Rodríguez-Gómez R, Jiménez-Díaz I, Zafra-Gómez A, Ballesteros O, Navalón A
Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, University of Granada, Campus of Fuentenueva, E-18071 Granada, Spain.
Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, University of Granada, Campus of Fuentenueva, E-18071 Granada, Spain.
Talanta. 2014 Dec;130:561-70. doi: 10.1016/j.talanta.2014.07.047. Epub 2014 Jul 26.
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.
近几十年来，与工业发展并行出现了大量能够扰乱人体内分泌系统的新型化学物质。这类物质，即所谓的内分泌干扰化学物质（EDCs），包括许多化合物家族，如对羟基苯甲酸酯、二苯甲酮类紫外线过滤剂和双酚类。鉴于这些化合物已证实的生物活性，有必要开发新的分析程序来评估暴露情况，最终目标是以准确的方式确定EDCs浓度与人群中观察到的有害健康影响之间的关系。在本研究中，提出并验证了一种基于简化样品处理的方法，该方法包括沉淀、蒸发以及用C18对提取物进行净化等步骤，随后采用超高效液相色谱 - 串联质谱（UHPLC-MS/MS）分析来测定人母乳样品中的双酚A及其氯化衍生物（单氯、二氯、三氯和四氯双酚A）、对羟基苯甲酸酯（甲基、乙基、丙基和丁基对羟基苯甲酸酯）以及二苯甲酮类紫外线过滤剂（二苯甲酮 -1、-2、-3、-6、-8和4-羟基二苯甲酮）。所发现的检测限范围为0.02至0.05 ng mL⁻¹。该方法采用基质匹配标准校准进行验证，随后对加标样品进行回收率测定。所有化合物的回收率范围为91%至110%，精密度（以相对标准偏差评估）低于15%，均在所选生物分析方法验证指南的可接受范围内。该方法成功应用于从10名随机选择的女性收集的人母乳样品中这些化合物的测定。
