A Rapid and Simple TLC-Densitometric Method for Assay of Clobetasol Propionate in Topical Solution.

Malgorzata Dolowy,Maciej Thomas,Krzysztof Barbusinski,Alina Pyka-Pajak,Violetta Kozik,Josef Jampilek,Andrzej Bak

doi:10.3390/molecules22111888

Abstract

A rapid, simple to use and low-cost thin-layer chromatographic procedure in normal phase system with densitometric detection at 246 nm was carefully validated according to the International Conference on Harmonisation (ICH) guidelines for assay of clobetasol propionate in topical solution containing clobetasol propionate in quantity 0.50 mg/mL. The adopted thin-layer chromatographic (TLC)-densitometric procedure could effectively separate clobetasol propionate from its related compound, namely clobetasol. It is linear for clobetasol propionate in the range of 0.188 ÷ 5 µg/spot. The limit of detection (LOD) and limit of quantification (LOQ) value is 0.061 and 0.186 µg/spot, respectively. Accuracy of proposed procedure was evaluated by recovery test. The mean recovery of studied clobetasol propionate ranges from 98.7 to 101.0%. The coefficient of variation (CV, %) obtained during intra-day and inter-day studies, which was less than 2% (0.40 ÷ 1.17%), confirms the precision of described method. The assay value of clobetasol propionate is consistent with the pharmacopoeial requirements. In conclusion, it can be suitable as a simple and economic procedure for routine quality control laboratories of clobetasol propionate in topical solution.

Highlights

The corticosteroids are a group of chemical compounds which have potent immunosuppressive and anti-inflammatory activity
Based on the literature review, several chromatographic systems consisted of various chromatographic plates for thin-layer chromatographic (TLC) precoated with silica gel 60F254 as well as silica gel RP-18F254 or mixture of silica gel 60 and Kieselguhr F254 and different mobile phases such as acetonitrile-methanol, chloroform-acetone-methanol, toluene-chloroform-methanol-ammonium and toluene-methanol in different ratio have been tried in order to find the best developing system for the analysis of clobetasol propionate in form of solution for skin [22,23,24]
Experimental results showed that the amount of propionate clobetasol in examined pharmaceutical formulation expressed as a percentage of label claim was in good agreement with pharmacopoeial requirements for clobetasol propionate topical solution

Summary

Introduction

The corticosteroids are a group of chemical compounds which have potent immunosuppressive and anti-inflammatory activity. Clobetasol 17-propionate (21-chloro-9-fluoro-11β,17-dihydroxy-16β-methylpregna-1,4-diene-3,20-dione 17-propionate) is one of the most potent topical corticosteroids [1]. It belongs to US class I of the corticosteroids, namely superpotent corticosteroids [1]. Clobetasol propionate is commercially available in different pharmaceutical formulations as ointment, cream, gel, lotion, spray, emollient cream, foam, solution for skin and shampoo in amounts about 0.05% of total weight of the formulation [3]. It is used alone or Molecules 2017, 22, 1888; doi:10.3390/molecules22111888 www.mdpi.com/journal/molecules

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Results

Conclusion