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基于溶剂微萃取和 UHPLC-MS/MS 的分析方法的建立与验证,用于测定来自不同植物来源的蜂蜜中的双酚。

Development and validation of an analytical methodology based on solvent microextraction and UHPLC-MS/MS for determining bisphenols in honeys from different botanical origins.

机构信息

Analytical Chemistry Group (TESEA), I. U. CINQUIMA, Faculty of Sciences, University of Valladolid, 47011 Valladolid, Spain.

Analytical Chemistry Group (TESEA), I. U. CINQUIMA, Faculty of Sciences, University of Valladolid, 47011 Valladolid, Spain.

出版信息

Food Chem. 2024 Aug 30;450:139358. doi: 10.1016/j.foodchem.2024.139358. Epub 2024 Apr 15.

DOI:10.1016/j.foodchem.2024.139358
PMID:38631201
Abstract

A new analytical methodology was proposed to determine fourteen bisphenols in honeys from different botanical origins using ultra-high performance liquid chromatography-tandem mass spectrometry. A fast, efficient, environmentally-friendly and simple sample treatment (recoveries between 81% and 116%; matrix effect <20% for all studied compounds except for bisphenol E, F and S) was proposed, which involved a solvent microextraction with acetone and a small volume/amount of 1-hexanol. Chromatographic analysis (< 15 min) was performed in a Kinetex EVO C column under gradient elution mode. The method was validated in terms of selectivity, limits of detection (0.2-1.5 μg/kg) and quantification (0.5-4.7 μg/kg), linearity, matrix effect, trueness, and precision (relative standard deviation <17%). Finally, thirty honey samples were analyzed, revealing the presence of residues of nine bisphenols in some of them. However, quantification was possible only in two cases for bisphenol A, with a concentration of approximately 13 μg/kg.

摘要

提出了一种新的分析方法,用于使用超高效液相色谱-串联质谱法测定来自不同植物来源的蜂蜜中的十四种双酚。提出了一种快速、高效、环保且简单的样品处理方法(回收率在 81%至 116%之间;除双酚 E、F 和 S 外,所有研究化合物的基质效应均<20%),涉及丙酮溶剂微萃取和少量 1-己醇。在 Kinetex EVO C 柱下以梯度洗脱模式进行色谱分析(<15 min)。该方法在选择性、检测限(0.2-1.5μg/kg)和定量限(0.5-4.7μg/kg)、线性、基质效应、准确度和精密度(相对标准偏差<17%)方面进行了验证。最后,分析了 30 个蜂蜜样品,结果表明其中一些样品中存在九种双酚的残留。然而,仅在两种情况下可以对双酚 A 进行定量,浓度约为 13μg/kg。

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