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目的:建立对肉类食品中9种β-受体激动剂的高效液相色谱-串联质谱测定方法。方法:捣碎的样品用酶水解后,高氯酸提取,经离心后过滤,滤液用HLB和MCX固相萃取柱净化,氮气吹干,流动相溶解,液相色谱-串联质谱仪测定,选用D3-沙丁胺醇、D6-莱克多巴胺、D9-克伦特罗作为内标,峰面积定量。对样品前处理和色谱、质谱条件进行了优化。结果:样品测定的相对标准偏差在0.7%~9.6%,加标回收率在74.9%~106.9%,检出限和定量限分别为0.01μg/kg-0.05μg/kg和0.03μg/kg-0.20μg/kg。结论:方法灵敏度高、定性及定量准确,满足肉类食品中9种β-受体激动剂的测定要求。
Objective: To establish a method for the determination of nine β-agonists in meat by high performance liquid chromatography-tandem mass spectrometry. Methods: The mashed samples were enzymatically hydrolyzed, extracted with perchloric acid, centrifuged and filtered. The filtrate was purified with HLB and MCX SPE cartridges, dried with nitrogen, dissolved in mobile phase and determined by liquid chromatography-tandem mass spectrometry D3-salbutamol, D6-ractopamine, D9-clenbuterol as internal standard, peak area was quantified. Sample preparation and chromatographic, mass spectrometry conditions were optimized. Results: The relative standard deviations (RSDs) were 0.7% ~ 9.6% and the spiked recoveries were 74.9% ~ 106.9%. The limits of detection and limit of quantification were 0.01μg / kg-0.05μg / kg and 0.03μg / kg-0.20 μg / kg. Conclusion: The method is sensitive, qualitative and quantitative, and meets the requirements for the determination of nine β-agonists in meat products.