高效液相色谱串联质谱测定鸡、猪肉中万古霉素

Determination of Vancomycin in Chicken,Pork by High Performance Liquid Chromatography-tandem Mass Spectrometry

建立了鸡肉和猪肉样品中万古霉素的高效液相色谱串联质谱检测方法。鸡肉和猪肉样品经5%三氯乙酸:乙腈(4:1)提取,阳离子交换固相萃取柱净化后,以0.1%甲酸5 mmol乙酸铵溶液和乙腈作为流动相,经C 18色谱柱分离后,采用多反映离子监测模式进行测定,外标法定量。结果表明,万古霉素在1.0~20.0 ng/mL范围内呈现良好的线性关系,相关系数(r 2)大于0.99,在5,25,50μg/kg加标水平下,万古霉素平均回收率60%~120%,方法检出限(LOD)为2.0μg/kg,方法定量限(LOQ)为5.0μg/kg。

A high performance liquid chromatography-tandem mass spectrometry method was developed for the determination of vancomycin in chicken and pork samples.Chicken and pork samples were weighed,extracted with deionized water containing 5%trichloracetic acid-acetonitrile(4:1,V:V).Vancomycin was cleaned on a cation exchange column.Acetonitrile-water containing 0.1%formic acid 5 mmol ammonium acetate 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,an external standard method was used for quantification.The results showed that there was a good linear relationship in the range of 1.0~20.0 ng/mL,and the correlation coefficient(r 2)was greater than 0.99.The average recoveries of the method were in range of 60%~120%at spike levels of 5,25,50μg/k.The limit of detection(LOD)and the limit of quantification(LOQ)were 2 and 5μg/kg for vancomycin.