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采用胶束电动毛细管色谱法测定水中的灭多威

Single-step extraction and cleanup of bisphenol A in soft drinks by hemimicellar magnetic solid phase extraction prior to liquid chromatography/tandem mass spectrometry.

机构信息

Department of Chemistry, Faculty of Sciences, Ferdowsi University of Mashhad, Mashhad, Iran.

出版信息

Anal Chim Acta. 2013 May 17;778:31-7. doi: 10.1016/j.aca.2013.03.025. Epub 2013 Apr 1.

Abstract

Hemimicelles of tetradecanoate chemisorbed onto magnetic nanoparticles (MNPs) are here proposed as a sorbent for the single-step extraction and cleanup of bisphenol A (BPA) in soft drinks. The purpose of this work was to develop a simple, rapid and low-cost sample treatment suitable to assess the human exposure to BPA from this type of high consumption food. The nanoparticles were easily coated by mixing commercially available magnetite of 20-30 nm mean particle diameter with tetradecanoate at 85°C for 30 min. The extraction/cleanup procedure involved stirring the samples (3 mL) with 200mg of tetradecanoate-coated MNPs for 20 min, isolating the sorbent with a Nd-Fe-B magnet and eluting BPA with methanol. The extraction efficiency was not influenced by salt concentrations up to 1M and pH values over the range 4-9. No cleanup of the extracts was needed, and the method proved matrix-independent. The extracts were analyzed by liquid chromatography, electrospray ionization tandem mass spectrometry. Quantitation was performed by internal standard calibration using BPA-(13)C12. The limit of quantitation obtained for the method, 0.03 ng mL(-1), was below the usual range of concentrations reported for BPA in soft drinks (0.1-3.4 ng mL(-1)). The proposed method was successfully applied to the determination of BPA in different samples acquired from various supermarkets in southern Spain; the concentrations found ranged from 0.066 to 1.08 ng mL(-1). Recoveries from samples spiked with 0.33 ng mL(-1) of BPA ranged from 91% to 105% with relative standard deviations from 3% to 8%.

摘要

十四烷酸化学吸附在磁性纳米粒子(MNPs)上的类脂囊泡被提议作为一种吸附剂,用于软饮料中单步提取和净化双酚 A(BPA)。本工作的目的是开发一种简单、快速和低成本的样品处理方法,适用于评估人类从这种高消费食品中接触 BPA 的情况。纳米粒子很容易通过将商业上可用的 20-30nm 平均粒径的磁铁矿与十四烷酸在 85°C 下混合 30 分钟来涂覆。提取/净化程序包括用 200mg 十四烷酸涂覆的 MNPs 搅拌样品(3mL)20min,用 Nd-Fe-B 磁铁分离吸附剂并用甲醇洗脱 BPA。盐浓度高达 1M 和 pH 值在 4-9 范围内对萃取效率没有影响。不需要对提取物进行净化,该方法证明与基质无关。用液相色谱、电喷雾串联质谱法分析提取物。使用 BPA-(13)C12 进行内标校准进行定量。该方法的定量下限为 0.03ng mL(-1),低于软饮料中 BPA 的常用浓度范围(0.1-3.4ng mL(-1))。该方法成功应用于测定西班牙南部不同超市采集的不同样品中的 BPA;发现的浓度范围为 0.066-1.08ng mL(-1)。从 BPA 浓度为 0.33ng mL(-1)的样品中回收的 BPA 回收率在 91%-105%之间,相对标准偏差在 3%-8%之间。

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