高效液相-串联质谱法测定猪肉中7种青霉素残留量  

Determination of seven kinds of penicillin residues in pork by high performance liquid chromatography-mass spectrometry

作　　者：陈娟 翟纹静 CHEN Juan;ZHAI WENJING

机构地区：[1]苏州出检验检疫综合技术中心/苏州华博检测技术有限公司

出　　处：《肉类工业》2019年第10期47-51,共5页Meat Industry

摘　　要：[目的]建立了高效液相色谱串联质谱法对猪肉中7种青霉素类药物残留的快速分析。[方法]样品经乙腈提取,涡旋混匀离心后氮吹干,加入10mL0.5%乙酸-50g/L钨酸钠混合液溶解。经过Waters Oasis HLB固相萃取柱净化,经高效液相色谱-串联质谱测定,外标法定量。选用Atlantis d C18色谱柱(2.1×150 mm,3μm)为分析柱,0.1%甲酸水溶液和0.1%甲酸乙腈为流动相,电喷雾正离子多反应监测模式(MRM)进行检测。[结果]7种目标化合物在选定浓度范围内线性关系良好,相关系数(r^2)均大于0.99。方法的检出低限(LOQ)为0.5~10μg/kg,3个添加水平的加标回收率为65.10%~101.12%,相对标准偏差在0.65%~5.39%(n=7)。[结论]本方法前处理简便、灵敏度高、重复性好,可用于猪肉样品中7种青霉素的定量检测。[Objective]High performance liquid chromatography-mass spectrometry was established for rapid analysis of seven kinds of penicillin residues in pork.[Method]The sample was extracted by acetonitrile,and vortexed and mixed,and dried by nitrogen,and 10 mL mixture with 0.5%acetic acid and 50 g/L sodium tungstate was added to dissolve,and purified by Waters Oasis MCX solid phase extraction column,and determined by high performance liquid chromatography-mass spectrometry,and quantified by external standard method.The Atlantis dC18 column(2.1×150 mm,3μm)was used as the analytical column,and 0.1%formic acid solution and 0.1%formic acid acetonitrile were used as the mobile phase,and the positive electrospray ionization and multiple reactions monitoring was adopted to detect.[Results]The linear relationship of seven kinds of target compound was well in selected concentration range,and correlation coefficient(r 2)was more than 0.99.The limit of quantification(LOQ)of the method was 0.5μg/kg-10μg/kg,and the recovery of standard addition of three adding levels were 65.10%-101.12%,and the relative standard deviations was 0.65%-5.39%(n=7).[Conclusion]The method had simple pretreatment,and high sensitivity and good repeatability,and it could be used for the quantitative determination of seven kinds of penicillin in pork sample.

关 键 词：液质联用仪 猪肉 青霉素 

分 类 号：R28[医药卫生—中药学]