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基于离子液体的顶空微液滴液相微萃取-微滴热解吸-气相色谱分析。

Headspace ionic liquid-based microdrop liquid-phase microextraction followed by microdrop thermal desorption-gas chromatographic analysis.

机构信息

Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore.

出版信息

Talanta. 2010 Apr 15;81(1-2):537-42. doi: 10.1016/j.talanta.2009.12.039. Epub 2010 Jan 7.

Abstract

Headspace microdrop liquid-phase microextraction (LPME) using ionic liquids as extracting solvents, followed by gas chromatography-electron capture detection was successfully developed to determine organochlorine pesticides in soil samples. A feature of the developed procedure is the simple handling of the ionic liquid extract in a normal, unmodified gas chromatograph injection port such that no special provision was needed to ensure that the ionic liquid did not contaminate it. This was achieved by only exposing the ionic liquid extract in the injection port while it was still attached to the syringe needle tip (i.e. mirroring the extraction configuration) to permit volatilization of the analytes, instead of injecting the extract. In this way, the spent ionic liquid could be recovered from the injection port, obviating the need to clean the port. Four 1-butyl-3-methylimidazolium-based ionic liquids were investigated, and 1-butyl-3-methylimidazolium hexafluorophosphate was finally selected as the most suitable extracting solvent. Parameters that affect the extraction and determination of the organochlorine pesticides were studied. Under the optimal conditions, the proposed method produced good linearity over a concentration range of 5-250 ng/g. Limits of detection ranging from 0.25 to 0.5 ng/g were achieved.

摘要

采用离子液体作为萃取溶剂的顶空微滴液相微萃取(LPME),结合气相色谱-电子捕获检测,成功地用于土壤样品中有机氯农药的测定。所开发方法的特点是可以在普通的、未经修饰的气相色谱进样口中简单地处理离子液体萃取物,因此不需要特殊的措施来确保离子液体不会污染它。这是通过仅在进样口暴露离子液体萃取物,同时仍然附着在注射器针尖上(即镜像萃取配置)来实现的,以允许分析物挥发,而不是注射萃取物。这样,用过的离子液体可以从进样口中回收,从而无需清洁进样口。研究了四种基于 1-丁基-3-甲基咪唑的离子液体,最终选择 1-丁基-3-甲基咪唑六氟磷酸盐作为最适合的萃取溶剂。研究了影响有机氯农药萃取和测定的参数。在最佳条件下,该方法在 5-250ng/g 的浓度范围内产生了良好的线性关系。检测限范围为 0.25-0.5ng/g。

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