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Direct Coupling of Ionic Liquid Based Single-Drop Microextraction and GC/MS

机译:基于离子液体的单滴微萃取与GC / MS的直接耦合

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摘要

The use of ionic liquids as extracting media in single-drop liquid-phase microextraction (SDME) and its direct coupling to gas chromatography/mass spectrometry (GC/MS) is presented. For this purpose, a new removable interface that enables the introduction of the extracted analytes into the GC system, while preventing the ionic liquid from entering the column, has been developed. The determination of three representative pollutants in water samples has been used as a model analytical problem in order to demonstrate the feasibility of the proposed interface. The analytes (dichloromethane, p-xylene, and n-undecane) were coextracted from the aqueous sample in a 2-(mu)L drop of 1-butyl-3-methylimidazolium hexaflourophosphate. Then, the syringe used to perform the SDME was directly introduced into the interface, which was held at 140 deg C in order to achieve a complete volatilization of the target compounds. After the injection, the ionic liquid was retained in the interface, while a carrier gas transferred the volatilized analytes into the GC inlet. The optimization of the operational variables affecting the new interface (temperature, carrier flow rate, sample volume and injection technique) was accomplished. The analytes could be determined with detection limits in the low-nanogram per milliliter concentration range, and the relative standard deviations were between 3.3 and 4.4percent.
机译:介绍了离子液体在单滴液相微萃取(SDME)中作为萃取介质的用途,以及它与气相色谱/质谱(GC / MS)的直接耦合。为此,已经开发了一种新的可移动接口,该接口可将提取的分析物引入气相色谱系统,同时防止离子液体进入色谱柱。为了证明所提出的界面的可行性,已将水样品中三种代表性污染物的测定用作模型分析问题。在2-μL的1-丁基-3-甲基咪唑鎓六氟磷酸盐滴眼液中,从水性样品中共萃取分析物(二氯甲烷,对二甲苯和正十一烷)。然后,将用于执行SDME的注射器直接引入接口,接口保持在140℃,以实现目标化合物的完全挥发。进样后,离子液体保留在界面中,而载气将挥发的分析物转移到GC进样口中。优化了影响新界面的操作变量(温度,载流子流速,样品量和进样技术)。可以在低纳克/毫升浓度范围内确定检测限,并且相对标准偏差在3.3%和4.4%之间。

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