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采用亲水作用液相色谱-质谱联用同时测定三种抗惊厥药。

Simultaneous determination of three anticonvulsants using hydrophilic interaction LC-MS.

作者信息

Oertel Reinhard, Arenz Norman, Pietsch Jörg, Kirch Wilhelm

机构信息

Institute of Clinical Pharmacology, Medical Faculty Carl Gustav Carus, Technical University Dresden, Dresden, Germany.

出版信息

J Sep Sci. 2009 Jan;32(2):238-43. doi: 10.1002/jssc.200800461.

DOI:10.1002/jssc.200800461
PMID:19072899
Abstract

A specific and automated method was developed to quantify the anticonvulsants gabapentin, pregabalin and vigabatrin simultaneously in human serum. Samples were prepared with a protein precipitation. The hydrophilic interaction chromatography (HILIC) with a mobile phase gradient was used to divide off ions of the matrix and for separation of the analytes. Four different HILIC-columns and two different column temperatures were tested. The Tosoh-Amid column gave the best results: single small peaks. The anticonvulsants were detected in the multiple reaction monitoring mode (MRM) with ESI-MS-MS. Using a volume of 100 microL biological sample the lowest point of the standard curve, i.e. the lower LOQs were 312 ng/mL. The described HILIC-MS-MS method is suitable for therapeutic drug monitoring and for clinical and pharmcokinetical investigations of the anticonvulsives.

摘要

已开发出一种特定的自动化方法,可同时对人血清中的抗惊厥药物加巴喷丁、普瑞巴林和氨己烯酸进行定量分析。采用蛋白质沉淀法制备样品。使用具有流动相梯度的亲水相互作用色谱法(HILIC)去除基质离子并分离分析物。测试了四种不同的HILIC柱和两种不同的柱温。Tosoh-Amid柱给出了最佳结果:单个小峰。采用电喷雾串联质谱(ESI-MS-MS)的多反应监测模式(MRM)检测抗惊厥药物。使用100微升生物样品时,标准曲线的最低点,即较低的定量下限为312纳克/毫升。所描述的HILIC-MS-MS方法适用于治疗药物监测以及抗惊厥药物的临床和药代动力学研究。

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A sensitive spectrophotometric method for the determination of pregabalin in bulk, pharmaceutical formulations and in human urine samples.一种用于测定原料药、药物制剂及人体尿液样本中普瑞巴林的灵敏分光光度法。
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