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采用在线填充固相微萃取与气相色谱-质谱联用技术测定水样中的多环芳烃。

Determination of polycyclic aromatic hydrocarbons in water samples using online microextraction by packed sorbent coupled with gas chromatography-mass spectrometry.

机构信息

Key Laboratory of Combinatorial Biosynthesis and Drug Discovery (Wuhan University), Ministry of Education, Wuhan University School of Pharmaceutical Sciences, Wuhan 430071, China.

出版信息

Talanta. 2012 May 30;94:152-7. doi: 10.1016/j.talanta.2012.03.010. Epub 2012 Mar 10.

DOI:10.1016/j.talanta.2012.03.010
PMID:22608428
Abstract

A fully automated microextraction by packed sorbents (MEPS) coupled with large volume injection gas chromatography-mass spectrometry (GC-MS) has been developed for the determination of eight polycyclic aromatic hydrocarbons (PAHs) in environmental water samples. Naphthalene (Nap), pyrene (Pyr), anthracene, acenaphthylene, phenanthrene, fluoranthene (Flr), fluorene and acenaphthene were the PAHs studied. The performance of the microextraction-GC-MS protocol was compared with solid phase extraction (SPE) and GC-MS analysis. Under optimized experimental conditions, the methods were linear for all analytes in the following ranges: 0.05-2.0 μg L(-1) (MEPS) and 0.25-10.0 μg L(-1) (SPE). The correlation coefficients (R(2)) were in the range 0.9965-0.9997 (MEPS) and 0.9978-0.9998 (SPE) for all the analytes. Limits of detection (LODs) for 2 mL samples (MEPS) ranged from 0.8 ng L(-1) to 8.2 ng L(-1). LODs for 50 mL samples (SPE) were between 4.8 ng L(-1) and 35.9 ng L(-1). The two methods were successfully applied to the determination of the 8 PAHs in environmental waters, with recoveries in the range of 70-117% (MEPS) and 72-134% (SPE) for a real spiked sample. The two sample preparation processes showed good repeatabilities with intra-day relative standard deviations below 14.0% (MEPS) and 14.6% (SPE). Nap, Flr and Pyr were found in a river water sample.

摘要

已开发出一种完全自动化的填充吸附剂微萃取(MEPS)与大体积进样气相色谱-质谱联用(GC-MS),用于测定环境水样中的 8 种多环芳烃(PAHs)。萘(Nap)、芘(Pyr)、蒽、苊烯、菲、荧蒽(Flr)、芴和苊是研究的多环芳烃。比较了微萃取-GC-MS 方案与固相萃取(SPE)和 GC-MS 分析的性能。在优化的实验条件下,该方法对所有分析物均呈线性,范围为 0.05-2.0 μg L(-1)(MEPS)和 0.25-10.0 μg L(-1)(SPE)。所有分析物的相关系数(R(2))在 0.9965-0.9997(MEPS)和 0.9978-0.9998(SPE)之间。2 mL 样品(MEPS)的检出限(LOD)范围为 0.8 ng L(-1)至 8.2 ng L(-1)。50 mL 样品(SPE)的 LOD 为 4.8 ng L(-1)至 35.9 ng L(-1)。这两种方法成功应用于环境水中 8 种 PAHs 的测定,实际加标样品的回收率在 70-117%(MEPS)和 72-134%(SPE)之间。两种样品制备过程具有良好的重复性,日内相对标准偏差低于 14.0%(MEPS)和 14.6%(SPE)。在河水水样中发现了 Nap、Flr 和 Pyr。

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