TLC—Densitometric Determination of Sulfasalazine and Its Possible Impurities in Pharmaceutical Preparations

A Kwiecień,K Piątek,J Krzek,P Żmudzki

doi:10.1556/achrom.27.2015.4.4

Abstract

A simple, selective, and sensitive thin-layer chromatographic—densitometric method has been developed for the determination of sulfasalazine besides its possible impurities in pharmaceutical preparations. The mobile phase was composed of ethyl acetate—methanol—ammonia 25% 10:7:3 (υ/υ/υ), and the stationary phase was aluminum plates precoated with silica gel 60 F254 that enabled to obtain well resolved peaks of sulfasalazine and its impurities. The developed chromatograms were analyzed densitometrically at λ = 360 nm. RF values and ultraviolet (UV) spectra were used to identify the compounds. The developed method is highly sensitive (limit of detection [LOD] = 17.11 ng spot−1, limit of quantitation [LOQ] = 51.84 ng spot−1), precise (relative standard deviation [RSD] = 1.43%–4.28%), and accurate (RSD = 1.64%–4.27%). The linearity of the method was checked within the range 20–120 ng spot−1. The method was successfully applied for the determination of sulfasalazine in pharmaceutical preparations besides its i...

Highlights

Sulfasalazine 5-[4-(2-pyridylsulfamoyl)phenylazo]salicylic acid was designed by Svartz in 1942 by combining an antibiotic sulfapyridine with an anti-inflammatory agent 5-aminosalicylic acid through an azo bond [1]
Myofibroblasts cells contribute to scar tissue in a diseased liver; these cells secrete proteins that prevent the breakdown of the scar tissue
The obtained plots of residuals were without trends, which proves the linearity of the working range

Summary

Introduction

Sulfasalazine 5-[4-(2-pyridylsulfamoyl)phenylazo]salicylic acid was designed by Svartz in 1942 by combining an antibiotic sulfapyridine with an anti-inflammatory agent 5-aminosalicylic acid through an azo bond [1]. Different analytical methods were applied for the determination of sulfasalazine in pharmaceutical preparations and biological fluids. The aim of this study was to develop a chromatographic–densitometric method for the determination of sulfasalazine besides its possible impurities in pharmaceutical preparations. Chromatograms were developed over a distance of 95 mm using ethyl acetate–methanol–ammonia 25% 10:7:3 (v/v/v) in a chromatographic chamber 18 × 9 × 18 cm in size (Sigma-Aldrich, USA) saturated for 10 min with the mobile phase vapour at room temperature. To check linearity of the method, 2, 4, 6, 8, 10, and 12 μL of sulfasalazine standard solution at a concentration of 0.001% w/v were applied to the chromatographic plate 120 × 100 mm in size. The concentration of sulfasalazine in preparations under examination was computed by comparing the peak areas for the standard and sample solutions.

Results and Discussion

Result

Conclusion