UPLC-MS/MS法同时测定动物源性食品中8种多肽类抗生素

Determination of eight polypeptide antibiotics in animal derived food by ultra performance liquid chromatography tandem mass spectrometry

建立了一种超高效液相色谱-串联质谱（UPLC-MS/MS）同时测定动物源性食品中8种多肽类抗生素残留量分析方法。试样经甲醇-水-甲酸（40∶60∶0.1,v/v/v）提取,固相萃取法净化后,以0.1%甲酸水溶液和0.1%甲酸乙腈溶液为流动相,梯度洗脱,经C18色谱柱分离后,在正离子扫描模式下,采用选择反应监测（SRM）,外标法定量。结果表明,8种多肽抗生素方法检出限为0.1~10μg/kg,去甲万古霉素和万古霉素在20~1000μg/L范围内,多粘菌素B和E在40~1000μg/L范围内,杆菌肽A在10~1000μg/L范围内,杆菌肽B在6~614μg/L范围内,维吉尼霉素M1和S1在1~100μg/L范围内,线性关系良好,相关系数r〉0.999,加标回收率为61.0%~99.6%,RSD为1.2%~9.8%。该方法简便快速、灵敏度高、重现性好,可满足动物源性食品中多肽类抗生素残留的同时测定。

An ultra performance liquid chromatography tandem mass spectrometry（UPLC-MS-MS） method had been established for the simultaneous determination of eight polypeptide antibiotics in animal derived food.Test sample was extracted by methanol-water-formic acid（40∶60∶0.1,v/v/v）,followed by cleaning up method based on solid phase extraction（SPE）. Extracts were separated on a C18 column using a gradient elution of0.1% formic acid water solution and 0.1% formic acid acetonitrile solution. Analytes were detected by ultra-perform liquid chromatography tandem mass spectrometry in positive ion mode with selected reaction monitoring（SRM）. The results showed that the limits of detection（LOD） of 8 polypeptide antibiotics were 0.1~10 μg/kg.The calibration curves for norvancomycin and vancomycin（concentration range 20~1000 μg/L）,polymyxin B and E（concentration range 40 ~1000 μg/L）,bacitracin A（concentration range 10 ~1000 μg/L）,bacitracin B（concentration range 6~614 μg/L）,virginiamycin M1 and S1（concentration range 1~100 μg/L） were linear with correlation coefficients more than 0.999. The recoveries were in the range of 61.0% ~99.6%. The relative standard deviations（RSDs） ranged from 1.2%~9.8%. The method was simple and rapid with high sensitivity and good reproducibility,and was appropriate for the identification and quantification of polypeptide antibiotics residue in animal derived food.