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水中全氟辛烷磺酸和全氟辛烷酸的实验室间分析试验:性能与建议。

Inter-laboratory trials for analysis of perfluorooctanesulfonate and perfluorooctanoate in water samples: performance and recommendations.

机构信息

National Institute of Advanced Industrial Science and Technology (AIST), Tsukuba, Ibaraki, Japan.

出版信息

Anal Chim Acta. 2013 Apr 3;770:111-20. doi: 10.1016/j.aca.2013.01.056. Epub 2013 Feb 8.

Abstract

The ISO 25101 (International Organization for Standardization, Geneva) describes a new international standard method for the determination of perfluorooctanesulfonate (PFOS) and perfluorooctanoate (PFOA) in unfiltered samples of drinking and surface waters. The method is based on the extraction of target analytes by solid phase extraction, solvent elution, and determination by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). For the determination of the performance of this method, more than 20 laboratories from 9 different countries participated in an inter-laboratory trial in 2006. In addition, inter-laboratory trials were conducted in 2008 and 2009 for the analysis of perfluoroalkylsubstances (PFASs), including PFOS and PFOA, in water samples by following the protocols of Japanese Industrial Standard (JIS). Overall, the repeatability coefficients of variation (i.e., within-laboratory precision) for PFOS and PFOA in all water samples were between 3 and 11%, showing a adequate precision of the ISO and JIS methods. The reproducibility coefficients of variation (i.e., between-laboratory precision) were found to vary within a range of 7-31% for surface water and 20-40% for wastewater. The recoveries of PFOS and PFOA, as a measure of accuracy, varied from 84 to 100% for surface water and from 84 to 100% for wastewater among the samples with acceptable criteria for internal standards recovery. The determined concentrations of PFASs in samples compared well with the "true" values. The results of the inter-laboratory trial confirmed that the analytical methods are robust and reliable and can be used as a standard method for the analysis of target compounds in water samples.

摘要

ISO 25101(国际标准化组织,日内瓦)描述了一种新的国际标准方法,用于测定饮用水和地表水中未经过滤的样品中的全氟辛烷磺酸(PFOS)和全氟辛酸(PFOA)。该方法基于固相萃取、溶剂洗脱和高效液相色谱-串联质谱(HPLC-MS/MS)测定目标分析物。为了确定该方法的性能,来自 9 个不同国家的 20 多个实验室于 2006 年参加了一项实验室间试验。此外,2008 年和 2009 年还按照日本工业标准(JIS)的协议,对水中的全氟烷基物质(PFASs)(包括 PFOS 和 PFOA)进行了实验室间试验。总体而言,所有水样中 PFOS 和 PFOA 的重复性变异系数(即实验室内部精度)在 3%至 11%之间,表明 ISO 和 JIS 方法具有足够的精度。再现性变异系数(即实验室间精度)在地表水范围内为 7%至 31%,在废水范围内为 20%至 40%。作为准确性的衡量标准,PFOS 和 PFOA 的回收率在地表水样本中为 84%至 100%,在废水样本中为 84%至 100%,这些样本的内标回收率符合可接受标准。与“真实”值相比,样品中 PFASs 的测定浓度相当准确。实验室间试验的结果证实,该分析方法具有稳健性和可靠性,可作为分析水样中目标化合物的标准方法。

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