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当前位置: 首页 > 文章 > 液相色谱串联质谱法测定猪肉中克伦特罗手性对映体残留量 肉类研究 2015 (5) 22-26
Position: Home > Articles > Determination of Residual Clenbuterol Enantiomers in Pork by Liquid Chromatography with Tandem Mass Spectrometry MEAT RESEARCH 2015 (5) 22-26

液相色谱串联质谱法测定猪肉中克伦特罗手性对映体残留量

作  者：
陈国;刘勇军;吕燕;孙亚米;吴银良
单  位：
宁波市农业科学研究院;中国动物疫病预防控制中心
关键词：
克伦特罗;手性对映体;液相色谱串联质谱法;固相萃取
摘  要：
建立测定猪肉中克伦特罗手性对映异构体残留量的液相色谱串联质谱分析方法。5 g猪肉样品在碱化的条件下用乙酸乙酯提取,提取后用稀盐酸进行反萃取,萃取液过SCX固相萃取小柱,最后用5%氨化甲醇洗脱,洗脱液经氮气吹干后用500μL甲醇(含0.02%的乙酸和0.1%的乙酸铵)定容。采用Astec CHIROBIOTICTM V手性色谱柱,以甲醇∶冰乙酸∶乙酸铵=99.88∶0.02∶0.10(V/V)为流动相进行液相分离,电喷雾正离子(ESI+)模式电离,多反应监测(MRM)模式检测,内标法定量。克伦特罗单一对映体在2.0~200μg/L质量浓度范围内呈良好的线性,线性相关系数均大于0.997 0,猪肉样品中克伦特罗最低检测限和定量限分别为0.10μg/kg和0.25μg/kg。猪肉中克伦特罗手性对映体在0.25~0.75μg/kg范围内的回收率为95.8%~102.1%之间,相对标准偏差均小于5%。
译  名：
Determination of Residual Clenbuterol Enantiomers in Pork by Liquid Chromatography with Tandem Mass Spectrometry
作  者：
CHEN Guo;LIU Yongjun;Lü Yan;SUN Yami;WU Yinliang;The Ningbo Academy of Agricultural Sciences;The Center for Animal Disease Control and Prevention of China;
关键词：
clenbuterol;;enantiomers;;liquid chromatography with tandem mass spectrometry;;solid phase extraction
摘  要：
A method was developed for determining residual clenbuterol enantiomers in pork by liquid chromatography with tandem mass spectrometry. Five grams of samples were extracted with ethyl acetate under basic condition. Then,clenbuterol enantiomers were back-extracted from the extracts using diluted hydrochloric acid. The hydrochloric acid extract was purified by SCX solid phase extraction(SPE) cartridge. The eluent was dried by blowing nitrogen and the residue was dissolved in 500 μL of methanol with 0.02% acetic acid and 0.1% ammonium acetate. The analytes were analyzed by LC-MS/MS on a chiral column(Astec CHIOBIOTICTM V) with a mixture of methanol-acetic acid-ammonium acetate as the mobile phase and quantified by the internal standard calibration curve method. Good linearities were obtained for two enantiomers in the concentration range of 2.0 – 200 μg/L with a correlation coefficient more than 0.997 0. The recoveries for the two enantiomers in pork were 95.8% – 102.1% at the fortified levels of 0.25 – 0.75 μg/L with relative standard deviations less than 5.0%. The limits of detection(LOD) and quantitation(LOQ)were 0.10 and 0.25 μg/L, respectively.

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