of 1.0-100 μ g/L based on the internal standard calibration. The detection limits of the method were 0.03-0.09 μ g/kg. The mean recoveries of the six target compounds spiked at three levels from 1.0-10.0 μ g/kg ranged from 76.7% to 100.5% with the relative standard deviations (RSDs) less than 20%. The proposed method is simple, sensitive, reproducible, and complies with the regulations for the determination of trace contaminant residues in food matrices.

Key words: mycotoxin, solid-phase extraction (SPE), ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), zearalanol

CLC Number:

O658

LI Liping, FAN Sai, ZHAO Rong, LI Bing, LIU Wei, WU Guohua. Determination of zearalanol and related mycotoxins in pork by solid-phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2013, 31(7): 703-708.

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