急性瘦肉精中毒检材的QuEChERS净化-液质联用快速确证方法

目前液相色谱串联质谱法测定动物源性食品中瘦肉精普遍采用酶水解提取、固相萃取净化的方式处理样品,该方法耗时长、分析成本高。本研究采用酸水解和酶水解两种提取方式结合QuEChERS(Quick,Easy,Cheap,Effective,Rugged,Safe)净化和高效液相色谱串联质谱建立了动物性食品中特布他林、沙丁胺醇、莱克多巴胺和克伦特罗4种β2受体激动剂的快速定性确证和定量检测方法。采用酶水解提取-QuEChERS净化处理样品,在电喷雾离子源正离子扫描(ESI+)和多反应监测(MRM)模式下,4种瘦肉精在1.0~ 20.0 μg/L 浓度之间呈线性,线性相关系数均大于0.999,检出限和定量限分别为0.1和0.3 μg/kg,猪肉和牛肉样品中4种化合物的回收率为78.5%~112%,相对标准偏差RSD为2.8%~8.9%。采用酸水解法代替酶水解提取时,尽管对于样品中莱克多巴胺测定结果稍偏低,但样品前处理时间大大缩短。两种提取方法结合使用对于提高瘦肉精引起的食物中毒应急处置效率具有重要意义。

QuEChERS Purification with HPLC-MS/MS for Rapid Confirmation in Acute Clenbuterol Poisoning Case Sample

The pretreatment procedure of enzymatic hydrolysis and extraction coupled with solid phase extraction(SPE) purification is usually employed for the determination of β-agonists by high performance liquid chromatography(HPLC) with tandam mass spetroscopy(MS) in food originated from animals. In this study, a HPLC-MS/MS with QuEChERS(Quick, Easy, Cheap, Effective, Rugged, Safe) purification procedures was developed for the determination of terbutaline, salbutamol, ractopamine and clenbuterol in food of animal origin using both acid hydrolysis extraction method and enzymatic hydrolysis extraction method in food poisoning event caused by clenbuterol and analogs. Using enzymatic hydrolysis extraction with QuEChERS purification and electrospray ionization mass spectrometry in positive mode adopting multiple reaction monitoring(MRM) mode, four analytes were analyzed in the range of 1.0~20.0 μg/L with correlation coefficients(R) higher than 0.999. The limit of detection(LOD) and the limit of quantification(LOQ) was 0.1 μg/kg and 0.3 μg/kg, respectively, and recoveries for 4 β₂-agonists in pork and beef samples ranged from 78.5% to 112% with relative standard deviation(RSD) of 2.8%~8.9%. When acid hydrolysis extraction was used alternatively, the pretreatment time was shortened greatly, but the result for ractopamine was slightly lower than that using the enzymatic hydrolysis extraction procedure. The combined use of two pretreatment procedures will promote the emergency response in real food poisoning case caused by clenbuterol and analogs.