超高效液相色谱——串联质谱同时测定猪肉中传统型和新型瘦肉精

建立一种超高效液相色谱—串联质谱同时测定猪肉中传统型和新型“瘦肉精”(克伦特罗、沙丁胺醇、莱克多巴胺、特布他林、异丙喘宁、氯丙那林、西马特罗、非诺特罗和喹乙醇及其代谢物)的分析方法。结果显示,在0.2~20.0μg/L范围内各化合物有良好的线性关系,相关系数>0.9962。非诺特罗、莱克多巴胺和氯丙那林的检出限和定量限分别为0.1,0.3μg/kg;克伦特罗的检出限和定量限分别为0.05,0.2μg/kg,其他化合物的检出限和定量限分别为0.2,0.5μg/kg。在3个添加水平下,各目标化合物的回收率为89.1%~121.5%,相对标准偏差为2.6%~12.9%(n=6)。该检测方法快速、准确、灵敏度高,适用于猪肉等动物源性食品中传统型和新型“瘦肉精”残留的测定和确证。

Simultaneous determination of traditional and new types of "lean meat powder" in pork by ultra performance liquid chromatography-tandem mass spectrometry

An analytical method for the simultaneous determination of new and traditional "lean meat powder"(Clenbuterol, Salbutamol, Ractopamine, Terbutaline, Isoprophane, Chlorpheniramine, Simmatrol, Fenoterol and Olaquindox and its metabolites) in pork by ultra performance liquid chromatography-tandem mass spectrometry was established. Pork samples were extracted with 2% formic acid-acetonitrile solution. The extracts were purified by neutral alumina column. After being dried and concentrated by nitrogen, the hexane was degreased and determined by ultra performance liquid chromatography-tandem mass spectrometry and quantified by internal standard method. Waters HSS C 18 column (100 mm×2.1 mm, particle size 1.8 μm) was used. The mobile phase was separated by acetonitrile and 0.1% formic acid aqueous solution. The electrospray ionization mode was used to determine the multi-reaction monitoring mode. The test can be completed in 7 minutes. The results showed that there was a good linear relationship between the compounds in the range of 0.2~20 μg/L, and the correlation coefficient was greater than 0.996 2. The detection limits and quantitation limits of fenoterol, ractopamine and clorprenaline were 0.1 μg/kg and 0.3 μg/kg;the detection limits and quantitation limits of clenbuterol were 0.05 μg/kg and 0.2 μg/kg, the detection limits and limit of quantitation of other compounds were 0.2 μg/kg and 0.5 μg/kg . At the three levels of addition (detection limit, 2 times limit of detection, 10 times limit of detection), the recovery of each target compound was 89.1% to 121.5%, and the relative standard deviation was 2.6% to 12.9%( n =6). The method is rapid, accurate and sensitive, and is suitable for the determination and confirmation of traditional and new " lean meat powder " residues in animal-derived foods such as pork.