超高效液相色谱-串联质谱法测定牛奶中4种β-内酰胺类抗生素及其主要代谢产物  

Determination of 4 kinds ofβ-lactam antibiotics and their main metabolites in milk by ultra performance liquid chromatography tandem mass spectrometry

作　　者：路杨[1] 王丽英[1] 秦振顺[1] 任贝贝[1] 刘梦颖 常凤启[1] LU Yang;WANG Li-Ying;QIN Zhen-Shun;REN Bei-Bei;LIU Meng-Ying;CHANG Feng-Qi(Hebei Provincial Center for Disease Control and Prevention,Shijiazhuang 050021,China)

机构地区：[1]河北省疾病预防控制中心,石家庄050021

出　　处：《食品安全质量检测学报》2021年第5期1662-1668,共7页Journal of Food Safety and Quality

基　　金：河北省卫健委项目(20090036)。

摘　　要：目的建立超高效液相色谱-串联质谱法检测牛奶中青霉素G、青霉素V、氨苄西林、阿莫西林及其代谢产物脱羧噻唑酸含量的分析方法。方法样品经0.2%氨水乙腈溶液超声离心提取,通过Oasis PRiME HLB固相萃取柱进行净化,采用超高效液相色谱-串联质谱法进行测定。结果青霉素G、青霉素V、氨苄西林、阿莫西林及其代谢产物脱羧噻唑酸在所考察的线性范围内线性良好,相关系数不低于0.999;方法回收率为70.9%~101.6%,相对标准偏差(relative standard deviation, RSD)为4.0%~7.5%。市售的35份样品中,均未检出青霉素G、青霉素V、阿莫西林、氨苄西林及其代谢产物。结论该方法操作简单、重现性好,可用于牛奶中青霉素G、青霉素V、阿莫西林、氨苄西林及其代谢产物脱羧噻唑酸的检测。Objective To establish a analytical method for the determination of penicillin G,penicillin V,ampicillin,amoxicillin and their metabolites decarboxythiazolinic acid in milk by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods After the target compound were extracted from sample by 0.2%ammonia acetonitrile solution and purified by solid-phase extraction with Oasis PRiME HLB,and the samples were analyzed by UPLC-MS/MS.Results The linearity of penicillin G,penicillin V,ampicillin,amoxicillin and their metabolites decarboxythiazolinic acid was good within the investigated linear range,and the correlation coefficients were not less than 0.999;the recoveries of the method were 70.9%‒101.6%and the relative standard deviations were 4.0%‒7.5%.Penicillin G,penicillin V,amoxicillin,ampicillin,and their metabolites were not detected in 35 commercially available samples.Conclusion This method is simple and reproducible,and can be used for the detection of penicillin G,penicillin V,amoxicillin,ampicillin and their metabolites decarboxythiazolic acid in milk.

关 键 词：Β-内酰胺类抗生素 牛奶 超高效液相色谱-串联质谱法 

分 类 号：O657.63[理学—分析化学] TS252.7[理学—化学]