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建立了胶束电动色谱法用于测定器官凝胶中地塞米松、昂丹司琼和阿瑞匹坦这三种止吐药物的浓度。

A validated micellar electrokinetic chromatography method for the quantitation of dexamethasone, ondansetron and aprepitant, antiemetic drugs, in organogel.

机构信息

Univ Lille Nord de France, UDSL, EA 4481, UFR Pharmacie, 59000 Lille, France.

出版信息

J Pharm Biomed Anal. 2013 Dec;86:40-8. doi: 10.1016/j.jpba.2013.07.029. Epub 2013 Jul 31.

DOI:10.1016/j.jpba.2013.07.029
PMID:23978340
Abstract

A micellar electrokinetic chromatography (MEKC) method was developed for the determination of three anti-vomiting drugs (aprepitant, dexamethasone and ondansetron) in pharmaceutical formulations. The method was optimized using a central composite design (CCD). Four main factors (borate buffer concentration, pH, methanol content and sodium dodecyl sulfate concentration) were optimized in order to obtain best resolutions and peak efficiencies in a minimum runtime. The separation was performed in a fused-silica capillary. After optimization, the background electrolyte consisted of a borate buffer (62.5mM, pH 8.75) containing sodium dodecyl sulfate (77.5mM) and methanol (3.75%). Under these conditions, a complete separation of each antiemetic drug and its respective internal standards was achieved in 38min. The method was validated with trueness values from 94.9 to 107.2% and precision results (repeatability and intermediate precision) lower than 5.9%. MEKC-UV was the first method allowing the separation of aprepitant, dexamethasone and ondansetron and was suitable for the quantitation of these three antiemetic drugs in organogel formulations. The rapid sample preparation coupled with an automated separation technique make this method convenient for quality control of extemporaneous magistral ready-to-use formulation.

摘要

建立了一种胶束电动色谱(MEKC)法,用于测定药物制剂中的三种止吐药物(阿瑞匹坦、地塞米松和昂丹司琼)。该方法采用中心复合设计(CCD)进行了优化。为了在最短运行时间内获得最佳分辨率和峰效率,优化了四个主要因素(硼酸盐缓冲液浓度、pH 值、甲醇含量和十二烷基硫酸钠浓度)。分离在熔融石英毛细管中进行。优化后,背景电解质由硼酸盐缓冲液(62.5mM,pH8.75)组成,其中含有十二烷基硫酸钠(77.5mM)和甲醇(3.75%)。在这些条件下,每种止吐药及其各自的内标物在 38min 内完全分离。该方法的准确度值在 94.9%至 107.2%之间,精密度(重复性和中间精密度)结果低于 5.9%。MEKC-UV 是第一种能够分离阿瑞匹坦、地塞米松和昂丹司琼的方法,适用于凝胶制剂中这三种止吐药物的定量分析。快速的样品制备与自动化分离技术相结合,使这种方法便于对临时调配即用型制剂的质量控制。

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