A liquid chromatography-tandem mass spectrometry method for the analysis of primary aromatic amines in human urine.
A liquid chromatography-tandem mass spectrometry method for the analysis of primary aromatic amines in human urine.
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DOI：
10.1016/j.jchromb.2021.122888
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发表时间：
2021-08-15
期刊：
影响因子：
--
通讯作者：
Kannan K
中科院分区：
文献类型：
--
作者：
Chinthakindi S;Kannan K
芳香胺广泛用于个人护理产品中，人类接触这类化学物质的情况很普遍。测定人类尿液中痕量芳香胺的生物分析方法很少。本研究建立了液相色谱-串联质谱（LC-MS/MS）法测定人尿中39种伯芳香胺（AAs）、尼古丁和可替宁。41种分析物在超联苯（100 mm x 2.1 mm, 5 μm）柱上进行色谱分离。质谱分析采用电喷雾电离正离子多反应监测（MRM）模式。该方法具有良好的线性动态范围（0.1 ~ 50 ng/mL），相关系数(r)为>0.999。尿液样本（2ml）用10m NaOH在95℃下水解15h，目标分析物用甲基叔丁基醚（MTBE）提取。样品提取物中加入15 μL的0.25M HCl可提高几种目标分析物的回收率。通过对强化品控样品和认证标准参比物质的分析，验证了该方法的有效性。41种QC样品中37种目标分析物的相对回收率（%）在75-114%之间，而其他分析物的相对回收率较低（16-74%）。目标分析物的检出限（LOD）和定量限（LOQ）分别为0.025 ~ 0.20 ng/mL和0.1 ~ 1.0 ng/mL。通过分析三种不同浓度强化尿液QC样品，评估该方法的日内和日内精密度分别<11.7%和<15.9%（以RSD测量）。该方法应用于一般人群和已知吸烟者的尿液样本分析；在所有吸烟者的尿液中发现苯胺、对苯胺、对甲苯胺、邻甲苯胺/间甲苯胺、3-氯苯胺、4-氯苯胺、3,4-二氯苯胺和4,4'-亚甲苯胺的总浓度为0.04至9.16 ng/mL。
Aromatic amines are widely used in personal care products and human exposure to this class of chemicals is widespread. Bioanalytical methods to determine trace levels of aromatic amines in human urine are scarce. In this study, a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed to determine 39 primary aromatic amines (AAs) along with nicotine and cotinine in human urine. Chromatographic separation of the 41 analytes was achieved on an Ultra biphenyl (100 mm x 2.1 mm, 5 μm) column. Mass spectrometry was operated in electrospray ionization positive ion multi-reaction monitoring (MRM) mode. The method exhibited excellent linear dynamic range (0.1-50 ng/mL) with correlation coefficients (r) >0.999 for all analytes. Urine samples (2 mL) were hydrolyzed using 10 M NaOH at 95 0C for 15 h and target analytes were extracted using methyl-tert-butyl ether (MTBE). Addition of 15 μL of 0.25M HCl to the sample extracts improved the recoveries of several target analytes. The method was validated through the analysis of fortified quality control (QC) samples and a certified standard reference material (SRM). Relative recoveries (%) of target analytes fortified in QC samples were in the range of 75-114% for 37 of the 41 analytes while the other analytes exhibited lower recoveries (16-74%). The limits of detection (LOD) and limits of quantification (LOQ) of target analytes were in the range of 0.025-0.20 ng/mL and 0.1-1.0 ng/mL, respectively. Intra-day and inter-day precision of the method assessed through the analysis of fortified urine QC samples at three different concentrations were <11.7% and <15.9% (measured as RSD), respectively. The method was applied in the analysis of urine samples from the general population and known smokers; aniline, para-anisidine, para-toluidine, ortho/meta-toluidine, 3-chloroaniline, 4-chloroaniline, 3,4-dichloroaniline, and 4,4'-methylenedianiline were found in all smoker’s urine at sum concentrations ranging from 0.04 to 9.16 ng/mL.
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6.1
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