牛奶中青霉素G及青霉噻唑酸的UPLC-MS/MS法测定  

Simultaneous Detection of Penicillin G and Benzylpenicillin Acid in Milk by UPLC-MS/MS

作　　者：刘静[1,2] 郑增忍[2] 赵思俊[2] 曲志娜[2] 王君玮[2] 孙晓亮[2] 谭维泉[2] 刘坤[2] 曹旭敏[2] 邹明[1] 

机构地区：[1]青岛农业大学,山东青岛266109 [2]中国动物卫生与流行病学中心,山东青岛266032

出　　处：《动物医学进展》2014年第9期85-89,共5页Progress In Veterinary Medicine

摘　　要：为建立同时检测牛奶中青霉素G及青霉噻唑酸的UPLC-MS/MS检测法,将牛奶样品经乙腈∶乙醇(3∶1,V∶V)提取后离心分离,用Oasis HLB固相萃取柱净化,进行超高效液相色谱-串联质谱法检测。青霉素和青霉噻唑酸在线性范围内相关系数在0.993以上,方法的检出限(LOD,S/N=3)为0.3μg/kg^0.5μg/kg,定量限(S/N=10)为1.0μg/kg^2.0μg/kg。选用基质添加标准曲线消除基质干扰,样品加标回收率为75.88%~106.01%,变异系数为6.65%~14.17%。说明方法的灵敏度高,重复性良好,为快速准确的检测该类药物提供可靠的技术支撑。An ultra performance liquid chromatography tandem mass spectrometric （UPLC-MS/MS）anal-ysis method was established for simultaneous analysis of penicillin G and benzylpenicillin acid in milk.The milk samples were precipitated with acetonitrile：alcohol（3 ∶ 1,V∶ V）,and the extracts were applied to HLB cartridge for clean up,the separation was performed by ultra performance liquid chromatography-tan-dem mass spectrometry.The correlation coefficients were above 0.993.The detection limits （S/N〉3）of penicillin acid G and benzylpenicillin acid were 0.3 μg/kg-0.5 μg/kg.The detection limits （S/N〉10）of penicillin G and benzylpenicillin were 1.0 μg/kg-2.0 μg/kg.The results quantified by matrix spiked cali-bration curve,the recoveries ranged from 75.88%-106.0%,and RSD were in the range of 6.65%-14.17%. The method is sensitive and repeatable,and can be applied to the field of residue analysis about penicillin and their metabolites.

关 键 词：超高效液相色谱-串联质谱 青霉素G 青霉噻唑酸 牛奶 

分 类 号：S859.84[农业科学—临床兽医学]