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采用中空纤维-固相微萃取法提取瓶装水中的邻苯二甲酸酯,然后进行闪蒸蒸发气相色谱-火焰离子化检测。

Hollow fiber-solid phase microextraction of phthalate esters from bottled water followed by flash evaporation gas chromatography-flame ionization detection.

机构信息

College of Chemical Engineering, Zhejiang University of Technology, Hangzhou 310014, China.

College of Chemical Engineering, Zhejiang University of Technology, Hangzhou 310014, China.

出版信息

J Chromatogr A. 2020 May 24;1619:460953. doi: 10.1016/j.chroma.2020.460953. Epub 2020 Feb 7.

Abstract

A solid phase microextraction coupled with flash evaporation gas chromatography method was applied to the determination of phthalate esters (PAEs). Polysulfone (PSF) hollow fiber at 1 cm length was employed as extraction element to adsorb PAEs directly. Predominant parameters including stirring velocity, salt concentration, extraction time and extraction temperature were optimized. PSF fiber with absorbed PAEs was put into a small sample cup. The extracted analytes were thermally desorbed at 300 °C in a pyrolyzer, and then entered into a column for separation. The linearity of the method was satisfactory over a concentration range of 2-1000 µg/L with the correlation coefficients r>0.99 for all analytes except dimethoxyethyl phthalate. The relative standard deviations for peak areas were below 9.5% (n = 6). The developed technique achieved high enrichment factors (280-9930 times) and low limits of detection (0.001-0.130 µg/L). The recoveries over the range of 87.0-117.7% were obtained by analyzing real spiked samples. The results demonstrated that this was a simple, environmentally friendly and accurate method for the determination of PAEs in bottled water samples.

摘要

采用固相微萃取结合闪蒸蒸发气相色谱法测定邻苯二甲酸酯(PAEs)。将 1cm 长的聚砜(PSF)中空纤维用作萃取元件,直接吸附 PAEs。优化了主要参数,包括搅拌速度、盐浓度、萃取时间和萃取温度。将吸附有 PAEs 的 PSF 纤维放入小样品杯中。在热解器中,在 300°C 下对提取的分析物进行热解吸,然后进入色谱柱进行分离。该方法在 2-1000µg/L 的浓度范围内具有良好的线性,除二甲氧基乙基邻苯二甲酸酯外,所有分析物的相关系数 r 均大于 0.99。峰面积的相对标准偏差均低于 9.5%(n=6)。该技术实现了高富集因子(280-9930 倍)和低检测限(0.001-0.130µg/L)。通过分析实际加标样品,获得了 87.0-117.7%的回收率。结果表明,该方法简单、环保、准确,适用于测定瓶装水中的 PAEs。

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