药物辅助性犯罪中兽药麻醉剂舒泰的UPLC-MRM-IDA-EPI-MS鉴定

Identification of Veterinary Drug Shutai in Drug-assisted Crime by UPLC-MRM-IDA-EPI-MS

关键词:  多反应监测  增强子离子扫描  唑拉西泮  替来他明

Key words:  multi-reaction monitoring, enhancer ion scanning, Zolazepam, Tiletamine

摘要:

建立了使用UPLC-MRM-IDA-EPI-MS技术同时定性、定量检验唑拉西泮、替来他明的方法并应用于实际案例。血、尿样品经乙腈提取，PRIME-HLB固相萃取小柱净化后，以001%的甲酸1 mM甲酸铵水-乙腈作为液相流动相，经phenomenex Kinetex F5(100×3.0 mm，2.6 μm)色谱柱分离后，选择电喷雾离子源，用多反应监测联合信息依赖性采集与增强子离子扫描(MRM-IDA-EPI-MS)模式采集，外标法定量。结果表明：唑拉西泮和替来他明均在1~100 ng/mL的浓度范围内线性关系良好，相关系数(R2)均大于0.998，低、中、高三水平添加的回收率范围在85%~89%之间，唑拉西泮和替来他明的检出限分别为0.004 ng/mL和0.002 ng/mL，定量限均为0.01 ng/mL，样品批次间精密度均小于4%。该方法灵敏、准确、高效，能够满足法医毒物学日常鉴定要求。

Abstract:

To establish a method to simultaneously qualitatively and quantitatively test zolazepam and tiletamine using UPLC-MRM-IDA-EPI-MS technology and apply it to actual cases，the blood and urine samples were extracted with acetonitrile, purified by PRIME-HLB solid phase extraction cartridge, with 0.01% formic acid 1 mM ammonium formate water-acetonitrile as the liquid mobile phase, and subjected to phenomenex Kinetex F5 (100×3.0 mm, 2.6 μm). After the chromatographic column is separated, the electrospray ion source is selected, and the multi-reaction monitoring combined information-dependent acquisition and enhancer ion scanning (MRM-IDA-EPI-MS) are used for quantification by external standard method. Results showed that both zorazepam and tiletamine have a good linear relationship within the concentration range of 1～100 ng/mL, the correlation coefficient (R2) is greater than 0.998, and the recovery rate of low, medium and high levels is 85%~89%, the detection limits of zolazepam and tiletaminee are 0.004 ng/mL and 0.002 ng/mL, respectively, the quantification limits are both 0.01 ng/mL, and the precision between samples is less than 4%.The method is sensitive, accurate and efficient, and can meet the daily identification requirements of forensic toxicology.