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建立并验证用于测定和定量人血浆中茶苯海明的带紫外检测的反相高效液相色谱法。

Development and validation of RP- HPLC method with UV detection to determine and quantify dimenhydrinate in human plasma.

作者信息

Zeb-Un-Nisa -, Shoaib Muhammad Harris, Ali Syed Imran, Rizvi Mehwish, Ali Huma Ali, Fatima Rasheeda, Khan Maqsood Ahmed, Kashif Sadia Suri

机构信息

Faculty of Pharmacy, Ziauddin University, Karachi, Pakistan.

Department of Pharmaceutics, Faculty of Pharmacy & Pharmaceutical Sciences, University of Karachi, Karachi, Pakistan.

出版信息

Pak J Pharm Sci. 2018 May;31(3(Supplementary)):979-984.

PMID:29731433
Abstract

A simple, sensitive and rigorous method for estimation of dimenhydrinate in human plasma was searched and its validation was carried out. LLE (Liquid-Liquid extraction) of analyte with mixture of Hexane and ethyl acetate (1:1 v/v) was carried out for the preparation of Plasma Samples, Chromatographic elution of dimenhydrinate was conducted in human plasma and mobile phase with C-18 bonda Pack column (10μm; 250 × 4.6), using a mobile phase consisting a solution of ammonium bicarbonate in water and methanol at a flow rate of 0.5ml/minute with UV detection at 229 nm. The resolution of dimenhydrinate was well performed from plasma components. This method was validated and exhibited linearity with concentration range of 6 to 380ng/ml of dimenhydrinate in plasma. The Intra day precision was 89.2 to 96.89% and Inter day precision was 88.6% to 93.26%, the average recovery of dimenhydrinate was 97.02%. The efficacy of extraction was proved by above mentioned results. 2ng/ml and 6ng/ml, were appraised as the LOD and LOQ of dimenhydrinate, stability studies disclosed that dimenhydrinate exhibited stability in Plasma after Freeze & thaw cycles and upon -20°C storage, the method was developed well.

摘要

探索了一种简单、灵敏且严谨的测定人血浆中茶苯海明的方法并进行了验证。采用正己烷和乙酸乙酯(1:1 v/v)混合物对分析物进行液液萃取(LLE)以制备血浆样品,使用C-18键合柱(10μm;250×4.6)在人血浆和流动相中对茶苯海明进行色谱洗脱,流动相由碳酸氢铵水溶液和甲醇组成,流速为0.5ml/分钟,在229nm处进行紫外检测。茶苯海明与血浆成分的分离效果良好。该方法经过验证,在血浆中茶苯海明浓度范围为6至380ng/ml时呈线性。日内精密度为89.2%至96.89%,日间精密度为88.6%至93.26%,茶苯海明的平均回收率为97.02%。上述结果证明了萃取的有效性。茶苯海明的检测限(LOD)和定量限(LOQ)分别评估为2ng/ml和6ng/ml,稳定性研究表明茶苯海明在冻融循环后以及在-20°C储存时在血浆中表现出稳定性,该方法开发良好。

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