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微波介导合成及用于反相高效液相色谱法批量测定新型1,4 - 二氢吡啶的分析方法开发

Microwave Mediated Synthesis and Analytical Method Development for the Estimation of Novel 1,4-Dihydropyridines in Bulk by RP-HPLC.

作者信息

Kaur Anupreet, Kaur Jaspreet, Bansal Ranju

机构信息

University Institute of Engineering & Technology, Panjab University, Chandigarh, India.

University Institute of Pharmaceutical Sciences, Panjab University, Chandigarh, India.

出版信息

Drug Res (Stuttg). 2018 May;68(5):296-300. doi: 10.1055/s-0043-120663. Epub 2017 Nov 3.

DOI:10.1055/s-0043-120663
PMID:29100264
Abstract

The present work describes a rapid and green microwave mediated method for the synthesis and a simple and precise isocratic reverse phase HPLC method for the estimation of the biologically significant dihydropyridines. The conventional synthesis of these dihydropyridines has been previously reported from our lab. The analysis of a standard solution (1 mg/ml) was accomplished on a symmetry (4.6 mm I.D x 250 mm) C-18 column using mobile phase acetonitrile:water:triethylamine (TEA) (70:30:0.1 v/v/v) at a flow rate of 0.7 ml/min. Detection was monitored at 354 nm. The retention time for all the compounds was accomplished as less than 10 min. The compounds showed the linear response over the concentration range 10-100 µg/ml. The study is aimed to develop a rapid method for the quantification of these potent molecules. Various parameters like linearity (10-100 µg/ml), USP tailing and plate count were found to be satisfactory. The investigated parameters were studied with the freshly prepared solutions.

摘要

本工作描述了一种快速且绿色的微波介导合成方法,以及一种简单精确的等度反相高效液相色谱法,用于测定具有生物学意义的二氢吡啶类化合物。此前我们实验室已报道过这些二氢吡啶类化合物的传统合成方法。在一根对称(内径4.6 mm×250 mm)的C-18柱上,使用流动相乙腈:水:三乙胺(TEA)(70:30:0.1 v/v/v),流速为0.7 ml/min,对标准溶液(1 mg/ml)进行分析。检测波长为354 nm。所有化合物的保留时间均小于10分钟。这些化合物在10 - 100 µg/ml的浓度范围内呈线性响应。该研究旨在开发一种快速方法来定量这些强效分子。发现线性(10 - 100 µg/ml)、美国药典拖尾因子和理论塔板数等各种参数均令人满意。所研究的参数是用新制备的溶液进行研究的。

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