Objective: A simple, precise and accurate UV-spectrophotometric method is developed and statistically validated for estimation of Testosterone in gel formulation. The proposed method includes using regression equation, area under curve (AUC), first order derivative and second order derivative spectroscopic method.Methods: based on measurement of absorbance at a selected wavelength using UV-visible spectrophotometer with 1cm matched quartz cell and acetonitrile as a solvent. All developed methods obeyed Beer's-lambert's law in the concentration range of 5-25μg/mL, with correlation coefficient value less than 1. Results:The percent amount of drug estimated was nearly 100%, found to be a good agreement with label claim of marketed gel formulation. The recovery study was carried out at three different levels, the validation study data was found to be statistically significant as all the statistical parameters are within the acceptance range (% RSD <2.0 and S.D. <±2.0). Conclusions:The results of estimation and validation parameters like accuracy, precision, ruggedness, linearity and range were studied for all the developed methods and were found to be within limits. The results obtained were statistically compared using paired t-test and one way ANOVA analysis. The proposed method can be adopted for routine quality control for estimation of drug in formulation.
Aim: The current study dealt with the degradation behavior of Bilastine and degradation kinetics of a drug in solution state. Background: Very limited information on the effect of pH on maximum stability has been published. In order to understand the degradation kinetics of bilastine, aqueous stability studies were carried out, because such studies on bilastine have not been reported in the literature, further no methods have reported about shelf-life determination of bilastine. The study design involves selection of stability indicating RP-HPLC method for estimation of drug then evaluation of degradation kinetics, shelf-life determination and validation of proposed method. Results: The Shimadzu HPLC series 1100 was used for stress degradation analysis of bilastine in tablet dosage form. The analysis was performed using Agilent ZORBAX SB-C8 (4.6×150×5µm) column and Phosphate Buffer: Acetonitrile (pH-5.0) in the ratio of 60:40 as mobile phase; wavelength selected for analysis was 254nm with the flow rate of 1mL/min at which drug showed sharp peak. The analysis was performed on the isocratic pump mode with the injection volume of 20µl. The mobile phase is used as diluent. The proposed method was found to be linear over the range 10 to 50 µg/mL. The analysis was performed by placing standard and samples with 7 different pH buffer, oxidative and neutral hydrolytic solutions in oven at 40ºC, 60⁰C and room temperature for an interval of 30, 60, 90, 120, 150, 180 mints for standard and samples. The results indicated that the pH, temperature, ionic strength and oxidation greatly influence the stability of Bilastine and the degradation behavior of Bilastine followed pseudo-first-order kinetics. Bilastine was most stable in neutral, alkaline, lower temperature conditions and lower ionic strength. Conclusion: The proposed method was found to be specific, selective and robust and successfully applied for its assay, degradation (stress testing) of drug and degradation kinetics in solution state. Keywords: Degradation, Stability, Bilastine, RP-HPLC, Kinetics
The research work aims to develop a bioanalytical method using liquid chromatography and validated for the determination of canagliflozin by using an internal standard. Department of Pharmaceutical Chemistry, Smt. Kishoritai Bhoyar College of Pharmacy, New Kamptee, Nagpur (MS). Isocratic chromatography separation was achieved on an LC system with PDA detector on an ACE C18 (150mm× 4.6mm × 5µm) column using a mobile phase composition of acetonitrile: ammonium acetate buffer in the ration of 50:50 v/v (pH 4.5), orthophosphoric acid is used to adjust pH of mobile phase and the flow rate at 1.0ml/ min. and estimation was carried out at 291 nm. The retention time of a drug was 4.633 minutes. The method was validated for several parameters (specificity, linearity, precision, and accuracy) and also successfully applied for the pharmacokinetic in female rats. Calibration plot was linear (r2 > 0.9973) over the concentration range of 5-30 µg/ml for canagliflozin. The high recovery and low relative standard deviation (%RSD) confirm the suitability of the method. The result of Limit of Detection (LOD) and Limit of Quantitation (LOQ) were found to be 0.1099 μg/ml and 0.3331 μg/ml, respectively. The new RP-HPLC method can be conveniently adapted for examining canagliflozin concentration in rat plasma after oral administration.
Aim: The aim of the research work has to development and validation of dissolution test method for Tapentadol using HPLC method, investigate the effects of stress on dissolution stability by thermal and non-thermal methods. The present research work mainly focused on the evaluation and compares the influence of accelerated-aging conditions on the drug content and in vitro dissolution stability. Place and duration of Study: Department of Pharmaceutical Chemistry, Smt. Kishoritai Bhoyar College of Pharmacy, New Kamptee, Nagpur (MS). Methodology and Results: Saturated solubility study of tapentadol were carried out using different dissolution media and different conditions such as type of dissolution medium, volume of dissolution medium and rotation speed of paddle were evaluated. Basis of it, dissolution testing were carried out on a suitably calibrated USP Apparatus II (TDT-06L) at 50 ± 1 rpm, under sink conditions in 900 mL of deaerated distilled water at 37±0.5ºC for each test and selected most optimized dissolution parameter which given maximum % release of drug. The drug release was evaluated by high-performance liquid chromatographic method. Also proposed method were validated as per ICH guidelines with respect to system suitability, linearity, precision, accuracy, range, robustness, ruggedness and solution stability parameters were evaluated and the obtained results were within the acceptable range. The stress on dissolution stability of standard powdered drug, tablet formulation and packed strip formulation were investigated by using thermal and non thermal methods. The results obtained in all stress conditions such as thermal, humidity, UV light and visible light were evaluated for drug content and drug release. The results were statistically evaluated by applying two-way ANOVA followed by post-hoc Bonferroni test and their results represented as a graphical plot. Conclusion: In our investigation of stress dissolution of drug it was found that Tapentadol HCl std. drug was susceptible to degradation. The tablet and packaged formulation were susceptible to photolytic degradation indicated by difference in drug content while the release was more affected under UV exposed to tablet and strip packaged formulation as compared to other stress conditions.
A simple and rapid reverse-phase HPLC method was developed for determination of Teneligliptin (TGP) in the presence of its degradation products generated from forced decomposition studies. The HPLC separation was achieved on a C18 ACE column (150x 4.6 mm i.d.; 5 μm) using mobile phase as a mixture of Phosphate buffer pH-7.2 using ortho-phosphoric acid: methanol (30:70v/v). The UV detection was carried out at 245nm at ambient temperature and the flow rate of 1.0 mL/min. The calibration curve was found to be linear in the concentration range of 10-50 μg/mL(r=0.9993). Force degradation study was performed under various conditions like acidic, alkaline, oxidative, photolytic and mass balance calculations were carried out from the degradation results. The developed method was validated as per ICH guidelines with respect to linearity, accuracy, precision, limit of detection and quantification. The robustness of the proposed method was evaluated by the Plackett Burman design. The purity of the degraded sample was checked by peak purity analysis. The peaks of degradation products did not interfere with that of pure Teneligliptin.
Aims: Synthesis/preparation of Lamotrigine (LMN) complexes with β-CD, Caffeine, Nicotinamide, EDTA and Development of a new reverse phase liquid chromatographic (HPLC) method for the investigation of Lamotrigine in rat plasma after oral administration and pharmacokinetic assessment of Lamotrigine. Study Design: The present work describes the formation of LMN drug complexes with β-Cyclodextrin, Caffeine, Nicotinamide and Disodium EDTA. Physical mixture, kneading and solvent evaporation methods were used to prepare LMN complexes (In ratios 1:1, 1:2, 2:1). Further characterization was performed by UV, FTIR, PXRD, and DSC. A reverse phase HPLC method was developed for the investigation of LMN in rat plasma using internal standardization method after oral administration of LMN and its complexes. Place and Duration of Study: Department of Pharmaceutical Chemistry, Smt. Kishoritai Bhoyar College of Pharmacy, RTMN University, Nagpur, between July 2018 and June 2019. Methodology: LMN complexes with β-CD, Caffeine, Nicotinamide, EDTA was prepared in three ratios i.e. 1:1, 1:2 and 2:1 and characterized by UV, FTIR, PXRD, and DSC. In-vitro Solubility study was performed by saturation solubility study, further % practical yield, drug content, melting point was determined. In-vitro dissolution study of prepared complexes was performed in dissolution apparatus using the paddle method, according to USP Type II. Dissolution studies were carried out using 900 mL 0.1M HCl at 37± 0.5°C at 50 revmin−1 (US FDA guidelines).The interaction of LMN with these hydrophilic complexing agents was characterized by UV, FTIR, PXRD and DSC. A reverse phase HPLC bioanalytical method was developed and validated as per ICH guidelines for the quantitative determination of LMN in rat plasma using internal standardization method (HTZ) after oral administration of LMN and its complexes. The method was successfully applied for the pharmacokinetic study in rat. The pharmacokinetic parameter like AUCt, AUCi, MRTi, Cmax, Tmax, t1/2, were calculated using pharmacokinetic software PK solver 2. The efficient separation was carried out for High Performance Liquid Chromatography (HPLC) method on Eclipse XDB-C18 (150×4.6×5 µ) column using a mobile phase consisting of filtered and degassed mixture of potassium dihydrogen orthophosphate buffer (pH 7.0) and Methanol in the ratio 65:35 v/v at a flow rate of 0.8 mL/min and UV detection at 307 nm. Results: The LMN complexes were successfully prepared and characterized by UV, FTIR, PXRD, and DSC from which solvent evaporation method was found to be best as per result of in-vitro dissolution study. In-vitro dissolution study reveals that LMN-Caffeine (C1) and LMN-NTM (N1) complexes showed 100.14 and 100.01% drug release at 15 min and 20 min respectively as compared to pure drug (LMN) which shows only 50.56% drug release at 75 min. LMN concentration in blood plasma reached (Cmax) was found to be 19.4732 µg/mL at Tmax of 5h, Whereas Cmax of LMN complexes were found to be 48.4876 (B1), 72.2160 (C1), 62.2739 (N1) and 49.3170 (E1) µg/mL at Tmax of 5h out of which complex C1 and N1 in the present study resulted in a sharp increase in Cmax. All complexes showed 4 to 5 time enhancement of Cmax as compared to LMN.. The results demonstrated that complexes of Lamotrigine were successful strategy to improve the solubility and dissolution behavior of Lamotrigine. The complex B1 shows maximum t1/2 and MRTi of 36.224 h and 52.441 h as compared to C1, N1 and E1 having t1/2 of 14.1575, 16.258 and 21.702 h and MRTi of 19.997, 22.994 and 30.883 h respectively. Hence B1 required lesser dosing frequency as compared to other complexes. Conclusion: The Lamotrigine complexes were prepared and confirmation of prepared complexes was done by physical characterization (FTIR. DSC, PXRD and UV) and solubility determination by saturation solubility study. The bioanalytical method was developed for estimation of plasma drug concentration of LMN. The method was validated according to ICH guidelines to estimate the mean plasma concentration of LMN after oral administration using internal standardization method (HTZ). Method was reproducible and high recovery of LMN from its complexes was achieved. The method was found to be highly satisfactory sensitive, accurate, linear and specific.
scite is a Brooklyn-based organization that helps researchers better discover and understand research articles through Smart Citations–citations that display the context of the citation and describe whether the article provides supporting or contrasting evidence. scite is used by students and researchers from around the world and is funded in part by the National Science Foundation and the National Institute on Drug Abuse of the National Institutes of Health.
hi@scite.ai
10624 S. Eastern Ave., Ste. A-614
Henderson, NV 89052, USA
Copyright © 2024 scite LLC. All rights reserved.
Made with 💙 for researchers
Part of the Research Solutions Family.