从血浆中离子对固相萃取西咪替丁并随后通过高效液相色谱法进行分析。

Ion-pair solid-phase extraction of cimetidine from plasma and subsequent analysis by high-performance liquid chromatography.

作者信息

Russel F G, Creemers M C, Tan Y, van Riel P L, Gribnau F W

机构信息

Department of Pharmacology, Faculty of Medical Sciences, University of Nijmegen, Netherlands.

出版信息

J Chromatogr B Biomed Appl. 1994 Nov 4;661(1):173-7. doi: 10.1016/0378-4347(94)00320-3.

DOI:10.1016/0378-4347(94)00320-3

PMID:7866547

Abstract

An improved method is described for the solid-phase extraction of cimetidine from plasma or serum with subsequent analysis by HPLC. New aspects of the method include protein precipitation with metaphosphoric acid (5%, w/v), followed by selective adsorption of cimetidine and the internal standard ranitidine on the surface of a solid-phase phenyl (PH Bond Elut) column, using octanesulfonate as an ion-pairing agent. Separation was achieved on a LiChrosorb RP-18 column with a mobile phase consisting of acetonitrile-0.01 M phosphate buffer pH 3.0 containing 0.005 M octanesulfonate (22:78, v/v). The intra-assay coefficient of variation varied between 0.7 and 4.0%. The procedure provides cleaner and more stable samples and a better recovery (90 +/- 2.3%) and sensitivity (limit of detection 5 ng/ml and limit of quantitation 25 ng/ml) as compared with previous methods.

摘要

本文描述了一种改进的方法，用于从血浆或血清中固相萃取西咪替丁，随后通过高效液相色谱法进行分析。该方法的新特点包括用偏磷酸（5%，w/v）进行蛋白质沉淀，然后使用辛烷磺酸盐作为离子对试剂，将西咪替丁和内标雷尼替丁选择性吸附在固相苯基（PH Bond Elut）柱表面。在LiChrosorb RP - 18柱上进行分离，流动相由乙腈 - 0.01 M磷酸盐缓冲液（pH 3.0）组成，其中含有0.005 M辛烷磺酸盐（22:78，v/v）。批内变异系数在0.7%至4.0%之间。与先前方法相比，该方法提供了更纯净、更稳定的样品，回收率更高（90±2.3%），灵敏度更高（检测限为5 ng/ml，定量限为25 ng/ml）。