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大体积进样在线湍流流动固相萃取-液相色谱-多波长紫外检测法直接分析尿液中的8种氯酚

Direct analysis of eight chlorophenols in urine by large volume injection online turbulent flow solid-phase extraction liquid chromatography with multiple wavelength ultraviolet detection.

作者信息

Guo Feng, Liu Qian, Shi Jian-bo, Wei Fu-sheng, Jiang Gui-bin

机构信息

State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, China.

State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, China.

出版信息

Talanta. 2014 Feb;119:396-400. doi: 10.1016/j.talanta.2013.11.006. Epub 2013 Nov 19.

Abstract

A novel method for determining eight chlorophenols (CPs) by large volume injection online turbulent flow solid-phase extraction high performance liquid chromatography in urine samples was developed. An aliquot of 1.0 mL urine sample could be analyzed directly after centrifugation. The analytes were preconcentrated online on a Turboflow C18-P SPE column, eluted in back-flush mode, and then separated on an Acclaim PA2 analytical column. Major parameters such as SPE column type, sample loading flow rate and elution time were optimized in detail. Eight CPs from monochlorophenol to pentacholophenol were measured by multiple-wavelength UV detection at four different wavelengths. The limits of detection (LODs) were between 0.5 and 2 ng/mL. The linearity range was from the limit of quantification to 1000 ng/mL for each compound, with the coefficients of determination (r(2)) ranging from 0.9990 to 0.9996. The reproducibility of intraday and interday relative standard deviations (RSDs) ranged from 0.6% to 4.5% (n=5). The method was successfully applied to analyze eight CPs in urine samples. Good recoveries, ranging from 76.3% to 122.9%, were obtained. This simple, sensitive and accurate method provides an alternative way to rapidly analyze and monitor CPs in urine samples, especially for matters of occupational exposure.

摘要

建立了一种通过大体积进样在线湍流固相萃取高效液相色谱法测定尿液样本中8种氯酚(CPs)的新方法。1.0 mL尿液样本的等分试样经离心后可直接进行分析。分析物在Turboflow C18-P固相萃取柱上进行在线预浓缩,以反冲模式洗脱,然后在Acclaim PA2分析柱上进行分离。详细优化了固相萃取柱类型、进样流速和洗脱时间等主要参数。通过在四个不同波长下的多波长紫外检测测定了从一氯酚到五氯酚的8种氯酚。检测限(LOD)在0.5至2 ng/mL之间。每种化合物的线性范围为定量限至1000 ng/mL,测定系数(r(2))在0.9990至0.9996之间。日内和日间相对标准偏差(RSD)的重现性范围为0.6%至4.5%(n = 5)。该方法成功应用于尿液样本中8种氯酚的分析,回收率良好,范围为76.3%至122.9%。这种简单、灵敏且准确的方法为快速分析和监测尿液样本中的氯酚提供了一种替代方法,尤其适用于职业暴露相关问题。

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