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高效液相色谱法结合紫外吸收检测法测定人血浆中的噻氯匹定

Determination of ticlopidine in human plasma by high-performance liquid chromatography and ultraviolet absorbance detection.

作者信息

Dal Bo L, Verga F, Marzo A, Ambrosoli L, Poli A

机构信息

Laboratory of Pharmacokinetics, I.P.A.S. S.A., Ligornetto, Switzerland.

出版信息

J Chromatogr B Biomed Appl. 1995 Mar 24;665(2):404-9. doi: 10.1016/0378-4347(94)00539-h.

Abstract

A simple HPLC method has been developed for the determination of ticlopidine in human plasma. Plasma samples were buffered at pH 9 and extracted with n-heptane-isoamyl alcohol (98.5:1.5, v/v). Imipramine was used as internal standard. Chromatography was performed isocratically with acetonitrile-methanol-0.05 M KH2PO4 (20:25:55, v/v) at pH 3.0 containing 3% triethylamine at a flow-rate of 1 ml/min. A reversed-phase column, Supelcosil LC-8-DB, 15 cm x 4.6 mm I.D., 5 microns particle size, was used. The effluent was monitored by UV absorbance detection at 235 nm. The method showed good accuracy, precision and linearity in the concentration range 5-1200 ng/ml. The limit of quantitation was 5 ng/ml, with a precision (C.V.) of 8.91%, which is the same as that achieved by other authors with a previously published GC-MS method. The procedure described in this paper is simple and allows the routine assessment of ticlopidine plasma concentration in pharmacokinetic studies following therapeutic doses in human subjects.

摘要

已开发出一种简单的高效液相色谱法用于测定人血浆中的噻氯匹定。血浆样品在pH 9条件下缓冲,并用正庚烷 - 异戊醇(98.5:1.5,v/v)萃取。以丙咪嗪作为内标。采用乙腈 - 甲醇 - 0.05 M磷酸二氢钾(20:25:55,v/v)在pH 3.0且含有3%三乙胺的条件下等度洗脱,流速为1 ml/min进行色谱分析。使用一根反相柱,Supelcosil LC - 8 - DB,15 cm×4.6 mm内径,5微米粒径。通过在235 nm处的紫外吸光度检测监测流出物。该方法在5 - 1200 ng/ml的浓度范围内显示出良好的准确度、精密度和线性。定量限为5 ng/ml,精密度(变异系数)为8.91%,这与其他作者使用先前发表的气相色谱 - 质谱法所获得的结果相同。本文所述方法简单,可用于在人体受试者接受治疗剂量后进行药代动力学研究时对噻氯匹定血浆浓度的常规评估。

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