分析测试学报2013,Vol.32Issue(2):162-167,6.DOI:10.3969/j.issn.1004-4957.2013.02.004
UPLC-MS/MS法测定猪肉中万古霉素与去甲万古霉素
Quantitative Determination of Vancomycin and Norvancomycin in Pork by Ultrahigh Performance Liquid Chromatography-Tandem Mass Spectrometry
摘要
Abstract
A simple, rapid and sensitive method was developed for the simultaneous determination of vancomycin and norvancomycin in pork by ultra-high performance liquid chromatography - tandem mass spectrometry (UPLC - MS/MS). The sample was supersonically extracted with a mixture of 0. 1 % formic acid - acetonitrile (7: 3), and cleaned up with hexane ( acetonitrile saturated) and a LC - C18 solid phase extraction cartridge. The separation of two targets was carried out on a Waters UPLC BEH C18 column by gradient elution with 0. 1% formic acid - acetonitrile as mobile phase. With positive electrospray ionization (ESI+) and multiple reaction monitoring (MRM), the two com pounds were identified with retention time and ion ratio. The results showed that the two compounds displayed excellent peak shapes within 3 min with correlation coefficients more than 0. 99. The limits of detection (LOD, S/N=3) of vancomycin and norvancomycin were 0. 5 μg/kg and 0. 3 μg/kg, respectively. The average recoveries were between 80% and 88% for the target compounds at spiked levels of 1 - 20 μg/kg. The intra-day RSDs were no more than 13. 4%, and the inter-day RSDs were no more than 12. 5% . The method was accurate and sensitive, and was suitable for the quantitative and qualitative analyses of glycopeptide antibiotics in pork sample.关键词
万古霉素/去甲万古霉素/猪肉/超高效液相色谱串联质谱法Key words
vancomycin/ norvancomycin/ pork/ ultra-high performance liquid chromatography -tandem mass spectrometry (UPLC - MS/MS)分类
化学化工引用本文复制引用
冼燕萍,陈立伟,罗海英,郭新东,吴玉銮,罗东辉,侯向昶..UPLC-MS/MS法测定猪肉中万古霉素与去甲万古霉素[J].分析测试学报,2013,32(2):162-167,6.基金项目
广州科信局资助项目(11C13190775) (11C13190775)
广州市科技计划项目([2011] 233-34) ([2011] 233-34)
广州市质量监督局科技项目(2012kj02) (2012kj02)