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首页> 外文期刊>Talanta: The International Journal of Pure and Applied Analytical Chemistry >Validated method for the determination of perfluorinated compounds in placental tissue samples based on a simple extraction procedure followed by ultra-high performance liquid chromatography tandem mass spectrometry analysis
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Validated method for the determination of perfluorinated compounds in placental tissue samples based on a simple extraction procedure followed by ultra-high performance liquid chromatography tandem mass spectrometry analysis

机译:经过简单的提取步骤然后进行超高效液相色谱串联质谱分析的胎盘组织样品中全氟化合物的验证方法

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摘要

Xenobiotic exposure during pregnancy is inevitable. Determination of perfluorinated compounds (PFCs), chemicals described as environmental contaminants by Public Health Authorities due to their persistence, bioaccumulation and toxicity, is a challenge. In the present work, a method based on a simplified sample treatment involving freeze-drying, solvent extraction and dispersive clean-up of the extracts using C-18 sorbents followed by an ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis was developed and validated for the determination of five per fluorinated carboxylic acids (C-4-C-8) and perfluorooctane sulfonate (PFOS) in placental tissue samples. The most influential parameters affecting the extraction method and clean-up were optimized using Design of Experiments (DOE). The method was validated using matrix-matched calibration. Found limits of detection (LODs) ranged from 0.03 to 2 ng g(-1) and limits of quantification (LOQs) from 0.08 to 6 ng g(-1), while inter- and intra-day variability was under 14% in all cases. Recovery rates for spiked samples ranged from 94% to 113%. The method was satisfactorily applied for the determination of compounds in human placental tissue samples collected at delivery from 25 randomly selected women. (C) 2015 Elsevier B.V. All rights reserved.
机译:怀孕期间异物暴露是不可避免的。全氟化合物(PFCs)的持久性,生物蓄积性和毒性被公共卫生当局确定为环境污染物,是一种挑战。在目前的工作中,一种基于简化样品处理的方法,包括冷冻干燥,溶剂萃取和使用C-18吸附剂对萃取物进行分散净化,然后进行超高效液相色谱-串联质谱分析(UHPLC-MS / MS)分析方法的开发并通过验证,可用于测定胎盘组织样品中的五种全氟化羧酸(C-4-C-8)和全氟辛烷磺酸(PFOS)。使用实验设计(DOE)对影响提取方法和净化的最有影响力的参数进行了优化。该方法已通过矩阵匹配校准进行了验证。发现的检测限(LOD)在0.03至2 ng g(-1)之间,定量限(LOQ)在0.08至6 ng g(-1)之间,而日间和日内变异性均低于14%案件。加标样品的回收率在94%至113%之间。该方法令人满意地用于测定从25位随机选择的妇女分娩时收集的人胎盘组织样品中的化合物。 (C)2015 Elsevier B.V.保留所有权利。

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