HPLC-MS/MS法测定人体尿液中的α-咔啉杂环胺  

Determination of α-Carboline HAAs in Urine of Smokers and Nonsmokers by HPLC-MS/MS

作　　者：付瑜锋[1] 赵阁[1] 张婷婷[1] 余晶晶[1] 王昇[1] 谢复炜[1] 张巧[2] 

机构地区：[1]中国烟草总公司郑州烟草研究院 [2]郑州大学公共卫生学院

出　　处：《烟草科技》2014年第3期60-65,共6页Tobacco Science & Technology

基　　金：国家科技支撑计划项目"食品中热反应伴生危害物毒理学检测及风险评估关键技术研究"(2012BAK01B03);国家自然科学基金项目"卷烟烟气中主要杂环胺类化合物的体内代谢研究"(21005087)

摘　　要：建立了分析人体尿液中α-咔啉杂环胺的溶剂-固相萃取-液相色谱串联质谱（HPLC-MS/MS）方法,并对58名吸烟者和20名非吸烟者的尿液样品中的2-氨基-9-氢-吡啶并[2,3-b]吲哚（AαC）和2-氨基-3-甲基-9-氢-吡啶并[2,3-b]吲哚（MeAαC）进行了测定.尿液样品依次经盐酸酸解、乙酸乙酯液液萃取、PXC阳离子柱固相萃取净化后,进行HPLC-MS/MS检测.结果表明：①AαC和MeAαC的检测限分别为1.86和3.25 pg/mL,加标回收率91.2％～121.0％,精密度2.72％～7.84％;②AαC的含量在3.11～101.71 pg/mL之间,但所有样品中均未检出MeAαC;③吸烟者尿液中AαC的含量和远高于非吸烟者,且二者存在显著差异（P＜0.001）.该方法适合用于尿液中α-咔啉杂环胺的检测,且AαC可作为烟气暴露的生物标志物.A method for determining the ct-carboline heterocyclic aromatic amines （HAAs） in human urine by tandem solvent-solid phase extraction and HPLC-MS/MS was developed and applied in the detection of 2-amino-9H-pyrido[2,3-b]indole （ActC） and 2-amino-3-methyl-9H-pyrido[2,3-b]indole （MeAαC） in the urine samples of 20 nonsmokers and 58 smokers. The urine samples were hydrolyzed with HC1, extracted with ethyl acetate, purified by PXC cation exchange cartridges, and determined by HPLC-MS/MS. The results showed that： 1） The detection limits of AαC and MeAαC were 1.86 and 3.25 pg/mL, respectively. The recoveries ranged from 91.2% to 121.0% with the precision of 2.72%-7.84%. 2） The contents of AαC detected in samples ranged from 3.11 to 101.71 pg/mL, no MeAαC was detectable. 3） The AaC levels in smokers＇ urine were much higher than those in nonsmokers, the difference was significant in variance analysis （P〈0.001）. This method is suitable for the determination of α-carboline HAAs in human urine, and AαC can be used as a biomarker of tobacco smoke exposure.

关 键 词：α-咔啉杂环胺 吸烟者 尿液 HPLC-MS MS 生物标志物 

分 类 号：TS416[农业科学—烟草工业]