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基于微基质固相分散与气相色谱-质谱联用的改良 Captiva EMR-lipid 方法优化及其在贻贝样品中 9 种双酚类化合物的测定。

Optimization of a modified Captiva EMR-lipid method based on micro-matrix solid-phase dispersion coupled with gas chromatography-mass spectrometry for the determination of nine bisphenols in mussel samples.

机构信息

Instituto Tecnolóxico para o Control Do Medio Mariño de Galicia, INTECMAR, Consellería Do Mar, Xunta de Galicia, Peirao de Vilaxoán s/n, 36611 Vilagarcía de Arousa, Spain.

出版信息

Anal Methods. 2024 Jun 20;16(24):3957-3967. doi: 10.1039/d4ay00738g.

DOI:10.1039/d4ay00738g
PMID:38847157
Abstract

This work describes a reliable, cheap, easy and fast method for analysis of nine bisphenols in mussel samples by gas chromatography-mass spectrometry after trimethylsilylation. The modified method consisted of miniaturized matrix solid phase dispersion (micro-MSPD) in a glass Pasteur pipette using Captiva EMR (enhanced matrix removal)-lipid as the sorbent. Good linearity was obtained in the work range (1-500 μg L) with a correlation coefficient () ≥ 0.998. The method accuracy and precision were determined at two concentration levels. The results show recoveries ranging from 55 to 111%. The precision varied from 1.95 to 11.4% (RSD). The whole quantification limits were between 0.056 and 3.42 μg per kg dry weight. The analytical procedure was applied for the analyses of five mussel samples collected from Galician Rias. The major compound was BPA, and wild mussels from Rías de Ferrol, Vigo and A Coruña had the highest levels. The proposed method is suitable for the analysis of BPA and its analogues in mussel samples.

摘要

本工作描述了一种可靠、廉价、简便、快速的方法,用于在三甲基硅烷化后通过气相色谱-质谱法分析贻贝样品中的九种双酚。改良方法包括使用 Captiva EMR(增强基质去除)-脂质作为吸附剂,在玻璃巴斯德吸管中进行微型基质固相分散(micro-MSPD)。工作范围内(1-500 μg L)获得了良好的线性关系,相关系数()≥0.998。在两个浓度水平下确定了方法的准确性和精密度。结果表明回收率在 55%至 111%之间。精密度变化范围为 1.95%至 11.4%(RSD)。整个定量限在每公斤干重 0.056 至 3.42 微克之间。该分析程序用于分析从加利西亚里亚斯采集的五个贻贝样本。主要化合物是 BPA,来自费罗尔、维哥和拉科鲁尼亚的野生贻贝含量最高。所提出的方法适用于贻贝样品中 BPA 及其类似物的分析。

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