ABSTRACT
Deflazacort is a glucocorticoid used as an anti-inflammatory and immunosuppressant drug. This drug is not official inany pharmacopeia. The objective of this study was to develop, validate, and compare spectrophotometric [absorptivityvalue method, derivative spectroscopy method, and area under curve (AUC) method] and high-performance liquidchromatography (HPLC) methods for the determination of deflazacort in the pharmaceutical dosage form (tablets).The Method A is simple absorptivity value method and is established on the determination of deflazacort in ethanoland water at 247 nm. The Method B is a derivative spectrophotometric method and engrosses the measurement ofdeflazacort using the zero-order- and first-order derivative technique at 276.5 nm as maxima and 228.2 nm as minima.Method C is an AUC method. This method entails the computation of the incorporated value of absorbance withcontext to the wavelength between two selected wavelengths 230.2 and 264.4 nm, respectively. Method D is byHPLC, which was carried out using C18 column, mobile phase consisting of acetonitrile:methanol:phosphate bufferpH 7.0 (90:5:5 v/v/v) with flow rate 1 ml/minute and detection done at 247 nm, which provide a sharp peak with ashort retention time of 4.025 minutes. The advantage of this HPLC method can be observed from its attributes, suchas asymmetry (1.1732), column efficiency (718610.6), and standard deviation (0.5929868), which indicated that thedeveloped system has better eluting characteristics than the previously developed method. However, the limit ofdetection is marginally lower than that of the previous method. Since, the method is not available in any pharmacopeiafor the routine analysis of deflazacort, the novel developed spectroscopic and RP-HPLC methods may be highly usefulfor the industries manufacturing and maintaining the quality aspects of this drug
ABSTRACT
A novel, selective, precise, and sensitive stability indicating Reverse Phase-High Performance Liquid Chromatography(RP-HPLC) method has been developed and validated for simultaneous estimation of Glecaprevir (GLE) andPibrentasvir (PIB) for bulk and pharmaceutical dosage form. The chromatographic separation was accomplished ona Denali C18 column (150 mm × 4.6 mm, 5 µm) by using mobile phase buffer (pH 4.8) and acetonitrile in the ratio of60:40 v/v. An injection volume of 10 µl was used via manual rheodyne and the solute was detected at a UV wavelengthof 260 nm. The mobile phase was pumped at an ambient temperature of 30°C with a flow rate of 1 ml/minute. Theretention time of GLE and PIB were found to be 2.13 and 3.46 minutes, respectively. The Q2b validation of theproposed analytical method revealed several features; linear regression analysis data showed good linearity over theconcentration range 25–150 µg/ml for GLE and 10–60 µg/ml for PIB with r2 of 0.999 in both the cases and the meanrecovery of them were found to be 100.33% and 100.47%, respectively. The accuracy and precision aspects expressed<2% relative standard deviation value along with adequate robustness. The acid, alkali, neutral, dry heat, UV, andphoto-degradation studies demonstrated the formation of various degradation products. The proposed analyticalmethod proved to be suitable for the routine simultaneous analysis of both the drugs in bulk and tablet formulations.potential, morphology, encapsulation efficiency, and stability of microcapsules. The characterization results from eachformulation reported that the ratio of mangosteen peel extract and maltodextrin at level 50%:50% (MP3) producedmore proportional characteristics than other treatments. The formulation of mangosteen peel extract with maltodextrinat a balanced ratio could be used as an alternative supply and processing of functional food.