Analysis of clobazam and its active metabolite norclobazam in plasma and serum using HPLC/DAD

作     者：Akerman, KK 

作者机构：UNIV KUOPIODEPT CLIN CHEMSF-70210 KUOPIOFINLAND 

出 版 物：《SCANDINAVIAN JOURNAL OF CLINICAL & LABORATORY INVESTIGATION》 (斯堪的纳维亚临床与实验研究杂志)

年 卷 期：1996年第56卷第7期

页      面：609-614页

核心收录：

学科分类：1001[医学-基础医学(可授医学、理学学位)] 1010[医学-医学技术（可授医学、理学学位）] 10[医学] 

主　　题：diode array detection clobazam high-performance liquid chromatography (HPLC) norclobazam solid-phase extraction (SPE) therapeutic drug monitoring (TDM) 

摘      要：This report describes a simple reversed-phase high-performance liquid chromatographic (HPLC) method with automated solid-phase extraction (SPE) for analysing clobazam and norclobazam concentrations in human serum or plasma. For the HPLC analysis the samples and standards are prepared with an ASPEC automatic sample preparer using 100-mg Bond-Elut C-18 solid-phase extraction columns. The HPLC method is an isocratic method with a mobile phase of acetonitrile :methanol: 10 mmol l(-1) dipotassium hydrogen phosphate, pH 3.7 (30:2:100), at a flow rate of 1.5 ml min(-1). The benzodiazepines are detected with a diode array detector (DAD) at 240 nm and the peak purity analyses are performed at 210-365 nm. The recovery is over 97% for both analytes, and it is independent of the drug concentration. The intra-assay CVs vary between 0.7 and 2.2% and inter-assay CVs between 3.8 and 4.6% at therapeutic drug concentrations. The detection limit is 15 nmol l(-1). The assay is linear from 30 to 20 000 nmol l(-1) (clobazam) and from 170 to 105 000 nmol l(-1) (norclobazam). This method leads to a very good separation of norclobazam from carbamazepine and phenytoin. None of the anti-epileptic or antidepressant drugs tested interfere with the assay.