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摘要:
An ultra-high performance liquid chroniatography-tandein mass spectrometry (UPLC-MS/MS) method with molecularly imprinted solid phase extraction for the determina-tion 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-glu-curonidase/arylsidfat ase enzyme. The solution was incubated at 55 °C for 2 h. After adjusting the pH of the solution, it was purified by a molecularly imprinted solid phase extraction col-umn, then analyzed on a BEH C18 column with inethanol-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 modi1. The analytcs 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, hi the range of 0-10 μg/kg, the correlation coefficients of linear calibration curves were not less than 0. 993 3. 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.
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来源 :
Chinese Journal of Chromatography (Se Pu)
ISSN: 1000-8713
年份: 2015
期: 8
卷: 33
页码: 838-842