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Purge-assisted headspace solid-phase microextraction combined with gas chromatography-mass spectrometry for determination of chlorophenols in aqueous samples

机译:吹扫辅助顶空固相微萃取-气相色谱-质谱法测定水溶液中的氯酚

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摘要

A simple, economical and very effective method is demonstrated for simultaneous determination of 2,4-dichlorophenol, 2,4,6-trichlorophenol, 2,3,4,6-tetrachlorophenol and pentachlorophenol, in aqueous samples, by using purge-assisted headspace solid-phase microextraction (PA/HS-SPME) coupled to gas chromatography-mass spectrometry (CC-MS). In the new method, purging the sample enhances the removal of the trace chlorophenols without derivatization from the matrices to the headspace. Extraction parameters including extraction temperature, purge gas How rate and extraction time were systematically investigated. Under optimal conditions, the relative standard deviations (RSDs) were 4-11% at 50 pg/mL and 5-14% at 5 pg/mL. respectively. The recoveries were in the range of 83-114%. Detection limits were determined at the fg level. These results indicate that PA/HS-SPME provides a significant contribution to highly efficient extraction of semi-volatile CPs. especially for pentachlorophenol, which has the smallest Henry's constant and large octanol-water partitioning coefficient. In addition, the proposed method was successfully applied to the analysis of chlorophenols in landfill leachate. New perspectives are opened for headspace extraction of relatively low vapor pressure compounds in complex matrices. (c) 2008 Elsevier B.V. All rights reserved.
机译:通过吹扫辅助顶空,同时测定了水中样品中的2,4-二氯苯酚,2,4,6-三氯苯酚,2,3,4,6-四氯苯酚和五氯苯酚固相微萃取(PA / HS-SPME)结合气相色谱-质谱(CC-MS)。在新方法中,吹扫样品可提高痕量氯酚的去除率,而无需从基质到顶空衍生化。系统研究了萃取温度,吹扫气的萃取率,萃取时间等萃取参数。在最佳条件下,相对标准偏差(RSD)在50 pg / mL时为4-11%,在5 pg / mL时为5-14%。分别。回收率在83-114%的范围内。检出限在fg级别确定。这些结果表明,PA / HS-SPME为高效提取半挥发性CP做出了重大贡献。特别是对于五氯苯酚,它具有最小的亨利常数和较大的辛醇-水分配系数。此外,该方法已成功地应用于垃圾渗滤液中氯酚的分析。为复杂基质中较低蒸气压化合物的顶空萃取开辟了新的前景。 (c)2008 Elsevier B.V.保留所有权利。

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