提出了超高效液相色谱-四极杆飞行时间质谱法(UHPLC-Q-TOF/MS^E)筛查尿液中150种药物与毒物的方法。尿液样品经液液萃取后,采用ACQUITY UPLC HSS C₁₈色谱柱分离,以不同体积比的含0.1%(体积分数)甲酸的乙腈溶液和5 mmol·L^-1甲酸铵溶液(pH 3.0)的混合液为流动相进行梯度洗脱,电喷雾离子源正离子全扫描模式筛查。根据化合物的保留时间、母离子和碎片离子信息鉴定150种化合物。结果表明,150种化合物中有13组同分异构体,基于不同的保留时间或独特的碎片离子,13组同分异构体中的10组可以成功地彼此区分;尿液中150种化合物的检出限(3S/N)为0.2~25.0 μg·L^-1。68个代表性化合物的绝对基质效应为23.1%~119%,提取回收率为30.8%~115%。方法用于120个实际尿液案例的筛查分析,有10个样品呈阳性。

A method for screening of 150 drugs and toxic compounds in urine by ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOF/MS^E) was proposed. Urine samples were prepared by liquid liquid extraction, then separated on ACQUITY UPLC HSS C₁₈ column, with mixtures of acetonitrile solution containing 0.1% (volume fraction) formic acid and 5 mmol·L^-1 ammonium formate solution (pH 3.0) at different volume ratios as the mobile phase for gradient elution. The positive ion mode of electric spray ionization was applied and full scan mode was used for screening. 150 compounds were identified according to their retention time and the information of parent ions and fragment ions. As shown by the results, there were 13 isomers in 150 compounds, and 10 out of 13 isomers could be successfully distinguished from each other based on different retention time or unique fragment ions. The detection limits (3S/N) for 150 compounds in urine were in the range of 0.2-25.0 μg·L^-1. The absolute matrix effects for 68 representative compounds ranged from 23.1% to 119%, and the extraction recoveries ranged from 30.8% to 115%. This method was used for screening analysis of 120 actual urine cases, and 10 samples were positive.