建立了一种高效液相色谱法定量测定茯苓提取物和复方制剂中黄芩苷含量的方法

Kedar Kalyani Abhimanyu , Chaudhari Sanjay Ravindra , Rao Srinivasa Avanapu
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引用次数: 13

摘要

建立了高效液相色谱(HPTLC)法测定大戟科黄芩叶、树皮提取物和复方制剂中黄芩苷的含量。采用流动相甲苯:氯仿(9:1 v/v)对样品进行TLC预涂铝板(60 F254)分析。用香兰素硫酸衍生化板,580 nm扫描。建立的方法在Rf值为0.43±0.01时给出了致密点。该方法采用国际协调委员会(ICH)指南进行验证,包括线性、精密度、准确度和鲁棒性。黄芪叶提取物(0.003% w/w)、树皮提取物(0.04% w/w)、制剂1 (0.002% w/w)和制剂2 (0.035% w/w)中均含有黄芪苷。弗里德林在(100 ~ 500 ng点−1)呈良好的线性关系,相关系数(r2)为0.9892。弗里德林的检出限和定量限分别为32.15、97.44 ng/波段。结果表明,该方法的精密度为0.78%,日内精密度为0.9% (%RSD)。通过三种不同浓度水平的回收率研究,验证了该方法的准确性,发现弗里德林的平均回收率为98.55%。结果表明,该方法简便、特异、准确、可靠。
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A validated HPTLC method for the quantification of friedelin in Putranjiva roxburghii Wall extracts and in polyherbal formulations

In present study HPTLC method was developed and validated for the determination of friedelin in Putranjiva roxburghii Wall (family: Euphorbiaceae) leaf, bark extract and in polyherbal formulations. Analysis of samples were performed on TLC aluminium precoated plate (60 F254) by using mobile phase toluene: chloroform (9:1 v/v). Plate was derivatized with vanillin sulphuric acid and scanned at 580 nm. Developed method found to give compact spot for friedelin at Rf value 0.43 ± 0.01. The method was validated using International Council for Harmonization (ICH) guidelines including linearity, precision, accuracy, and robustness. Friedelin was found to be present in leaf extract of Putranjiva roxburghii Wall (0.003% w/w), in bark (0.04% w/w), formulation 1 (0.002% w/w) and formulation 2 (0.035% w/w). A good linearity relationship was found to be (100–500 ng spot−1) with correlation coefficient (r2) value of 0.9892 for friedelin. Limit of detection and limit of quantitation was found to be 32.15, 97.44 ng/band respectively for friedelin. The developed method was found to be accurate and precise with 0.78%, 0.9% (%RSD) for interday and intraday precision. Accuracy of the method was performed by recovery studies at three different concentration levels and the average percentage recovery was found to be 98.55% for friedelin. The proposed method for the quantitation of friedelin was found to be simple, specific, accurate and robust in Putranjiva roxburghii Wall and polyherbal formulations.

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