超高效液相色谱-串联质谱测定尿样中甲苯二胺  

Determination of Toluene Diamine in Urine by Ultra High Performance Liquid Chromatography Tandem Mass Spectrometry

作　　者：张晓梅 孟祥娟 胡越 荣利 刘晓东 ZHANG Xiaomei;MENG Xiangjuan;HU Yue;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》2024年第4期475-479,共5页Journal of Analytical Science

摘　　要：建立了尿样中2,6-甲苯二胺(2,6-TDA)和2,4-甲苯二胺(2,4-TDA)的超高效液相色谱-串联质谱分析方法。尿样水解后经固相萃取,乙腈洗脱,以Waters HSS T3色谱柱分离,在电喷雾离子源正电离模式(ESI+)、多反应监测(MRM)条件下分析,以外标法定量测定尿样中2,6-TDA和2,4-TDA的含量。结果表明,在0.039~10 ng/mL和0.098~10 ng/mL的范围内2,6-TDA和2,4-TDA的测定线性情况良好,相关系数r>0.999,检出限分别为0.012 ng/mL和0.029 ng/mL;定量限分别为0.039 ng/mL和0.098 ng/mL,样品的加标回收率为94.65%~102.42%,批内和批间精密度分别为1.62%~6.67%和2.85%~4.10%。该方法可用于普通人群和职业接触甲苯二异氰酸酯人群尿样中2,4-TDA和2,6-TDA的监测评估。An ultra high performance liquid chromatography-tandem mass spectrometry method was established for the determination of 2,6-TDA and 2,4-TDA in urine.The urine sample was extracted by solid-phase extraction after hydrolysis,cleaned up with acetonitrile and separated on a Waters HSS T3 chromatography column.The analysis was carried out under positive ionization mode(ESI+)and multiple reaction monitoring(MRM)conditions,and the contents of 2,6-TDA and 2,4-TDA in urine were quantitatively determined by the external standard method.The results showed that the determination of 2,6-TDA and 2,4-TDA in urine achieved good linearity in the range of 0.039-10 ng/mL and 0.098-10 ng/mL,with a correlation coefficient(r)greater than 0.999.The limits of detection and the limits of quantification were 0.012 ng/mL,0.029 ng/mL and 0.039 ng/mL and 0.098 ng/mL,respectively.The recovery in spiked urine ranged from 94.65%to 102.42%.The intra batch and inter batch precisions were 1.62%-6.67%and 2.85%-4.10%,respectively.This method can be used for monitoring and evaluating urinary 2,4-TDA and 2,6-TDA in the general population and occupational exposure to toluene diisocyanate.

关 键 词：尿样 2 6-甲苯二胺 2 4-甲苯二胺 超高效液相-串联质谱 

分 类 号：O657.63[理学—分析化学]