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Determination of bisphenols in beverages by mixed-mode solid-phase extraction and liquid chromatography coupled to tandem mass spectrometry

机译:混合模式固相萃取-液相色谱-串联质谱法测定饮料中双酚

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摘要

Facing growing restrictions on the use of bisphenol A in food contact materials, several bisphenol analogues are coming in use as the main alternatives to replace this chemical in most of its applications. This work reports a simple and robust method based on mixed-mode solid-phase extraction and stable-isotope dilution liquid chromatography‒tandem mass spectrometry for the analysis of bisphenol A and its main analogues ‒ bisphenol S, 4,4'-sulfonylbis(2-methylphenol), bisphenol F, bisphenol E, bisphenol B, bisphenol Z, bisphenol AF, bisphenol AP, tetrabromobisphenol A and bisphenol P ‒ in alcoholic and non-alcoholic beverages. Mixed-mode solid-phase extraction, combining cationic exchange and reversed-phase mechanisms, was optimized to provide a selective extraction and purification of the target analytes. Derivatization of bisphenols with pyridine-3-sulfonyl chloride allowed increased their ionization efficiency by electrospray ionization. Validation of the proposed method was performed in terms of selectivity, matrix effects, linearity, precision, measurement uncertainty, trueness and limits of detection. Satisfactory repeatability and intermediate precision were obtained; the related relative standard deviations were ≤8.6 % and ≤12 %, respectively. The relative expanded uncertainty (k=2) was below 20 % for all bisphenol analogues and the trueness of the method was demonstrated by spike recovery experiments. Limits of detection ranged from 1.26 ng L-1 to 27.9 ng L-1 for all compounds. Eventually, several canned and non-canned popular beverages were analyzed to demonstrate the applicability of the method.
机译:面对在食品接触材料中使用双酚A的日益严格的限制,几种双酚类似物被用作在大多数应用中替代该化学品的主要替代品。这项工作报告了一种基于混合模式固相萃取和稳定同位素稀释液相色谱-串联质谱的简单而稳定的方法,用于分析双酚A及其主要类似物‒双酚S,4,4'-磺酰基双(2 -甲基苯酚),双酚F,双酚E,双酚B,双酚Z,双酚AF,双酚AP,四溴双酚A和双酚P ‒在酒精和非酒精饮料中的使用。优化了混合模式固相萃取,结合了阳离子交换和反相机制,可以选择性地萃取和纯化目标分析物。用吡啶-3-磺酰氯将双酚衍生化,可以通过电喷雾电离提高其电离效率。在选择性,基质效应,线性,精度,测量不确定度,真实性和检测限方面对提出的方法进行了验证。获得令人满意的重复性和中间精度;相关的相对标准偏差分别为≤8.6%和≤12%。所有双酚类似物的相对扩展不确定度(k = 2)均低于20%,并且该方法的真实性已通过加标回收实验证明。所有化合物的检出限为1.26 ng L-1至27.9 ng L-1。最终,对几种罐装和非罐装的流行饮料进行了分析,以证明该方法的适用性。

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