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采用电化学检测的液相色谱法测定血清中的西沙必利。

Liquid chromatographic method with electrochemical detection for determination of cisapride in serum.

作者信息

de Condado M C, Malave A, Dorantes-Hernandez M A, Rathinavelu A

机构信息

Central University of Venezuela, College of Pharmacy, Caracas.

出版信息

J AOAC Int. 2001 Jan-Feb;84(1):9-12.

PMID:11234857
Abstract

A sensitive liquid chromatographic (LC) method using electrochemical detection was developed for the identification and quantitation of cisapride in serum. The serum samples were deproteinized by a simple acetonitrile precipitation technique followed by n-hexane extraction. Cisapride in the deproteinized serum was separated by an isocratic elution with an ODS Hypersil LC column (150 x 4.6 mm) using a mobile phase consisting of 0.05M Na2HPO4-acetonitrile (60 + 40), pH 8.4. Cisapride eluted from the column was detected by a Coulochem II electrochemical detector. The precision of this assay method was determined by intra- and inter-day analyses of cisapride-free fetal bovine serum samples that were spiked with 25, 50, and 100 ng/mL cisapride. For the intra-day assay, recoveries were 94.3 +/- 1.4, 90.1 +/- 2.9, and 103.2 +/- 9.2%, respectively. This electrochemical detection LC method could be very useful in monitoring plasma levels of cisapride.

摘要

建立了一种采用电化学检测的灵敏液相色谱(LC)方法,用于血清中西沙必利的鉴定和定量。血清样品通过简单的乙腈沉淀技术进行脱蛋白处理,然后用正己烷萃取。采用ODS Hypersil LC柱(150×4.6 mm),以0.05M磷酸氢二钠-乙腈(60 + 40)、pH 8.4的流动相进行等度洗脱,分离脱蛋白血清中的西沙必利。用库仑电化学检测器检测从柱中洗脱的西沙必利。通过对添加了25、50和100 ng/mL西沙必利的无西沙必利胎牛血清样品进行日内和日间分析,确定了该测定方法的精密度。对于日内测定,回收率分别为94.3±1.4%、90.1±2.9%和103.2±9.2%。这种电化学检测LC方法在监测西沙必利的血浆水平方面可能非常有用。

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