LC-ToF-MS和LC-QqQ-MS测定动物肌肉组织中的青霉素

通过对前处理步骤的优化,建立了动物肌肉组织中青霉素的多组分残留检测方法.采用固相萃取富集净化提取液,吹氮浓缩后上机测试,利用高效液相色谱分离目标物,比较了飞行时间质谱(ToF-MS)和三重四极杆串联质谱(QqQ-MS)测定青霉素方法的精密度、回收率和检出限.结果表明,飞行时间质谱在检出限、精密度和回收率等方面均不如串联质谱的检测效果好.采用串联质谱对肌肉样品进行分析,实际样品加标回收率达75%以上(除阿莫西林外),精密度高,检出限低于欧盟规定的最大残留限值(MRL),该方法适合于肌肉样品中青霉素的测定.

Determination of penicillins in animal muscle tissues using LC-ToF-MS and LC-QqQ-MS

A multi-residue analytical method was developed for the simultaneous determination of penicillins in animal muscle tissues by the optimization of the pre-treatment processes.Solid phase extraction was used for the pre-concentration and cleaning of the samples,which was detected after blowing by nitrogen gas.Liquid chromatography was used for target compounds separation,then time-of-flight mass was compared with tandem mass spectrometry for detection of penicillins on analysis parameters,such as selectivity,detection limit and precision.The results showed that time-of-flight mass method was no better than tandam mass in parameters of selectivity,detection limit and precision of penicillins detection.Tendam mass was used for real muscles detection,the recoveris of penicillins were more than 75%(except amoxicillin),and the precision was high and the detection limit was lower than the maxiam residue limit(MRL) of European Union.The method was proved to be suitable for penicillins detection in muscle tissues.