Department of Management and Product Quality, Faculty of Chemical Engineering and Commodity Science, Kazimierz Pulaski University of Technology and Humanities, 27 Chrobrego St, 26-600, Radom, Poland.
Medicofarma S.A., 13 Tarnobrzeska St, 26-613, Radom, Poland.
Sci Rep. 2022 Jan 6;12(1):1. doi: 10.1038/s41598-021-99269-x.
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. 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.
75、100 或 150mg 乙酰水杨酸和 40mg 甘氨酸的新型药物制剂-片剂中水杨酸含量和各单个未知杂质含量的方法。通过 HPLC 分离各成分，采用 Waters Symmetry C18 柱（4.6×250mm，5μm）作为固定相。流动相由 85%磷酸、乙腈和纯净水（2:400:600V/V/V）组成。检测波长为 237nm，流速为 1.0ml/min。为了验证该方法，进行了线性、精密度（重复性和重现性）、准确度、专属性、范围、稳健性、系统精密度、测试和标准溶液稳定性、定量限和强制降解的研究。验证试验符合 ICH（人用药品注册技术要求国际协调会议）指南。该方法得到了成功验证。结果表明，在测试的 0.005-0.40%水杨酸（相对于乙酰水杨酸含量）范围内，该方法具有线性、精确和准确的特点。
