Development of a unified approach to the method of identification, quantitative determination of active substances and accompanying impurities in a combined drug by HPLC method

Abstract

The aim of the work is to develop a method of identification, quantification of acetylsalicylic and ascorbic acids in the combined presence and concomitant impurities in the combined drug in the form of effervescent powder for preparation of oral solution by liquid chromatography and study of validation characteristics. Materials and methods. ProStar liquid chromatograph with “Varian” spectrophotometric detector. Chromatographic column with a size of 150×4.6 mm, filled with aminopropylsilyl silica gel for chromatography (Supelcosil LC-NH2, “Supelco”) with a precolumn (particle size 3 μm), mobile phase - buffer solution pH 3.2 - acetonitrile P (80:20), elution mode – isocratic; mobile phase velocity – 1.2 ml/min; the detection wavelength is 240 nm. Results. To determine acetylsalicylic and ascorbic acids by high-performance liquid chromatography with UV detection, the optimal chromatographic conditions were selected considering the influence of other active and excipients in the drug. To prove the possibility of applying the proposed technique in the subsequent analysis of the effervescent powder, its validation was performed. The obtained validation characteristics indicate that the method of quantitative determination of acetylsalicylic acid in the studied dosage form corresponds to the parameters: accuracy, precision, linearity ( =0.92≤max =1.60, d=0.19≤maxd=0.51, a=0.17 max a=2.60, r=0.9994 min r=0.9981). In the quantitative determination of ascorbic acid in the combined effervescent powder it is established that the correctness, precision, linearity are performed ( =0.86≤max =1.60, d=0.02≤max d=0.51, a=1.99 max a=2.60, r=0.9997 min r=0.9981). Conclusions. A new method for the identification, quantification of acetylsalicylic and ascorbic acids in the combined presence and concomitant impurities in the effervescent powder using high performance liquid chromatography has been developed. The validation of the proposed method is carried out and its acceptability for use in pharmaceutical analysis is proved