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A multiresidue method for the determination of selected endocrine disrupting chemicals in human breast milk based on a simple extraction procedure

机译:一种基于简单提取程序的测定母乳中选定的内分泌干扰物的多残留方法

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In recent decades, in parallel to industrial development, a large amount of new chemicals have emerged that are able to produce disorders in human endocrine system. These groups of substances, so-called endocrine disrupting chemicals (EDCs), include many families of compounds, such as parabens, benzophenone-UV filters and bisphenols. Given the demonstrated biological activity of those compounds, it is necessary to develop new analytical procedures to evaluate the exposure with the final objective of establishing, in an accurate way, relationships between EDCs concentrations and the harmful health effects observed in population. In the present work, a method based on a simplified sample treatment involving steps of precipitation, evaporation and clean-up of the extracts with C18 followed by ultrahigh performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis for the determination of bisphenol A and its chlorinated derivatives (monochloro-, dichloro-, trichloro- and tetrachlorobisphenol A), parabens (methyl-, ethyl-, propyl- and butylparaben) and benzophenone-UV filters (benzophenone -1, - 2, - 3, - 6, - 8 and 4-hydroxybenzophenone) in human breast milk samples is proposed and validated. The limits of detections found ranged from 0.02 to 0.05 ng mL~(-1) The method was validated using matrix-matched standard calibration followed by a recovery assay with spiked samples. Recovery rates ranged from 91% to 110% and the precision (evaluated as relative standard deviation) was lower than 15% for all compounds, being within the acceptable limits for the selected bioanalytical method validation guide. The method was satisfactorily applied for the determination of these compounds in human breast milk samples collected from 10 randomly selected women.
机译:近几十年来,与工业发展并行的是,出现了能够在人类内分泌系统中引起疾病​​的大量新化学物质。这些物质组,即所谓的内分泌干扰化学物质(EDC),包括许多家族的化合物,例如对羟基苯甲酸酯,二苯甲酮-UV过滤剂和双酚。鉴于这些化合物具有证明的生物活性,有必要开发新的分析程序以评估暴露,最终目标是以准确的方式建立EDC浓度与人群中观察到的有害健康影响之间的关系。在当前的工作中,一种基于简化样品处理的方法,包括用C18沉淀,蒸发和纯化提取物,然后进行超高效液相色谱-串联质谱分析(UHPLC-MS / MS),从而测定双酚A及其氯化衍生物(一氯,二氯,三氯和四氯双酚A),对羟基苯甲酸酯类(对羟基苯甲酸甲酯,对羟基苯甲酸乙酯,对羟基苯甲酸丙酯和对羟基苯甲酸丁酯)和二苯甲酮UV过滤器(二苯甲酮-1,-2,-3,-提出并验证了人类母乳样品中的6、8和4-羟基二苯甲酮)。检出限范围为0.02到0.05 ng mL〜(-1)。使用基质匹配的标准校正方法,然后对加标样品进行回收率测定,验证了该方法的有效性。回收率范围从91%到110%,所有化合物的精密度(评估为相对标准偏差)均低于15%,在所选生物分析方法验证指南的可接受范围内。该方法令人满意地用于测定从10名随机选择的妇女那里收集的人母乳样品中的这些化合物。

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