Determination of five β2-agonist residues in pork by ultra-high performance liquid chromatography-tandem mass spectrometry with molecularly imprinted solid phase extraction

doi:10.3724/SP.J.1123.2015.04016

Abstract

Abstract:

An ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method with molecularly imprinted solid phase extraction for the determination of five β₂-gonists residues in pork has been developed. After the sample preparation, the ammonium acetate/acetic acid buffer was added, followed by the internal standard and β-glucuronidase/arylsulfatase enzyme. The solution was incubated at 55 ℃ for 2 h. After adjusting the pH of the solution, it was purified by a molecularly imprinted solid phase extraction column, then analyzed on a BEH C18 column with methanol-0.1% (v/v) formic acid aqueous solution as the mobile phases in gradient elution mode. The MS/MS analysis was in positive ion mode and multiple reaction monitoring mode. The analytes were quantified by the internal standard method. The limits of detection (LODs, S/N=3) and the limits of quantification (LOQs, S/N=10) were 0.005-0.009 μg/kg and 0.015-0.025 μg/kg, respectively. In the range of 0-10 μg/kg, the correlation coefficients of linear calibration curves were not less than 0.9933. At the spiked levels of 0.25, 1.0 and 5.0 μg/kg, the recoveries were 80.4%-92.9% with the relative standard deviations of 1.3%-6.3%. The method is of high sensitivity, good reproducibility, high recovery, and is useful for the simultaneous determination of multiple β₂-agonists residues.

Key words: β₂-gonists, molecularly imprinted solid phase extraction, pork, residues, ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

CLC Number:

O658

ZHANG Xueliang, LUO Yunjing, JIANG Jie, LU Yong, FENG Nan. Determination of five β₂-agonist residues in pork by ultra-high performance liquid chromatography-tandem mass spectrometry with molecularly imprinted solid phase extraction[J]. Chinese Journal of Chromatography, 2015, 33(8): 838-842.

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Determination of five β₂-agonist residues in pork by ultra-high performance liquid chromatography-tandem mass spectrometry with molecularly imprinted solid phase extraction

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