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验证的高效液相色谱法测定人血清中塞来昔布及其在临床药代动力学研究中的应用

Validated HPLC method for the determination of celecoxib in human serum and its application in a clinical pharmacokinetic study.

作者信息

Jayasagar G, Kumar M Krishna, Chandrasekhar K, Prasad P Siva, Rao Y Madhusudan

机构信息

Centre for Bio-Pharmaceutics and Pharmacokinetics, University College of Pharmaceutical Sciences, Kakatiya University, Warangal, Andhra Pradesh, India.

出版信息

Pharmazie. 2002 Sep;57(9):619-21.

PMID:12369449
Abstract

A simple high performance liquid chromatographic method using UV detection for the determination of celecoxib, a specific COX 2 inhibitor, in serum was developed. Serum samples containing the internal standard, tolbutamide, are eluted through a C18, Wakosil column. After extracting with dichloromethane, the eluent is monitored at 250 nm. The mobile phase comprised of 10 mM potassium dihydrogen ortho phosphate (pH 3.2) and acetonitrile (50:50 v/v) with a flow rate of 1 ml/min. Retention times of celecoxib and tolbutamide were 9.6 and 3.5 min, respectively. The mean absolute recovery value was about 70-80%, while the intra day and inter day coefficient of variation and percent error values of the assay method were less than 10%. The calibration curve was linear over a concentration range of 10-1000 ng/ml.

摘要

建立了一种使用紫外检测的简单高效液相色谱法,用于测定血清中特异性COX 2抑制剂塞来昔布。含有内标甲苯磺丁脲的血清样品通过Wakosil C18柱洗脱。用二氯甲烷萃取后,在250 nm处监测洗脱液。流动相由10 mM磷酸二氢钾(pH 3.2)和乙腈(50:50 v/v)组成,流速为1 ml/min。塞来昔布和甲苯磺丁脲的保留时间分别为9.6和3.5分钟。平均绝对回收率约为70-80%,而该测定方法的日内和日间变异系数及误差百分比值均小于10%。校准曲线在10-1000 ng/ml的浓度范围内呈线性。

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