TLC-密度测定法测定胶囊中的丙戊酸。

Use of TLC-Densitometric Method for Determination of Valproic Acid in Capsules.

机构信息

Department of Analytical Chemistry, Faculty of Pharmaceutical Sciences in Sosnowiec, Medical University of Silesia in Katowice, Jagiellońska 4, 41-200 Sosnowiec, Poland.

出版信息

Molecules. 2022 Jan 24;27(3):752. doi: 10.3390/molecules27030752.

DOI:10.3390/molecules27030752

PMID:35164016

原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC8839749/

Abstract

Determination of valproic acid in the drug was carried out on the aluminum silica gel 60F plates and using acetone-water-chloroform-ethanol-ammonia at a volume ratio of 30:1:8:5:11 as the mobile phase, respectively. Two methods of detection of valproic acid were used. The first was a 2% aqueous CuSO×5HO solution, and the second was a 2',7'-dichlorofluorescein-aluminum chloride-iron (III) chloride system. The applied TLC-densitometric method is selective, linear, accurate, precise, and robust, regardless of the visualizing reagent used for the determination of valproic acid in Convulex capsules. It has low limits of detection (LOD) and limits of quantification (LOQ), which are equal to 5.8 μg/spot and 17.4 μg/spot using a 2% aqueous CuSO×5HO solution as visualizing agent and also 0.32 μg/spot and 0.97 μg/spot using a 2',7'-dichlorofluorescein-aluminum chloride-iron (III) chloride system as visualizing reagent, respectively. The described analytical method can additionally be used to study the identity of valproic acid in a pharmaceutical preparation. The linearity range was found to be 20.00-80.00 μg/spot and 1.00-2.00 μg/spot for valproic acid detected on chromatographic plates using a 2% aqueous CuSO×5HO solution and the 2',7'-dichlorofluorescein-aluminum chloride-iron (III) chloride system, respectively. A coefficient of variation that was less than 3% confirms the satisfactory accuracy and precision of the proposed method. The results of the assay of valproic acid equal 96.2% and 97.0% in relation to the label claim that valproic acid fulfill pharmacopoeial requirements. The developed TLC-densitometric method can be suitable for the routine analysis of valproic acid in pharmaceutical formulations. The proposed TLC-densitometry may be an alternative method to the modern high-performance liquid chromatography and square wave voltammetry in the control of above-mentioned substances, and it can be applied when other analytical techniques is not affordable in the laboratory.

摘要

采用硅胶 G 薄层板，以丙酮-水-氯仿-乙醇-氨（30:1:8:5:11）为展开剂，分别对药物中的丙戊酸进行测定。采用两种检测方法检测丙戊酸。第一种是 2%的硫酸铜五水合物溶液，第二种是 2'，7'-二氯荧光素-氯化铝-三氯化铁体系。所应用的 TLC-密度测定法是选择性的、线性的、准确的、精密的和稳健的，无论用于测定 Convulex 胶囊中丙戊酸的可视化试剂如何。它具有较低的检测限（LOD）和定量限（LOQ），使用 2%的硫酸铜五水合物溶液作为可视化试剂时，LOD 和 LOQ 分别等于 5.8μg/斑点和 17.4μg/斑点，使用 2'，7'-二氯荧光素-氯化铝-三氯化铁体系作为可视化试剂时，LOD 和 LOQ 分别等于 0.32μg/斑点和 0.97μg/斑点。该分析方法还可用于研究药物制剂中丙戊酸的特性。使用 2%的硫酸铜五水合物溶液和 2'，7'-二氯荧光素-氯化铝-三氯化铁体系在色谱板上检测到的丙戊酸的线性范围分别为 20.00-80.00μg/斑点和 1.00-2.00μg/斑点。变异系数小于 3%，证实了所提出方法的令人满意的准确性和精密度。丙戊酸测定的结果分别为 96.2%和 97.0%，与标签声称丙戊酸符合药典要求的结果相符。所开发的 TLC-密度测定法可适用于药物制剂中丙戊酸的常规分析。所提出的 TLC-密度测定法可作为现代高效液相色谱法和方波伏安法的替代方法，用于控制上述物质，并且当实验室无法使用其他分析技术时，可以应用该方法。