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采用 2,3,4,5,6-五氟苯甲溴化衍生化和气相色谱-质谱法同时测定水样中的七种全氟烷酸。

Simultaneous determination of seven perfluoroalkyl carboxylic acids in water samples by 2,3,4,5,6-pentafluorobenzyl bromide derivatization and gas chromatography-mass spectrometry.

机构信息

Hebei Key Laboratory of Applied Chemistry, College of Environmental and Chemical Engineering, Yanshan University, Qinhuangdao, 066004, PR China.

Technology Center of Qinhuangdao Customs, Qinhuangdao, 066004, PR China.

出版信息

Environ Pollut. 2020 Nov;266(Pt 3):115043. doi: 10.1016/j.envpol.2020.115043. Epub 2020 Jun 21.

Abstract

A new derivatization reagent, 2,3,4,5,6-pentafluorobenzyl bromide (PFBBr), was employed to determine seven perfluoroalkyl carboxylic acids (PFCAs) simultaneously in tap water with gas chromatography-mass spectrometry (GC-MS) technique in this study. Firstly, seven PFCAs were derivatized to their corresponding esters under alkaline condition. The derivatization conditions including the amount of PFBBr and KCO, derivatization temperature and time were optimized to increase the derivatization efficiency. The 14 tap water samples collected from different places of China were enriched and purified through solid phase extraction pretreatment. The limits of detection (LODs) and the limits of quantitation (LOQs) ranged from 0.1 ng/L to 0.28 ng/L and from 0.3 ng/L to 0.84 ng/L, respectively. The new method offers a linear relationship in the range from 2 ng/L to 2000 ng/L, and the correlation coefficients ranged from 0.9938 to 0.9994. The results showed that GC-MS combined with pre-column derivatization is a reliable method for the analysis of PFCAs in the aqueous environment.

摘要

本研究采用 2,3,4,5,6-五氟苯甲酰溴(PFBBr)作为衍生化试剂,结合气相色谱-质谱(GC-MS)技术,建立了同时测定自来水中七种全氟羧酸(PFCAs)的分析方法。首先,在碱性条件下,七种 PFCAs 被衍生为相应的酯。优化了衍生化条件,包括 PFBBr 和 KCO 的用量、衍生化温度和时间,以提高衍生化效率。通过固相萃取预处理,对来自中国不同地区的 14 个自来水样品进行了富集和净化。方法的检出限(LODs)和定量限(LOQs)范围分别为 0.10.28ng/L 和 0.30.84ng/L。该方法在 22000ng/L 范围内呈线性关系,相关系数在 0.99380.9994 之间。结果表明,柱前衍生化 GC-MS 是一种可靠的分析水环境中 PFCAs 的方法。

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