A method was established for the simultaneous determination of vancomycin and norvancomycin residues in milk and dairy products by solid-phase extraction and ultra performance liquid chromatography coupled with tandem mass spectrometry(UPLC-MS/MS).The sample was extracted with a mixed solution of acetonitrile and water.Then the protein was precipitated with trichloroacetic acid, the fat and other impurities were eliminated with dichloromethane.The extration solution was purified with Strata-X-C solid phase extraction(SPE) column.The target compounds were separated on a reversed phase column by gradient elution of acetonitrile and 0.1% formic acid water solution,and then detected with positive electrospray ionization under multiple reaction monitoring(MRM) mode.The SPE conditions and UPLC-MS/MS parameters were optimized.Under the optimized conditions,the calibration curves for two target compounds were linear in the range of 4-5 000 μg/L with correlation coefficients(r2) greater than 0.99.The average recoveries of blank matrix sample at three spiked levels of 15,60, 150 μg/kg were all more than 80%,and the relative standard deviations(RSDs)were less than 5%.The limits of detection(LODs)for vancomycin and norvancomycin were 0.5 μg/kg and 0.8 μg/kg,respectively.The limits of quantitation(LOQs)were 2.0 μg/kg and 3.0 μg/kg,respectively.The method was practical,accurate and sensitive,and was suitable for the determination of vancomycin and norvancomycin in milk and dairy products.
关键词
液相色谱-串联质谱固相萃取乳和乳制品万古霉素去甲万古霉素
Keywords
UPLC-MS/MSsolid phase extractionmilk and dairy productsvancomycinnorvancomycin
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Key Laboratory of Pesticide Environmental Assessment and Pollution Control,Ministry of Environmental Protection,Nanjing Institute of Environmental Sciences,Ministry of Ecology and Environment of the People’s Republic of China
College of Carbon Neutral Modern Industry,College of Environmental and Resource Science,Fujian Normal University