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

摘要

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. (C) 2013 Elsevier B.V. All rights reserved.