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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 establish a rapid method for the analysis of clenbuterol enantiomers in meat products by liquid chromatography-tandem mass spectrometry (LC-MS / MS), and to analyze the ratio of clenbuterol enantiomers in meat products. Methods: The samples were homogenized, acidified and purified by MCX 6cc solid phase extraction. The mobile phase consisted of 10 mmol / L ammonium formate in methanol and separated on a Astec CHIROBIOTICTM T 150 mm × 2.1 mm × 5 μm column , Electrospray ionization source, positive ion multi-reaction monitoring mode scan analysis and detection, D9-clenbuterol as an internal standard. This method was used to analyze the R - (-) - Clenbuterol and S - (+) - Clenbuterol ratio in 85 patients with clenbuterol. RESULTS: Baseline separation of R - (-) - clenbuterol and S - (+) - clenbuterol was achieved with a limit of detection of 0.1 μg / kg, with the exception of high, medium and low relative concentrations The recovery rates range from 81% to 111%. Conclusion: The method of sample preparation is simple, rapid and reliable.