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采用液相色谱-电喷雾串联质谱法同时测定环境水样和固体样品中的七种双酚。

Simultaneous determination of seven bisphenols in environmental water and solid samples by liquid chromatography-electrospray tandem mass spectrometry.

机构信息

Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning, Beijing Research Center for Preventive Medicine, Beijing 100013, China.

Key Laboratory of Food Safety Risk Assessment, Ministry of Health and China National Center for Food Safety and Risk Assessment, Beijing 100021, China.

出版信息

J Chromatogr A. 2014 Feb 7;1328:26-34. doi: 10.1016/j.chroma.2013.12.074. Epub 2013 Dec 30.

Abstract

This article presents a simple and universal analytical method for the simultaneous analysis of bisphenol S (BPS), bisphenol F (BPF), bisphenol A (BPA), bisphenol B (BPB), bisphenol AF (BPAF), tetrachlorobisphenol A (TCBPA), and tetrabromobisphenol A (TBBPA) in environmental water (river water, sewage) and solid samples (sediment, sludge) based on liquid chromatography-electrospray tandem mass spectrometry (LC-MS/MS). Analytes were extracted from water samples using hydrophilic lipophilic balanced (HLB) solid-phase extraction (SPE) cartridges, and the extracts were further purified using MAX SPE cartridges. For the solid samples, a combination of ultrasonic extraction with the same SPE clean-up procedures used for the water samples was employed. The absolute recoveries for all analytes in the water and solid samples ranged from 57.1 to 114.3%. Good method reproducibility was achieved in terms of intra- and inter-day precision, yielding relative standard deviations (RSDs) less than 16.9 and 18.1%, respectively. The method limits of quantitation (MLOQ) for the seven compounds in environmental water and solid samples ranged from 0.05 to 4.35ng/L and from 0.06 to 2.83ng/g (dry weight, d.w.), respectively. Finally, this method was successfully applied to real environmental sample analysis, which revealed that all of the tested BPs were present, with the exception of BPB.

摘要

本文提出了一种基于液相色谱-电喷雾串联质谱(LC-MS/MS)的同时分析环境水样(河水、污水)和固体样品(沉积物、污泥)中双酚 S(BPS)、双酚 F(BPF)、双酚 A(BPA)、双酚 B(BPB)、双酚 AF(BPAF)、四氯双酚 A(TCBPA)和四溴双酚 A(TBBPA)的简单通用分析方法。采用亲水亲脂平衡(HLB)固相萃取(SPE)小柱从水样中提取分析物,并用 MAX SPE 小柱进一步纯化提取物。对于固体样品,采用超声提取与水样相同的 SPE 净化程序相结合的方法。所有分析物在水和固体样品中的绝对回收率范围为 57.1%至 114.3%。该方法在日内和日间精密度方面具有良好的重现性,相对标准偏差(RSD)分别小于 16.9%和 18.1%。该方法在环境水样和固体样品中的七种化合物的定量限(MLOQ)范围分别为 0.05 至 4.35ng/L 和 0.06 至 2.83ng/g(干重,d.w.)。最后,该方法成功应用于实际环境样品分析,结果表明除 BPB 外,所有测试的 BPs 均存在。

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