超高效液相色谱-串联高分辨质谱法检测人体尿液中的对苯二胺-醌类新污染物

该文建立了一种基于液液萃取的超高效液相色谱-串联高分辨质谱测定人体尿液中5种新污染物对苯二胺-醌（PPD-Qs）的方法。优化确定了样品前处理条件及色谱、质谱仪器参数，并采用氘代N-（1,3-二甲基丁基）-N’-苯基-对苯二胺醌（6PPD-Q-D5）作为内标进行定量分析。结果表明，该方法在0.01～50 ng/mL范围内线性关系良好，相关系数大于0.999，方法检出限低至2.4～7.5 pg/mL。尿液中5种PPD-Qs的基质效应为81.3%～110%;3种不同浓度水平加标样本的平均回收率为80.5%～114%，日内及日间相对标准偏差（RSD）均不大于11%。将该方法应用于人群队列尿液中5种PPD-Qs的检测，5种PPD-Qs的平均质量浓度为0.04～1.06 ng/mL。该方法操作简单、灵敏度高、重复性好，适用于人体尿液中新污染物PPD-Qs的检测。

A liquid-liquid extraction based ultra-high performance liquid chromatography-high resolution mass spectrometry（UPLC-HRMS） method was developed for the determination of 5 emerging contaminants of p-phenylenediamine quinones（PPD-Qs） in human urine. The process of sample pretreatment and parameters of both chromatography and mass spectrometry were optimized in detail. Using 6PPD-Q-D5 as an internal standard,the method established in this study had a good linear relationship in the range of 0.01-50 ng/mL,whereas the linear correlation coefficients were greater than 0. 999,and the detection limits of the method（LODs） were as low as 2.4-7.5 pg/mL. The matrix effects of the five PPD-Qs in urine samples were detected at 81.3%-110%. The average recoveries were 80.5%-114%,and intra-day and inter-day relative standard deviations（RSDs） were less than 11%. The method was applied to the determination of 5 PPD-Qs in human urine samples,and the mean concentrations of 5 PPD-Qs ranged from 0.04 ng/mL to 1.06 ng/mL. The method in our study has the advantages of simple operation,high sensitivity,and good repeatability,which is suitable for the determination of PPD-Qs in human urine.