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顶空固相微萃取气相色谱-同位素稀释质谱法测定人尿中13种优先多环芳烃

Quantification of 13 priority polycyclic aromatic hydrocarbons in human urine by headspace solid-phase microextraction gas chromatography-isotope dilution mass spectrometry.

作者信息

Campo Laura, Mercadante Rosa, Rossella Federica, Fustinoni Silvia

机构信息

Department of Occupational and Environmental Health, University of Milan and Fondazione IRCCS Ospedale Maggiore Policlinico, Mangiagalli e Regina Elena, Milan, Italy.

出版信息

Anal Chim Acta. 2009 Jan 12;631(2):196-205. doi: 10.1016/j.aca.2008.10.041. Epub 2008 Nov 1.

Abstract

Polycyclic aromatic hydrocarbons (PAHs) are common environmental pollutants in both living and working environments. The aim of this study was the development of a headspace solid-phase microextraction gas chromatography-isotope dilution mass spectrometry (HS-SPME/GC-IDMS) method for the simultaneous quantification of 13 PAHs in urine samples. Different parameters affecting PAHs extraction by HS-SPME were considered and optimized: type/thickness of fiber coatings, extraction temperature/time, desorption temperature/time, ionic strength and sample agitation. The stability of spiked PAHs solutions and of real urine samples stored up to 90 days in containers of different materials was evaluated. In the optimized method, analytes were absorbed for 60min at 80 degrees C in the sample headspace with a 100mum polydimethylsiloxane fiber. The method is very specific, with linear range from the limit of quantification to 8.67 x 10(3)ngL(-1), a within-run precision of <20% and a between-run precision of <20% for 2-, 3- and 4-ring compounds and of <30% for 5-ring compounds, trueness within 20% of the spiked concentration, and limit of quantification in the 2.28-2.28 x 10(1)ngL(-1) range. An application of the proposed method using 15 urine samples from subjects exposed to PAHs at different environmental levels is shown.

摘要

多环芳烃(PAHs)是生活和工作环境中常见的环境污染物。本研究的目的是开发一种顶空固相微萃取气相色谱 - 同位素稀释质谱法(HS - SPME/GC - IDMS),用于同时定量尿液样本中的13种多环芳烃。考虑并优化了影响HS - SPME萃取多环芳烃的不同参数:纤维涂层的类型/厚度、萃取温度/时间、解吸温度/时间、离子强度和样品搅拌。评估了加标多环芳烃溶液和在不同材料容器中储存长达90天的实际尿液样本的稳定性。在优化方法中,使用100μm聚二甲基硅氧烷纤维在80℃下于样品顶空中吸收分析物60分钟。该方法特异性很强,线性范围从定量限到8.67×10³ ngL⁻¹,对于2、3和4环化合物,批内精密度<20%,批间精密度<20%,对于5环化合物批间精密度<30%,真实度在加标浓度的20%以内,定量限在2.28 - 2.28×10¹ ngL⁻¹范围内。展示了所提出方法在15份来自不同环境水平下接触多环芳烃受试者的尿液样本中的应用。

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