超高效液相色谱-串联质谱联用快速测定尿样中14种镇静催眠类药物  

Rapid Determination of 14 Sedative Hypnotic Drugs in Urine by Ultra High Performance Liquid Chromatography Tandem Mass Spectrometry

作　　者：张晓梅 胡越 孟祥娟 荣利 刘晓东 ZHANG Xiaomei;HU Yue;MENG Xiangjuan;RONG Li;LIU Xiaodong(The Beijing Prevention and Treatment Hospital of Occupational Disease for Chemical Industry,Central Laboratory,Beijing 100093)

机构地区：[1]北京市化工职业病防治院中心实验室,北京100093

出　　处：《分析科学学报》2023年第6期699-704,共6页Journal of Analytical Science

摘　　要：建立了尿样中14种镇静催眠类药物的超高效液相色谱-串联质谱快速定量分析的方法。将尿样离心,取上清液用流动相稀释后过膜,经Waters BEH C18色谱柱分离,在多反应监测(MRM)模式下,以外标法定量测定14种镇静催眠类药物含量。结果表明,14种目标化合物在5.86~300μg/L或7.74~500μg/L范围内线性关系良好,相关系数r>0.999,方法的检出限为0.18~2.32μg/L,定量限为0.59~7.74μg/L。尿样加标回收率为86.84%~118.6%,批内和批间精密度(RSD)分别为0.56%~3.85%和1.54%~7.93%。该方法简单、快速,准确度和精密度满足定量检测需求,可实现尿样中14种镇静催眠类药物的测定。A rapid quantitative analysis method for determination of 14 sedative and hypnotic drugs in urine by high performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)was established.The urine samples were directly diluted with the mobile phase,separated by Waters BEH C 18 column after passing through the membrane,and analyzed under multiple reaction monitoring(MRM)conditions,the contents of 14 sedative hypnotic drugs in human urine were quantitatively determined by external standard method.The results show that 14 target compounds have good linearity within the range of 5.86-300μg/L or 7.74-500μg/L,the was all greater than 0.999,the detection limit is 0.18-2.32μg/L,and the lower limit of quantification is 0.59-7.74μg/L.The average spiking recovery of urine samples was 86.84%-118.6%,the intra assay and inter assay precision were 0.56%-3.85%and 1.54%-7.93%,respectively.The method is simple and rapid,accurate and precise to meet the needs of quantitative detection,and can realize the determination of 14 sedative and hypnotic drugs in urine.

关 键 词：尿样 镇静催眠类药物 超高效液相-串联质谱 

分 类 号：O657.63[理学—分析化学]