INVESTIGATION OF VALIDATION CHARACTERISTICS OF THE METHOD OF QUANTITATIVE DETERMINATION OF PARACETAMOL AND ITS MAIN IMPURITY IN RECTAL SUPPOSITORIES

Abstract

Еxploration of validation characteristicsof the method for the quantitative determination of paracetamol and its main impurity 4-aminophenol in rectal suppositories by spectrophotometry (UV) and high performance liquid chromatography (HPLC). Spectrophotometric measurements were carried out on a UV VIS Lambda 35 spectrophotometer (Perkin Elmer, USA) in cuvettes l = 1 cm. We used a Waters 2695 liquid chromatography with a Waters 2489 UV-detector, as well as a Nucleosil C18 chromatographic column with a size of 250 × 4.6 mm, filled with octadecylsilyl sorbent with a particle size of 10 microns. We used reagents: purified water, which was obtained from the Milli Q plant, manufactured by Millipore Corporation (Germany), sodium hydroxide Sigma-Aldrich, cat. № 06203, sodium 1-butanesulfonate Sigma-Aldrich, cat. № 19022-10G-F; ethanol 96%, methanol Sigma-Aldrich (purity 99.9%), formic acid Sigma-Aldrich, cat. № 33015. Validation characteristics were confirmed as specificity, correctness, precision. The total predicted uncertainty of the analytical method for quantitative determination and the limit of quantitative determination of the main impurity of paracetamol, at which the signal-to-noise ratio is fulfilled, is 10% of the initial concentration of the reference solution (0.5 μg / ml). Confirmed linearity for quantitative determination of paracetamol content in the range of 80 to 120% of the nominal value. Statistical processing of experimental data was carried out; the correlation coefficient of the linear dependence (r) between the entered and found values for the quantitative determination of paracetamol is > 0.990, which indicates the correctness of the method. Methods for the quantitative determination of paracetamol and its main impurity in suppositories have been developed and validated. The method for quantitative determination of paracetamol in suppositories is significantly simpler for routine control of a batch of drugs and is cost-effective compared to the HPLC method. The obtained experimental results indicate that according to the studied validation characteristics, the technique is correct and can be reproduced in other laboratories.