高效液相色谱-串联质谱测定猪肉中万古霉素、去甲万古霉素和替考拉宁  

Determination of Vancomycin, Norvancomycin and Teicoplanin in Pork by High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：卢剑[1] 范素芳[2,3] 李强[2,3] 夏静[2,3] 李挥[2,3] 张岩[2,3] 

机构地区：[1]江苏省产品质量监督检验研究院,江苏南京210029 [2]河北省食品检验研究院,河北石家庄050091 [3]河北省食品安全重点实验室,河北石家庄050091

出　　处：《食品科学》2016年第10期193-197,共5页Food Science

基　　金：国家自然科学基金青年科学基金项目(31401584);河北省自然科学基金面上项目(C2015321005)

摘　　要：建立猪肉样品中万古霉素、去甲万古霉素和替考拉宁的高效液相色谱-串联质谱测定方法,采用选择反应监测方式,外标法定量。猪肉样品经0.1%甲酸-乙腈（85：15,V/V）溶液提取,正己烷脱脂后,万古霉素和去甲万古霉素经阳离子交换柱净化、替考拉宁经C18固相萃取柱净化,以乙腈-0.1%甲酸为流动相梯度洗脱,经C18柱分离、质谱进行测定。添加量为10、20 μg/kg和50 μg/kg时,方法回收率范围为75.3%-83.3%,相对标准偏差小于9%。猪肉中万古霉素、去甲万古霉素的检出限、定量限分别为2 μg/kg和4 μg/kg,替考拉宁的检出限、定量限分别为4 μg/kg和8 μg/kg。该方法适用于猪肉样品中万古霉素、去甲万古霉素和替考拉宁的定性、定量检测。A high performance liquid chromatography-tandem mass spectrometry method was developed for the determination of vancomycin, norvancomycin and teicoplanin in pork samples. The selective reaction monitoring mode was applied in the experiment and an external standard method was used for quantification. Pork samples were weighed, extracted with deionized water containing 0.1% formic acid-acetonitrile（85：15, V/V）. Hexane was added to decrease fatty acid. Vancomycin and norvancomycin were cleaned on a cation exchange column, while teicoplanin was cleaned up on an SPE C18 cartridge. Acetonitrile-water containing 0.1% formic acid was used as mobile phase and gradient elution was used in the experiment. The analytes were separated on a C18 column and then detected by mass spectrometry. The average recoveries of the method were in range of 75.3%-83.3% at spike levels of 10, 20 and 50 μg/kg, with relative standard deviations（RSDs） lower than 9%. The Limit of detection（LOD） and the limit of quantitation（LOQ） were 2 and 4 μg/kg for vancomycin, and 4 and 8 μg/kg for norvancomycin, respectively. The method could be used for the qualitative and quantitative detection of vancomycin, norvancomycin and teicoplanin in pork samples.

关 键 词：猪肉 万古霉素 去甲万古霉素 替考拉宁 高效液相色谱-串联质谱 

分 类 号：TS207.3[轻工技术与工程—食品科学]