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| Determination of Vancomycin and Norvancomycin Residues in Milk and Dairy Products by Solid Phase Extraction/UPLC-MS/MS |
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| DOI：10.3969/j.issn.1004-4957.年份.月份 |
| KeyWord:UPLC-MS/MS solid phase extraction milk and dairy products vancomycin norvancomycin |
| Author | Institution |
| 綦艳，李锦清,赵明桥,龙顺荣,郦明浩，佘之蕴，黄宝莹 |
广东产品质量监督检验研究院 |
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| Abstract: |
| 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. |
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