液相色谱串接质谱联用快速分析肉食品中克仑特罗对映异构体  

Rapid Analysis of Clenbuterol Enantiomers in Edible Meat by High Performance Liquid Chromatography-tandem Mass Spectrometry

作　　者：王占良[1] 张建丽[1] 赵宇[1] 张亦农[1] 

机构地区：[1]国家体育总局反兴奋剂中心食品药品兴奋剂检测实验室,北京100029

出　　处：《中国运动医学杂志》2015年第12期1186-1191,共6页Chinese Journal of Sports Medicine

摘　　要：目的：建立液相色谱串接质谱联用法快速分析肉食品中克仑特罗对映异构体的方法,分析现有肉食品中克仑特罗对映异构体的比值情况。方法：样品经匀浆处理后,酸化提取,MCX 6cc固相萃取柱纯化,以流动相为10 mmol/L甲酸铵的甲醇为流动相,采用Astec CHIROBIOTICTM T 150 mm×2.1 mm×5μm色谱柱分离,电喷雾离子源,正离子多反应监测模式扫描分析检测,D9-克仑特罗为内标。采用该方法分析了85例含有克仑特罗肉食品中的R-（-）-克仑特罗与S-（＋）-克仑特罗比值和分布情况。结果：R-（-）-克仑特罗和S-（＋）-克仑特罗实现基线分离,方法的检测限为0.1μg/kg,在添加的高、中、低三种浓度的相对回收率分布在81%~111%之间。结论：该方法样品前处理简单、快速、可靠。Objective To analyze the clenbuterol enantiomers in edible meat by high performance liquid chromatography-mass spectrometry （HPLC-MS/MS）. Method The edible meat sample was extracted under acidic condition and purified by MCX Oasis solid prepared extraction column. Using D9-clenbuterol as internal standard,the S-（＋）-clenbuterol and R-（-）-clenbuterol were separated by Astec CHIROBIOTICTMT column （150mm×2.1mm×5μm）and then detected by HPLC-MS/MS . A total of 85 edible meat samples containing clenbuterol were analyzed in this study. The ratios of R-（-）-clenbuterol and S-（＋ ）-clenbuterol were calculated. Results In this study,the limit of detection for clenbuterol was 0.1μg/kg and the relative recovery of target compounds spiked in blank sample at high, moderate, and low concentration ranged from 81.0 to 111.2%. Conclusion The method introduced in this study is a simple,rapid,reliable,and suitable for routine analysis of clenbuterol enantiomers in edible meat.

关 键 词：克仑特罗对映异构体 兴奋剂 肉食品 液相色谱串接质谱联用法(HPLC-MS/MS) 

分 类 号：R155.55[医药卫生—营养与食品卫生学]