超高效液相色谱-串联质谱法测定动物尿液中5种镇静剂类药物残留

为建立动物尿液中异丙嗪亚砜、异丙嗪、氯丙嗪、安眠酮和地西泮5种镇静剂类药物残留的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法,本研究以固相萃取为净化手段,采用HPLC-MS/MS检测猪、牛和羊尿液中5种镇静剂类药物的残留量。结果表明,尿液样品经离心,调节pH值,Oasis MCX固相萃取柱净化后,能够有效去除杂质,5种镇静剂在0.6～20.0μg·L^-1范围内呈良好的线性关系,相关系数(R²)均大于0.993;5种镇静剂类药物的检出限和定量限分别为0.1和0.6μg·L^-1,0.6、2.5和9.0μg·L^-1 3个添加水平的回收率介于64.6%～110.2%之间,相对标准偏差(RSD)均小于6.0%。本研究结果为不同动物尿液中镇静剂类兽药残留的精准检测提供了技术支持。

Determination of Five Sedative Drug Residues in Animal Urine by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

The purpose of this study was to establish an ultra-high performance liquid chromatogram-tandem mass spectrometry (UPLC-MS/MS) method for the determination of 5 sedative drug residues including promethazine sulfoxide, promethazine, chlorpromethazine, quaaludes and diazepam in animal urine. After purification by solid phase extraction, UPLC-MS/MS was used to detect residues of 5 sedatives in the urine of pigs, cattle and sheep. The results showed that impurities can be effectively removed after centrifugation, pH adjustment and purification by Oasis MCX SPE column. The five sedatives suggested good linear relationship in the range of 0.6-20 g·L^-1, and the correlation coefficient (R²) was greater than 0.993. Besides, the detection limits and quantitative limits of the 5 sedatives were 0.1 and 0.6 g·L^-1, respectively. The recoveries of the 3 spiked levels at 0.6, 2.5 and 9.0 g·L^-1 ranged from 64.6% to 110.2%, with relative standard deviation (RSD) less than 6.0%. This method can be used for the accurate detection of sedative drug residues in the urine of different animals.