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采用非接触式电导检测的毛细管电泳进行大体积样品堆积,用于快速灵敏测定人尿液和血清中的抗糖尿病药物二甲双胍。

Large volume sample stacking for rapid and sensitive determination of antidiabetic drug metformin in human urine and serum by capillary electrophoresis with contactless conductivity detection.

作者信息

Tůma Petr

机构信息

Institute of Biochemistry, Cell and Molecular Biology, Third Faculty of Medicine, Charles University, Ruská 87, 100 00 Prague 10, Czech Republic.

出版信息

J Chromatogr A. 2014 Jun 6;1345:207-11. doi: 10.1016/j.chroma.2014.04.016. Epub 2014 Apr 13.

Abstract

Two CE methods with contactless conductivity detection have been developed for determining the oral antidiabetic drug metformin in human urine and blood. The determination of metformin is performed on a separation capillary with an effective length of 14 cm, using a maximum voltage of 30 kV and with a small injection of 50-fold diluted urine into the capillary. Under these conditions, the migration time of metformin is 35s and the LOD is 0.3 μM. Large-volume sample stacking was used to determine low metformin levels in serum. The injection of a sample of serum deproteinized with acetonitrile was 10 times greater compared to the injected amount of urine. This enabled reduction of the LOD to 0.03 μM and the metformin migration time equalled 86 s. The undesirable solvent from sample zone was forced out of the capillary to ensure rapidity and good repeatability of the determination. The RSD values for the migration time are 0.1% for urine and 0.7% for serum; RSD for the peak areas equalled 1.4% for urine and 2.6% for serum. The developed CE technique was tested on performance of routine analyses of metformin in the urine and serum of patients suffering from type II diabetes mellitus.

摘要

已开发出两种采用非接触式电导检测的毛细管电泳(CE)方法,用于测定人尿液和血液中的口服抗糖尿病药物二甲双胍。在有效长度为14 cm的分离毛细管上测定二甲双胍,使用的最大电压为30 kV,将50倍稀释的尿液少量进样到毛细管中。在这些条件下,二甲双胍的迁移时间为35 s,检测限为0.3 μM。采用大体积样品堆积法测定血清中低水平的二甲双胍。用乙腈脱蛋白的血清样品进样量比尿液进样量高10倍。这使得检测限降低到0.03 μM,二甲双胍的迁移时间为86 s。将样品区的不良溶剂从毛细管中驱出,以确保测定的快速性和良好的重复性。尿液迁移时间的相对标准偏差(RSD)值为0.1%,血清为0.7%;尿液峰面积的RSD为1.4%,血清为2.6%。所开发的CE技术在II型糖尿病患者尿液和血清中二甲双胍的常规分析性能上进行了测试。

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