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超声辅助提取-气相色谱-质谱法测定土壤中环硅氧烷和线型硅氧烷。

Determination of cyclic and linear siloxanes in soil samples by ultrasonic-assisted extraction and gas chromatography-mass spectrometry.

机构信息

Departamento de Medio Ambiente, INIA, Ctra de la Coruña, Km 7, 28040 Madrid, Spain.

出版信息

J Chromatogr A. 2010 Nov 5;1217(45):7024-30. doi: 10.1016/j.chroma.2010.09.031. Epub 2010 Sep 17.

Abstract

A rapid method, based on sonication-assisted extraction in small columns (SAESC) and subsequent quantification and identification by gas chromatography-mass spectrometry (GC-MS), was developed for the determination of cyclic and linear siloxanes in soil. In the experiments with spiked samples (10-50 ng g(-1)), the recovery of cyclic and linear siloxanes ranged from 87.7 to 108.0% and from 84.9 to 107.6%, respectively. The validated method was used to determine the levels of these compounds in various types of soil samples collected from different locations in Spain. The cyclic siloxanes, decamethylcyclopentasiloxane (D5) and dodecamethylcyclohexasiloxane (D6) were detected in all the soil samples analyzed at concentrations from 9.2 to 56.9 ng g(-1) for D5 and from 5.8 to 27.1 ng g(-1) for D6 in agricultural soils and from 22 to 184 ng g(-1) for D5 and from 28 to 483 ng g(-1) for D6 in industrial soils. The total linear siloxanes concentrations (L5-L14) (sum of the 10 congeners) ranged from 191 to 292 ng g(-1) in agricultural soils and from 1411 to 8532 ng g(-1) in industrial soils.

摘要

一种基于超声辅助提取小柱(SAESC)和随后通过气相色谱-质谱(GC-MS)进行定量和鉴定的快速方法被开发用于测定土壤中环和线性硅氧烷。在加标样品(10-50 ng g(-1))的实验中,环状和线性硅氧烷的回收率分别为 87.7-108.0%和 84.9-107.6%。经验证的方法用于测定从西班牙不同地点采集的各种类型土壤样品中这些化合物的水平。在分析的所有土壤样品中均检测到环状硅氧烷,十甲基环戊硅氧烷(D5)和十二甲基环己硅氧烷(D6),其浓度范围为 9.2-56.9 ng g(-1)的 D5 和 5.8-27.1 ng g(-1)的 D6,在农业土壤中;浓度范围为 22-184 ng g(-1)的 D5 和 28-483 ng g(-1)的 D6,在工业土壤中。总线性硅氧烷浓度(L5-L14)(10 种同系物的总和)在农业土壤中为 191-292 ng g(-1),在工业土壤中为 1411-8532 ng g(-1)。

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