Abstract
The work mainly focused on a validation of the method for determining the content of salicylic acid and individual unknown impurities in new pharmaceutical product—tablets containing: 75, 100 or 150 mg of acetylsalicylic acid and glycine in the amount of 40 mg for each dosage. The separation of the components was carried out by means of HPLC, using a Waters Symmetry C18 column (4.6 × 250 mm, 5 μm) as the stationary phase. The mobile phase consisted of a mixture of 85% orthophosphoric acid, acetonitrile and purified water (2:400:600 V/V/V). Detection was carried out at a wavelength of 237 nm, with a constant flow rate of 1.0 ml min−1. In order to verify the method, linearity, precision (repeatability and reproducibility), accuracy, specificity, range, robustness, system precision, stability of the test and standard solution, limit of quantification and forced degradation were determined. Validation tests were performed in accordance with ICH (International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use) guidelines. The method was validated successfully. It was confirmed that the method in a tested range of 0.005–0.40% salicylic acid with respect to acetylsalicylic acid content is linear, precise and accurate.
Highlights
The work mainly focused on a validation of the method for determining the content of salicylic acid and individual unknown impurities in new pharmaceutical product—tablets containing: 75, 100 or 150 mg of acetylsalicylic acid and glycine in the amount of 40 mg for each dosage
System suitability is an important parameter which allows to ensure that the resolution and reproducibility of the chromatographic system are adequate for the analysis and whether the used method is valid or n ot3,13. %RSD for peak areas of six consecutive injections of System suitability solution (SSS) solution was found to be ≤ 2.0% (0.2% for SA and Acetylsalicylic acid (ASA)) (Table 1)
The forced degradation study confirmed that there was no merging of the peaks of the active ingredients nor salicylic acid with those of any other degradation products
Summary
The work mainly focused on a validation of the method for determining the content of salicylic acid and individual unknown impurities in new pharmaceutical product—tablets containing: 75, 100 or 150 mg of acetylsalicylic acid and glycine in the amount of 40 mg for each dosage. Accurate verification of analytical methods is necessary to ensure high quality of products, which primarily affects the safety of their use. For this purpose, validation is performed, which is the confirmation of meeting the requirements for a specific use or application of a method, by providing objective evidence. The concept has been popularised by quality management systems, mainly ISO 9000 standards, and refers to the validation of analytical methods as well as processes and control measures. The primary direction of the development of analytical procedures of impurities control in pharmaceutical products is the aspiration of determination of the lowest concentrations of substances in the tested samples, which are within the tolerance limits[1]. Often the content of impurities in a pharmaceutical product refers to its quality, which may impose a risk to patient s afety[3]
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