动物性食品样品中多肽类抗菌药物的超高效液相色谱-串联质谱快速测定法  

Rapid determination of polypeptide antibiotics in animal food samples by ultra high liquid chromatography-series mass spectrometry

作　　者：李敏[1] 王紫纹[1] 刘佳[1] 李斯[1] LI Min;WANG Zi-wen;LIU Jia;LI Si(Physical and Chemical Laboratory,Beijing Xicheng District Centers for Disease Control and Prevention,Beijing,100120,China)

机构地区：[1]北京市西城区疾病预防控制中心理化检验科

出　　处：《职业与健康》2019年第24期3341-3345,共5页Occupation and Health

摘　　要：目的建立超高效液相色谱质谱法快速测定动物性食品中粘杆菌素A、粘杆菌素B、多粘菌素B和万古霉素4种多肽类抗菌药物的方法。方法针对不同的样品,采用两种提取方法提取:动物肝脏类脂肪含量较高的肉类采用1%的乙酸乙腈水-正己烷提取,HLB固相萃取柱净化;蛋白质含量高的样品采用2%的三氯乙酸水溶液提取,WCX弱阳离子固相萃取柱富集净化。电喷雾正离子模式下液相色谱质谱法进行定性和定量分析。结果4种多肽类抗菌药物采用2种提取方法提取后,3个添加水平的平均回收率范围在62.8%~131.5%,每种物质的相对标准偏差均在10%范围内,定量限均可达到10μg/kg。测定物质在10~500μg/kg范围内均呈良好线性。线性相关系数>0.995。结论本方法针对不同的样品,采用不同的提取方式,均能够快速和准确地用于动物性食品中多肽类抗菌药物的测定。Objective To establish a liquid chromatography-mass spectrometry method for the rapid determination of polypeptide antibiotics in animal foods,including Colistin A,Colistin B,Polymyxin B and Vancomycin.Methods For different samples,two extraction methods were used:the meat with higher fat content in animal liver was extracted with 1%acetic acid acetonitrile water-n-hexane,and purified by HLB solid phase extraction column,while the sample with high protein content was extracted with 2%aqueous solution of trichloroacetic acid and purified by WCX weak cationic solid phase extraction column.Qualitative and quantitative analysis was performed by liquid chromatography mass spectrometry in electrospray positive ion mode.Results After four kinds of polypeptide antibiotics were extracted with two methods,the average recovery range of the three addition levels ranged from 62.8%to 131.5%,the relative standard deviation of each substance was within 10%,and the limit of quantification reached 10μg/kg.The measured substance showed good linearity in the range of 10-500μg/kg,and the linear correlation coefficient was>0.995.Conclusion With different extraction methods for different samples,this method can be used for the rapid and accurate determination of polypeptide antibiotics in animal food.

关 键 词：液相-色谱质谱 多肽类抗菌药物 粘杆菌素 多粘菌素 万古霉素 动物性食品 

分 类 号：R115[医药卫生—公共卫生与预防医学]