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在采用乙酰化结合顶空-固相微萃取-带电子捕获检测器的气相色谱法测定氯酚过程中表面活性剂的干扰作用。

Interferences of surfactants during determination of chlorophenols by acetylation coupled to headspace-solid phase microextraction-gas chromatography with an electron capture detector.

作者信息

Stoichev Teodor, de Morais Paulo, Basto M Clara P, Vasconcelos M Teresa S D

机构信息

Centro Interdisciplinar de Investigação Marinha e Ambiental (CIIMAR/CIMAR), Universidade do Porto, Rua dos Bragas, 289, 4050-123 Porto, Portugal.

出版信息

J AOAC Int. 2015 Mar-Apr;98(2):524-8. doi: 10.5740/jaoacint.14-126.

Abstract

The micellar extraction (ME) of chlorophenols (CPs) from solid samples is rapid and avoids the use of organic solvents. The cationic surfactant cetyltrimethylammonium bromide (CTAB) is a powerful agent for ME of CPs. However, CTAB will be an important interference when the extracts are subsequently analyzed by direct solid phase microextraction (SPME) without a previous derivatization step. Therefore, CTAB is usually replaced by the nonionic surfactant polyoxyethylene-10-lauryl ether (POLE), which causes less interference but is less efficient in extracting CPs. In order to assess to what extent the derivatization of CPs with headspace (HS) sampling would be able to reduce surfactant interferences, CPs were measured in the presence of CTAB or POLE using acetylation and HS-SPME coupled to GC with an electron capture detector. Experiments were carried out both in water and in a 0.1 g/mL solution of NaCl (salting out agent). Acetylation and HS-SPME strongly decreased the interference of CTAB for CP determination. Therefore, the application of CTAB followed by SPME determination for an efficient ME of CPs from solid samples should be reconsidered since using CTAB with HS-SPME after acetylation proved to be a potential tool for CP determination in those matrixes after method optimization.

摘要

从固体样品中胶束萃取(ME)氯酚(CPs)速度快,且避免使用有机溶剂。阳离子表面活性剂十六烷基三甲基溴化铵(CTAB)是用于CPs胶束萃取的有力试剂。然而,若萃取物随后不经预先衍生化步骤直接通过直接固相微萃取(SPME)进行分析,CTAB将成为重要干扰物。因此,CTAB通常被非离子表面活性剂聚氧乙烯-10-月桂醚(POLE)取代,POLE产生的干扰较小,但萃取CPs的效率较低。为评估顶空(HS)采样对CPs进行衍生化在多大程度上能够减少表面活性剂干扰,在CTAB或POLE存在的情况下,使用乙酰化和HS-SPME结合带有电子捕获检测器的气相色谱法测定CPs。实验在水和0.1 g/mL氯化钠溶液(盐析剂)中均进行。乙酰化和HS-SPME极大地降低了CTAB对CPs测定的干扰。因此,鉴于乙酰化后将CTAB与HS-SPME联用经方法优化后被证明是在那些基质中测定CPs的潜在工具,对于从固体样品中高效胶束萃取CPs后接着进行SPME测定时CTAB的应用应重新考虑。

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