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在液相色谱-电喷雾串联质谱检测之前,通过基于混合半胶束的固相萃取法测定废水和河水样品中的全氟化合物。

Determination of perfluorinated compounds in wastewater and river water samples by mixed hemimicelle-based solid-phase extraction before liquid chromatography-electrospray tandem mass spectrometry detection.

作者信息

Zhao Xiaoli, Li Jidong, Shi Yali, Cai Yaqi, Mou Shifen, Jiang Guibin

机构信息

The State Key Laboratory of Environmental Chemistry and Ecotoxicology of Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, China.

出版信息

J Chromatogr A. 2007 Jun 22;1154(1-2):52-9. doi: 10.1016/j.chroma.2007.03.093. Epub 2007 Mar 30.

Abstract

A comparative study on the use of cetyltrimethylammonium bromide (CTAB)-coated silica and sodium dodecyl sulphate (SDS)-coated alumina mixed hemimicelles-based solid-phase extraction (SPE) for the pre-concentration of six perfluorinated compounds (PFCs) in environmental water samples was presented. The six analytes heptafluorobutyric acid (HFBA), perfluoroheptanic acid (PFHeA), perfluorooctanic acid (PFOA), perfluorooctanic sulfonic (PFOS), perfluorononanic acid (PFNA) and perfluorodecanic acid (PFDeA) were quantitatively retained on both sorbent materials. The cationic surfactant (CTAB adsorbed onto silica) was more appropriate for SPE of PFCs. The main factors affecting adsolubilization of PFCs including the amount of surfactant, pH of solution, sample loading volume and desorption were investigated and optimized. Concentration factor of 500 were achieved by SPE of 500 mL of several environmental water samples. The method detection limits obtained for HFBA, PFHeA, PFOA, PFOS, PFNA and PFDeA were 0.10, 0.28, 0.07, 0.20, 0.10 and 0.05 ng/L, respectively. The relative standard deviation of recoveries ranged from 2 to 8%, which indicated good method precision.

摘要

本文介绍了一项关于使用十六烷基三甲基溴化铵(CTAB)包覆的二氧化硅和十二烷基硫酸钠(SDS)包覆的氧化铝混合半胶束基固相萃取(SPE)对环境水样中六种全氟化合物(PFCs)进行预富集的比较研究。六种分析物七氟丁酸(HFBA)、全氟庚酸(PFHeA)、全氟辛酸(PFOA)、全氟辛烷磺酸(PFOS)、全氟壬酸(PFNA)和全氟癸酸(PFDeA)在两种吸附剂材料上均能被定量保留。阳离子表面活性剂(CTAB吸附在二氧化硅上)更适合用于PFCs的SPE。研究并优化了影响PFCs增溶吸附的主要因素,包括表面活性剂用量、溶液pH值、样品进样体积和解吸。通过对500 mL几种环境水样进行SPE,实现了500倍的浓缩因子。HFBA、PFHeA、PFOA、PFOS、PFNA和PFDeA的方法检出限分别为0.10、0.28、0.07、0.20、0.10和0.05 ng/L。回收率的相对标准偏差在2%至8%之间,表明该方法具有良好的精密度。

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