超高效液相色谱-串联质谱法测定动物源性食品中甲基睾丸酮残留量

Determination of Methyl Testosterone Residues in Foods of Animal Origin by Using Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

基于降低样品的基质效应、提高回收率和方法效率,建立采用超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)法测定动物源性食品中甲基睾丸酮残留量的方法。分别对样品的提取溶剂和净化方法进行优化,然后用UPLC-MS/MS仪进行测定,外标法定量。结果表明:采用乙腈作为提取溶剂、C_(18)固相萃取柱经甲醇活化后直接上样,且上样量为5 mL时的净化效果最佳。在此条件下,甲基睾丸酮在1~50 ng/mL范围内的线性关系良好,R^2≥0.998,方法检出限为0.3μg/kg,定量限为1.0μg/kg;以甲基睾丸酮的添加量分别为1.0、2.0、10.0、40.0μg/kg的水平进行方法学验证,回收率在70.60%~112.41%之间,相对标准偏差(relative standard deviations,RSD)为4.33%~9.26%。本方法操作简便、成本低、灵敏度高,适用于批量动物源性食品中甲基睾丸酮的残留量检测。

An efficient method for the determination of methyl testosterone residues in foods of animal origin with low matrix effect and high recovery was presented by ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS-MS）. Samples were extracted with acetonitrile, and the extract was cleaned up on a C18 solid phase extraction column （SPE-C18）, concentrated by nitrogen gas blowing, detected by UPLC-MS-MS and quantitated by external standard method. The calibration curve for methyl testosterone exhibited a good linearity with R2 higher than 0.998. The limit of detection （LOD） was 0.3 μg/kg, and the limit of quantification （LOQ） was 1.0 μg/kg. The recoveries of methyl testosterone in spiked samples were in the range of 70.60%–112.41% at spiked levels of 1.0, 2.0, 10.0 and 40.0 μg/kg, with relative standard deviations （RSD） between 4.33% to 9.26%. This method was simple, low-cost, sensitive and suitable for the batch determination of methyl testosterone residues in foods of animal origin.