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用于测定草药提取物和药物制剂中锥丝碱的高效薄层色谱法。

High-performance thin layer chromatography method for estimation of conessine in herbal extract and pharmaceutical dosage formulations.

作者信息

Kaur Aman D, Ravichandran V, Jain Prateek K, Agrawal Ram K

机构信息

Pharmaceutical Chemistry Research Laboratory, Department of Pharmaceutical Sciences, Dr. Hari Singh Gour University, Sagar, MP 470003, India.

出版信息

J Pharm Biomed Anal. 2008 Jan 22;46(2):391-4. doi: 10.1016/j.jpba.2007.10.001. Epub 2007 Oct 6.

DOI:10.1016/j.jpba.2007.10.001
PMID:18006264
Abstract

A new, simple, sensitive, precise and robust high-performance thin layer chromatographic (HPTLC) method was developed for the estimation of conessine in herbal extracts and pharmaceutical dosage forms. Analysis of conessine was performed on TLC aluminium plates pre-coated with silica gel 60F-254 as stationary phase. Linear ascending development was carried out in twin trough glass chamber saturated with mobile phase consisting of toluene-ethylacetate-diethyl amine (6.5:2.5:1, v/v/v) at room temperature (25+/-2 degrees C). After derivatized the plate with modified Dragendroff's reagent, Camag TLC scanner III was used for spectrodensitometric scanning and analysis of the plate in absorbance mode at 520 nm. The system was found to give compact spots for conessine (Rf value of 0.82). The data for calibration plots showed good linear relationship with r2=0.9998 in the concentration range of 1-10 microg with respect to peak area. The present method was validated for precision and recovery. The limits of detection and quantification were determined. Statistical analysis of the data showed that the method is reproducible and selective for estimation of conessine.

摘要

开发了一种新的、简单、灵敏、精确且稳健的高效薄层色谱(HPTLC)方法,用于测定草药提取物和药物剂型中的锥丝碱。以预涂硅胶60F - 254的TLC铝板为固定相进行锥丝碱分析。在室温(25±2℃)下,于充满由甲苯 - 乙酸乙酯 - 二乙胺(6.5:2.5:1,v/v/v)组成的流动相的双槽玻璃室中进行线性上行展开。用改良的碘化铋钾试剂对板进行衍生化后,使用Camag TLC扫描仪III在520 nm处的吸光度模式下对板进行光密度扫描和分析。该系统对锥丝碱产生致密斑点(Rf值为0.82)。校准曲线数据在1 - 10 μg浓度范围内相对于峰面积显示出良好的线性关系,r2 = 0.9998。对本方法进行了精密度和回收率验证。测定了检测限和定量限。数据的统计分析表明,该方法对于锥丝碱的测定具有可重复性和选择性。

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