高效液相色谱-串联质谱法测定动物肺组织中青霉素G和青霉素V  

Simultaneous Determination of Penicillin G and Penicillin V in Animal Lungs by High-performance Liquid Chromatography-mass Spectrometry/mass Spectrometry

作　　者：付体鹏[1,2] 李莉[2] 张峰[2] 储晓刚[2] 游洋[1] 许成保 刘力[1] 

机构地区：[1]西南大学,重庆400715 [2]中国检验检疫科学研究院,北京100123

出　　处：《安徽农业科学》2013年第2期638-639,654,共3页Journal of Anhui Agricultural Sciences

基　　金：国家科技支撑计划项目(2009BADB9B02);质检公益性行业科研项目(200910145)

摘　　要：[目的]建立一种动物肺组织中青霉素G和青霉素V的高效液相色谱-电喷雾-三重四极杆质谱检测方法。[方法]样品中青霉素经磷酸二氢钠溶液提取,加正己烷去除脂肪后过SPE柱,乙腈洗脱,氮气吹干后用乙腈-水(1∶1,V/V)定容至1 ml,过膜后采用AgilentEclipse Plus C18柱高效液相色谱分离,电喷雾串联质谱法检测,负离子模式下多反应监测,标准曲线法定量。[结果]加标水平为5.0、10.0和20.0μg/kg时,回收率在73.58%～101.18%,相对标准偏差为3.00%～8.82%,仪器检出限为0.1μg/L,方法的定量限均为5.0μg/kg。[结论]该方法快速、灵敏、操作简单、准确性高,可满足对动物肺组织中青霉素G和青霉素V残留的定量分析要求。[Objective] The aim was to establish a HPLC-MS/MS method to simultaneously determine penicillin G and penicillin V in animal lungs.[Method] These two kinds of penicillin in animal lungs were extracted by sodium dihydrogen phosphate,then purified by solid phase extraction cartridges after eliminating fat by normal hexane,blow dry by nitrogen after elution by acetonitrile.Constant volume to 1 ml by acetonitrile-water（1∶1,V/V）,analysis after filtration.LC analysis was performed on Agilent Eclipse Plus C18 column.Electro spray ionization and mass spectrometer were used to analyze these antibiotics by using negative ion.Standard curve method was used to quantitative calculation.[Result] When the labeled level were 5.0,10.0 and 20.0 μg/kg,the average recoveries were 73.58%-101.18%,and the relative standard deviation were 3.00%-8.82%.the limit of detection（LOD） was 0.1 μg/L,and the limit of quantitative（LOQ） was 5.0 μg/kg.[Conclusion] The method is fast,responsive,easy and accurate,and it is suitable for quantitative analysis of penicillin G and penicillin V in animal lungs.

关 键 词：高效液相色谱-电喷雾串联质谱 肺 青霉素G 青霉素V 固相萃取 

分 类 号：S121[农业科学—农业基础科学]