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应用于饮用水中气味化合物测定的搅拌棒吸附萃取法的优化

Optimization of stir bar sorptive extraction applied to the determination of odorous compounds in drinking water.

作者信息

Benanou D, Acobas F, de Roubin M R

机构信息

Anjou Recherche, Analytical Research Department, 1 place de Turenne, F-94417 Saint-Maurice, France.

出版信息

Water Sci Technol. 2004;49(9):161-70.

Abstract

The off-flavour compounds 2-methylisoborneol (MIB), geosmin, 2,4,6-trichloroanisole, 2,3,6-trichloroanisole, 2,3,4-trichloroanisole and 2,4,6-tribromoanisole were analyzed in water samples by Stir Bar Sorptive Extraction (SBSE) followed by on-line thermal desorption (TD)-capillary GC/MS. Quantification was performed using MS in the single ion monitoring mode (SIM) with 2,4,6-trichloroanisol-D5 as internal standard. Quantification limits are 0.1 ng/l to 0.2 ng/l for the haloanisoles, 0.5 ng/l for geosmin and 1 ng/l for MIB. The relative standard deviations at the quantification limit are ranging from 7 to 14.6%. SBSE-recovery was evaluated by spiking real water samples and varied from 87 to 117%. More than twenty samples per day can be analyzed by SBSE-TD-capillary GC-MS. The same technique in combination with olfactometry was used to elucidate unknown odorous compounds in water samples.

摘要

采用搅拌棒吸附萃取(SBSE)结合在线热脱附(TD)-毛细管气相色谱/质谱联用技术,对水样中的异味化合物2-甲基异冰片(MIB)、土臭素、2,4,6-三氯苯甲醚、2,3,6-三氯苯甲醚、2,3,4-三氯苯甲醚和2,4,6-三溴苯甲醚进行分析。以2,4,6-三氯苯甲醚-D5作为内标,采用质谱单离子监测模式(SIM)进行定量分析。卤代苯甲醚的定量限为0.1 ng/L至0.2 ng/L,土臭素为0.5 ng/L,MIB为1 ng/L。定量限处的相对标准偏差为7%至14.6%。通过向实际水样中加标来评估SBSE回收率,回收率在87%至117%之间。每天可通过SBSE-TD-毛细管气相色谱-质谱联用技术分析二十多个样品。相同技术结合嗅觉测定法用于鉴定水样中未知的异味化合物。

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