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在线单滴液-液-液微萃取与毛细管电泳联用:一种用于样品净化和浓缩的简单高效方法,用于测定实际基质中的痕量分析物。

On-line combination of single-drop liquid-liquid-liquid microextraction with capillary electrophoresis for sample cleanup and preconcentration: a simple and efficient approach to determining trace analyte in real matrices.

机构信息

National Key Laboratory of Applied Organic Chemistry, Lanzhou University, South Tianshui Road #222, Gansu, Lanzhou, China.

出版信息

J Chromatogr A. 2010 Mar 12;1217(11):1856-61. doi: 10.1016/j.chroma.2010.01.013. Epub 2010 Jan 14.

Abstract

In order to improve the sensitivity of capillary electrophoresis (CE) and overcome the deficiency of commercial CE instruments in handling complex matrices directly, we proposed a novel technique which combined single-drop liquid-liquid-liquid microextraction (SD-LLLME) with CE on-line. In this technique, SD-LLLME was realized using a commercial CE instrument and, to further concentrate the target analyte, large-volume sample stacking combined sweeping without polarity switching was utilized. Even though without agitating the donor phase in the extraction process, the model compound, adenine was enriched 550-fold in only 10 min. The enrichment factors were 760 and 1030 when the extraction time was extended to 30 and 60 min, respectively. The relative standard deviations (RSDs) of adenine were 5.24% and 2.29% for peak area and migration time, respectively, which indicated that this method was much more reproducible compared to the existing methods that combined sample-preparation strategies with CE. In addition, this approach was selective while cleaning up target analyte. These mentioned advantages allowed the developed method to be an attractive approach to determining trace target compounds in complex real samples.

摘要

为了提高毛细管电泳(CE)的灵敏度,并克服商业 CE 仪器在直接处理复杂基质方面的不足,我们提出了一种将单滴液-液-液微萃取(SD-LLLME)与 CE 在线联用的新技术。在该技术中,SD-LLLME 是利用商业 CE 仪器实现的,为了进一步浓缩目标分析物,采用了大体积样品堆积结合无极性切换的扫集。即使在萃取过程中不搅拌供体相,在 10 分钟内,模型化合物腺嘌呤也被富集了 550 倍。当萃取时间延长至 30 和 60 分钟时,富集因子分别为 760 和 1030。腺嘌呤的相对标准偏差(RSD)分别为峰面积和迁移时间的 5.24%和 2.29%,这表明与结合样品制备策略与 CE 的现有方法相比,该方法具有更高的重现性。此外,该方法在净化目标分析物时具有选择性。这些优点使得所开发的方法成为一种有吸引力的方法,可用于测定复杂实际样品中的痕量目标化合物。

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