UPLC/MS/MS法测定猪肉中万古霉素残留量

Determination of Vancomycin in meat by Ultra Performance Liquid chromatography-tandem mass spectrometry

建立了快速、准确、灵敏的猪肉中万古霉素的超高效液相色谱-串联质谱法(UPLC-MS/MS)检测方法。样品经0.1%甲酸-乙腈(1:1,体积比)溶液提取,scx固相萃取柱净化,洗脱液蒸干后正己烷除脂,采用乙腈-0.1%甲酸水为流动相进行梯度洗脱,ESI^+正离子模式电离,多反应监测模式(MRM)监测,用UPLC-MS/MS检测和确证,外标法定量。结果表明,万古霉素在5.0～200.0μg/L范围内具有良好的线性,相关系数r=0.998 9,检测限(S/N=3)为1.0μg/kg,定量限为3.0μg/kg,方法平均回收率为82.4%～101.4%,相对标准偏差在5.3%～17.3%。试验结果表明,该方法准确、灵敏,适用于猪肉中万古霉素残留量的测定。

A simple, rapid and sensitive method was developed for determination of vancomycin in pork by Ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). The sample was extracted with a mixture of 0.1% formic acid–acetonitrile(1:1), and cleaned up with SCX solid phase extraction cartridge. The separation of the target was carried out on a 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 results showed that correlation coefficient was 0.9989. The LOD and LOQ of vancomycin were 1.0 μg/kg and 3.0 μg/kg. The average recoveries were between 82.4%~101.4% at spiked levels of 5~15 μg/kg. The RSD were 5.3%~17.3%. The real sample tests showed this method can be used for the sensitive and accurate determination of Vancomycin residues in meat.