低共熔溶剂双水相萃取-UPLC法检测吸烟者尿液中杂环胺类化合物

Aqueous Two-phase Extraction Based on Deep Eutectic Solvents Coupled with UPLC for the Analysis of Heterocyclic Aromatic Amines in Urine of Smokers

为评估香烟烟气中杂环胺的暴露水平,建立了一种基于低共熔溶剂/无机盐双水相萃取-UPLC法测定吸烟者尿液中5种杂环胺(IQ,IQ[4,5-b],Harman,Norharman和Phe-P-1)的方法.制备了7种以氯化胆碱(ChCl)为氢键受体的低共熔溶剂,并对其进行了表征;系统考察了影响萃取效率的主要参数,并将该方法与其它方法进行了对比研究.结果表明,在最佳提取条件下,杂环胺(HAAs)的回收率为81.9%~106.2%,日内和日间精密度分别低于2.9%和3.2%,检出限和定量限分别为0.020~0.097 ng/g和0.19~0.39 ng/g.该方法具有操作简单、环境友好及单样品成本低等特点,为尿液中杂环胺的检测提供了一种新方法,在生物样品检测领域具有良好的开发与应用价值.

To assess the exposure to heterocyclic aromatic amines(HAAs)from tobacco smoke,a novel method,an aqueous two-phase system based on deep eutectic solvent(DES-APTS)followed by UPLC,was described to analyze five HAAs(IQ,IQ[4,5-b],Harman,Norharman,Phe-P-1)from the urine samples of smokers.Seven kinds of choline chloride(ChCl)-based DESs had been synthesized and characterized by 1H NMR and FTIR spectra.The significant parameters affecting the extraction efficiency of HAAs in the DES-ATPS procedure were systematically investigated.Under optimal extraction conditions,the recoveries for the target HAAs ranged from 81.9%to 106.2%.The obtained intra-and inter-day relative standard deviations(RSDs)were less than 2.9%and 3.2%,respectively.The detection limits(LODs)and quantification limits(LOQs)were obtained in ranges of 0.020—0.097 ng/g and 0.19—0.39 ng/g,respectively.The developed method of DES-ATPS,with its simplicity,good environment-friendliness and low-cost per sample,could be a promising alternative technique for rapidly extracting and quantifying HAAs from urine samples,and displayed great development potential in the field of the detection in biological samples.