Simultaneous determination of monepantel and its metabolite residues in cow and sheep milk by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry

doi:10.3724/SP.J.1123.2018.03014

Abstract

Abstract:

A method for the rapid and simultaneous determination of monepantel and its metabolite residues in cow and sheep milk has been developed using high performance liquid chromatography-tandem mass spectrometry. The samples were extracted with acetonitrile to precipitate the proteins and passed through a neutral alumina solid phase extraction (SPE) cartridge. The extracts were separated on an Inertsil C8-3 column (150 mm×4.6 mm, 5 μm) with a gradient elution program consisting of methanol and ammonium acetate. A triple stage quadrupole mass spectrometer equipped with an electrospray ionization source in negative ion mode was used to detect monepantel and its metabolite residues. The quantification of the analytes was performed by the external standard method. Good linear relationships between the peak areas and mass concentrations of the analytes were obtained in the range of 0.1-5.0 μg/L with correlation coefficients greater than 0.99 (n=6). The limits of quantification were 2.0 μg/kg. The recoveries of the analytes in cow and sheep milk at three spiked levels (2.0, 50, and 100 μg/kg) were in the range of 90.1%-103.3% with relative standard deviations between 2.0% and 6.2% (n=6). This method is fast, accurate, and highly sensitive, exhibits strong anti-interference capability with good recovery and repeatability, and can thus be used to simultaneously determine monepantel and its metabolite residues in cow and sheep milk.

Key words: high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), metabolites, milk, monepantel, solid phase extraction (SPE)

CLC Number:

O658

WU Yingxuan, XIE Minling, YAO Yangxun, LAN Cao. Simultaneous determination of monepantel and its metabolite residues in cow and sheep milk by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2018, 36(8): 752-757.

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