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发展一种改良的单液滴微萃取方法及其在水样中氨基甲酸酯和有机磷农药分析中的应用。

Development of an improved single-drop microextraction method and its application for the analysis of carbamate and organophosphorus pesticides in water samples.

机构信息

Key Laboratory of Pesticide and Chemical Biology, Ministry of Education, College of Chemistry, Central China Normal University, Wuhan 430079, China.

出版信息

Analyst. 2012 Nov 21;137(22):5339-45. doi: 10.1039/c2an35623f. Epub 2012 Sep 27.

Abstract

An improved single-drop microextraction (SDME) method combined with high performance liquid chromatography has been developed for the detection of trace carbamate and organophosphorus pesticides in water samples. The most fascinating feature of the proposed method is the use of an oval-shaped polychloroprene rubber (PCR) tube to load the extraction solvent, which efficiently loads more solvent and improves the stability of extraction microdrop. Furthermore, this device provides a larger contact surface between the extraction solvent and the inner surface of the oval-shaped PCR tube than that between the extraction solvent and the tip of a microsyringe needle in the conventional SDME. It thereby avoids the problem of the drop floating upwards or dislodging from the tip of the microsyringe needle as observed in the traditional SDME. This method is significant for the great improvement it can offer in extraction efficiency. A series of extraction parameters were investigated systematically using carbamate and organophosphorus as the model analytes. Under the optimal conditions, the enrichment factors for analysis were between 117 and 177, and the limits of detection were ≦0.63 μg L(-1) (S/N = 3). The repeatability study was carried out by extracting the spiked water samples. Here the relative standard deviations varied between 4.0 and 5.8% (n = 5). Additionally, the proposed method was successfully applied to the determination of pesticides in real water samples, and good recoveries were obtained from 79% to 112%. The proposed method was demonstrated to hold advantages of low cost, simplicity of operation, and successful application to in real water samples.

摘要

一种改进的单滴微萃取(SDME)方法与高效液相色谱法相结合,用于检测水样中的痕量氨基甲酸酯和有机磷农药。该方法最吸引人的特点是使用椭圆形氯丁橡胶(PCR)管来装载萃取溶剂,这有效地装载了更多的溶剂,并提高了萃取微滴的稳定性。此外,与传统 SDME 中萃取溶剂与微量进样器针尖之间的接触面积相比,该装置在萃取溶剂与椭圆形 PCR 管的内表面之间提供了更大的接触面积。因此,它避免了传统 SDME 中观察到的液滴向上漂浮或从微量进样器针尖上脱落的问题。该方法在提高萃取效率方面具有重要意义。使用氨基甲酸酯和有机磷作为模型分析物,系统地研究了一系列萃取参数。在最佳条件下,分析的富集因子在 117 到 177 之间,检测限为 ≦0.63 μg L(-1)(S/N = 3)。通过提取加标水样进行重复性研究。这里的相对标准偏差在 4.0 到 5.8%(n = 5)之间变化。此外,该方法成功应用于实际水样中农药的测定,回收率在 79%到 112%之间。该方法具有成本低、操作简单、成功应用于实际水样等优点。

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