Determination of degradation products and process related impurities of asenapine maleate in asenapine sublingual tablets by UPLC

14th International Conference on Science, Engineering and Technology

自然科学;工业技术

Kumar, Nitin^1,2 ; Sangeetha, D.^2 ; Kalyanraman, L.^1

Department of Analytical Research and Development, IPDO, Dr Reddy's Laboratories, Hyderabad

500 072, India^1

Department of Chemistry, School of Advanced Sciences, VIT University, Vellore, Tamilnadu, India^2

关键词: Ammonium hydrogen sulphate;    Degradation products;    Gradient elution mode;    Method validations;    Potassium dihydrogen phosphate;    Process-related impurities;    Stability-indicating;    Stability-indicating UPLC;   

Others  :  https://iopscience.iop.org/article/10.1088/1757-899X/263/2/022029/pdf
DOI  :  10.1088/1757-899X/263/2/022029

来源: IOP

【 摘 要 】

For determination of process related impurities and degradation products of asenapine maleate in asenapine sublingual Tablets, a reversed phase, stability indicating UPLC method was developed. Acetonitrile, methanol and potassium dihydrogen phosphate buffer with tetra-n-butyl ammonium hydrogen sulphate as ion pair (pH 2.2; 0.01 M) at flow rate of 0.2 ml/min were used in gradient elution mode. Separation was achieved by using acquity BEH Shield RP18 column (1.7 μm, 2.1 mm×100 mm) at 35 °C. UV detection was performed at 228 nm. Subsequently the liquid chromatography method was validated as per ICH. The drug product was exposed to the stress conditions of acid hydrolysis, base hydrolysis, water hydrolysis, oxidative, thermal, and photolytic. In oxidative stress and thermal stress significant degradation was observed. All the degradation products were well separated from analyte peak and its impurities. Stability indicating nature of the method was proved by demonstrating the peak purity of Asenapine peak in all the stressed samples. The mass balance was found >95% for all the stress conditions. Based on method validation, the method was found specific, linear, accurate, precise, rugged and robust.