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分散液液微萃取结合超高效液相色谱/串联质谱法测定水样中的有机磷酸酯。

Dispersive liquid-liquid microextraction combined with ultrahigh performance liquid chromatography/tandem mass spectrometry for determination of organophosphate esters in aqueous samples.

作者信息

Luo Haiying, Xian Yanping, Guo Xindong, Luo Donghui, Wu Yuluan, Lu Yujing, Yang Bao

机构信息

Guangzhou Quality Supervision and Testing Institute, Guangzhou 510110, China.

School of Chemical Engineering and Light Industry, Guangdong University of Technology, Guangzhou 510110, China.

出版信息

ScientificWorldJournal. 2014 Jan 29;2014:162465. doi: 10.1155/2014/162465. eCollection 2014.

Abstract

A new technique was established to identify eight organophosphate esters (OPEs) in this work. It utilised dispersive liquid-liquid microextraction in combination with ultrahigh performance liquid chromatography/tandem mass spectrometry. The type and volume of extraction solvents, dispersion agent, and amount of NaCl were optimized. The target analytes were detected in the range of 1.0-200 µ g/L with correlation coefficients ranging from 0.9982 to 0.9998, and the detection limits of the analytes were ranged from 0.02 to 0.07 µg/L (S/N = 3). The feasibility of this method was demonstrated by identifying OPEs in aqueous samples that exhibited spiked recoveries, which ranged between 48.7% and 58.3% for triethyl phosphate (TEP) as well as between 85.9% and 113% for the other OPEs. The precision was ranged from 3.2% to 9.3% (n = 6), and the interprecision was ranged from 2.6% to 12.3% (n = 5). Only 2 of the 12 selected samples were tested to be positive for OPEs, and the total concentrations of OPEs in them were 1.1 and 1.6 µg/L, respectively. This method was confirmed to be simple, fast, and accurate for identifying OPEs in aqueous samples.

摘要

在本研究中建立了一种鉴定八种有机磷酸酯(OPEs)的新技术。该技术采用分散液液微萃取结合超高效液相色谱/串联质谱法。对萃取溶剂的类型和体积、分散剂以及氯化钠的用量进行了优化。目标分析物的检测范围为1.0 - 200μg/L,相关系数在0.9982至0.9998之间,分析物的检测限为0.02至0.07μg/L(信噪比=3)。通过对水样中OPEs的加标回收率鉴定证明了该方法的可行性,磷酸三乙酯(TEP)的加标回收率在48.7%至58.3%之间,其他OPEs的加标回收率在85.9%至113%之间。精密度在3.2%至9.3%之间(n = 6),中间精密度在2.6%至12.3%之间(n = 5)。在所选的12个样品中,只有2个检测出OPEs呈阳性,其中OPEs的总浓度分别为1.1和1.6μg/L。该方法被证实对于鉴定水样中的OPEs简单、快速且准确。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/1155/3927578/1af960b21bbb/TSWJ2014-162465.001.jpg

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