Simultaneous Rp-Hplc Method For Determination Of Betamethasone Dipropionate And Tolnaftate In Combined Semisolid Formulation

A new RP-HPLC method was developed for selective and simultaneous determination of betamethasone dipropionate and tolnaftate in combined semisolid formulation containing other components. Further, the proposed method was validated for linearity, precision (system precision, method precision, intermediate or inter-day precision), accuracy, stability in analytical solution, robustness or system suitability and ruggedness. The developed method exhibited the best results in terms of the aforesaid validation parameters. The other components and additives did not interfere in their determinations. The method was found to be selective, simple, economical, accurate, reproducible, rapid and reliable for routine estimation purpose of these drugs in combined semisolid formulations.

LC-MS/MS CHARACTERIZATION OF FORCED DEGRADATION PRODUCTS OF TUCATINIB, A NOVEL TYROSINE KINASE INHIBITOR: DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD

Objective: The current study focused on the development, validation, and characterization of forced degradation products using LC-MS/MS. Methods: A simple, selective, validated and well-defined isocratic HPLC methodology for the quantitative determination of Tucatinib at a wavelength of 239 nm. An isocratic elution of samples was performed on an Inertsil ODS (250x4.6 mm, 5m) column with a mobile phase of 70:30v/v Acetonitrile and formic acid (0.1%) delivered at a flow rate of 1.0 ml/min. MS/MS was used to characterize degradation products formed in the forced degradation study. The validation and characterization of forced degradation products were performed in accordance with ICH guidelines. Results: Over the concentration range of 5-100μg/ml, a good linear response was obtained. Tucatinib's LOD and LOQ were determined to be 0.05 and 0.5, respectively. According to standard guidelines, the method was quantitatively evaluated in terms of system suitability, linearity, precision, accuracy, and robustness, and the results were found to be within acceptable limits. The drug was degraded under acidic, alkaline, and reduction conditions in forced degradation studies. Conclusion: The method was found to be applicable for routine tucatinib analysis. Because no LC-MS/MS method for estimating tucatinib and its degradation products has been reported in the literature. There is a need to develop a method for studying the entire tucatinib degradation pathway.

SIMULTANEOUS ESTIMATION OF AZILSARTAN AND CILNIDIPINE IN BULK BY RP-HPLC AND ASSESSMENT OF ITS APPLICABILITY IN MARKETED TABLET DOSAGE FORM

Objective: This study aims to build up the RP-HPLC process for Azilsartan and Cilnidipine and authenticate the RP-HPLC process according to ICH validation code Q2R1. Methods: System suitability testing was performed to discover the qualifying criterion of the method by injecting the identical standard solution of Azilsartan 40μg/ml and Cilnidipine 10μg/ml in mixture/combination in subsequent optimized chromatographic conditions and the chromatogram was recorded. Moreover, the planned method was validated as per ICH guideline Q2R1 for the following parameters: linearity and range, precision, accuracy, robustness, and determined % recovery. Results: The outcomes of %RSD for retention time and peak area were found to be 0.65 and 1.32 for Azilsartan and 0.85 and 1.90 for Cilnidipine. The correlation coefficient, y-intercept, slope of the regression line were 0.9996,-1127.1, 3313.9, and 0.9993, 1460.2, 2876.4 for Azilsartan and Cilnidipine, respectively. Moreover, the range of this method was observed to be 40-240μg/ml and 10-60 μg/ml for Azilsartan and Cilnidipine, standard concentrations respectively. The % RSD achieved for precision (repeatability) was observed in the range of 1.57 to 2.43 for Azilsartan and 0.70 to 1.88 for Cilnidipine. The % accuracy was found in the range of 96.96 to 101.92% w/w for Azilsartan and 99.19 to101.96%w/w for Cilnidipine. The percent recovery values achieved for Azilsartan were in the range of 99.87 to 106.39% w/w and for Cilnidipine in the range of 94.51 to 105.96% w/w. Conclusion: The author concludes that the simultaneous estimation of Azilsartan and Cilnidipine with predefined objectives was successfully achieved. Moreover, the method was found to be steadfast for the quantification of Azilsartan and Cilnidipine in marketed tablet dosage forms.

Detection and development of a quantitation method for undeclared compounds in antidiabetic biologically active additives and its validation by high performance liquid chromatography

An isocratic, high-performance liquid chromatography (HPLC) quantitation method was developed for the quantitative determination of metformin, glibenclamide, gliclazide, glimepiride in some antidiabetic biologically active additives. A Nucleosil C18, 5 μm, 4.6 mm × 150 mm, column with mobile phase containing buffer (10 mm Na2HPO4, 10 mm sodium dodecyl sulfate): acetonitrile = 68 : 32 (V/V), pH = 7.5 was used. The flow rate was 1.0 mL/min, and effluents were monitored at 226 nm. The retention times of gliclazide glibenclamide, glimepiride and metformin, were 2.203, 4.587, 5.667 and 10.182 min, respectively. Linearity was studied by preparing standard solutions of gliclazide, glibenclamide, glimepiride and metformin at the concentration range of 50% to 150% of working concentration from a stock solution. The method was successfully applied to the estimation of gliclazide, glibenclamide, glimepiride and metformin in some antidiabetic biologically active additives. This method was validated to confirm its system suitability, selectivity, linearity, precision and accuracy according to international conference on harmonization (ICH) guidelines.

Development and validation of a novel stability indicating HPLC method for the separation and determination of darolutamide and its impurities in pharmaceutical formulations

This study reports for the first time about a stability indicating RP-HPLC method for analysis of darolutamide and its impurities 1, 2, and 3 in bulk and formulations. The separation was achieved on Phenomenex column with Luna C18 (250 mm × 4.6 mm, 5 μm) as stationary phase, and 50 mM ammonium acetate: methanol solution 15:80 (v/v) at pH 5.2 as mobile phase at 1.0 mL/min flow rate. UV detection was carried at wavelength of 239 nm. In these conditions the retention time of darolutamide and its impurities 1, 2, and 3 was 7.05, 8.90, 4.63 and 5.95 min, respectively. The method was validated for system suitability, range of analysis, precision, specificity, stability, and robustness. Forced degradation study was done through exposure of the analyte to five different stress conditions and the % degradation was small in all degradation condition. The proposed method can separate and estimate the drug and its impurities in pharmaceutical formulations. Hence, the developed method was suitable for the quantification of darolutamide and can separate and analyse impurities 1, 2, and 3

Analysis of Ethyl p-Methoxycinnamate from Kaempferia galanga L. Extract by High Performance Liquid Chromatography

Ethyl para-methoxycinamate (EPMS) is a major compound of Kaempferia galanga L that has anti-inflammatory effect. The purpose of this study was to determine of EPMS in Kaempferiae galanga L rhizome extract by High Performance Liquid Chromatography (HPLC) and evaluated the performance of the analysis. This study included determination of system suitability, accuracy, precision, linearity and range, limit of detection (LOD) and Limit of quantitation (LOQ) and selectivity. The results of system suitability test HPLC System for EPMS analysis were as follows isocratic elution system of a mobile phase mixture of methanol: water (70:30) containing 0.1% TFA, uv detector at a wavelength of 308 nm using column C18 (150 × 4, 6mm, 5μm) flow rate 1 ml / min. From the analysis, it was found that the average EPMS content was 78.74%. Then method had linear concentration range from 5-360 ppm, with R ² = 0.9999. The LOD and LOQ were 7.0722 ppm and 21.4311 ppm respectively. The accuracy of this method that represented by % recovery was 98.02% - 101.26%. The precision of this method that expressed by Relative Standard Deviation (RSD) was 1.57%. The selectivity of this method that showed by resolution value was 2.6. Based on the results of the system suitability test and analysis performance evaluation,all parameters met the requirements.

The Development and the Validation of a Novel Dissolution Method of Favipiravir Film-Coated Tablets

The aim of this study was to develop and validate a dissolution test for favipiravir release in a tablet dosage form using ultra-high performance liquid chromatography (UHPLC). The dissolution method was developed by testing the solubility of favipiravir in media with different pH values. The results demonstrated that the best dissolution was achieved in phosphate buffer with a pH of 6.8. The amount of favipiravir that was released was about 100% after 30 min. The UHPLC method presented linearity (R = 1.000) in the concentration range of 0.044–0.44 mg/mL. The recovery parameter that was achieved ranged from 102.5% to 104.2%. The system suitability, repeatability, and intermediate precision RSD% results were found to be 0.36%, 1.99%, and 2.49%, respectively. In addition to these parameters and results, an F-test was performed using the Minitab 18 Statistical Software program for the intermediate precision and repeatability results. The standard and sample solutions were found to be stable for 2 days in their respective dissolution medium. This analytical method was also found to be selective for favipiravir. In conclusion, a simple and feasible dissolution method with a short run time of 2.5 min was developed and validated successfully. The obtained results demonstrated that the dissolution test developed here is adequate for its purpose and can be applied as the dissolution method for favipiravir in film-coated tablets for release analyses.

Selective SGLT2 Inhibitor’s Estimation and Validation from Galenical Form by RP-HPLC Method

Aim: The recent analysis is required to do novel and simple, sensitive, precise, efficient, instant and reproducible reverse phase high performance liquid chromatography (RP-HPLC) method for estimation of antidiabetic drug in the unit dosage form. Validation of this method is also planned to make it suitable for the actual use. Study Design: Department of Pharmaceutical Chemistry, Datta Meghe Institute of Medical Sciences deemed to be university, Wardha in collaboration with Balkh university, Mazar-e-sharif, Afghanistan between August 2021 and December 2021. Methodology: In that article develop the method and validate it by estimation of antidiabetic drugs in solid dosage form by RP-HPLC, by using System suitability test, Repeatability, Precision studies (Intra-day and Interday/Intermediate), Linearity/Calibration studies, Robustness, Force degradation, Specificity, Drug recovery/accuracy studies. Results: as per ICH guidelines, the performance if system suitability in remogliflozin were achieved all guidelines; in that, tailing factor (T),separation factors(α),theoretical plates(N),capacity factor (k’), resolution (R) and RSD (%). The validated stress degradation studies under thermal, oxidative, alkali and acid, in few degradation products for remogliflozin (REM). Conclusion: From the results we conclude that, this novel technique which validated for exploration by reverse phase high performance liquid chromatography (RP-HPLC) should be used for routine quality control of remogliflozin (REM) prediction from developed formulation.

Development of Analytical Profile of Lamotrigine and its API Formulation

Objective: The objective of this review is to put a light on the development of lamotrigine and its active pharmaceutical ingredients formulation with proper demonstration. Method: In the present work, one of the most imperative spectrophotometric method which is RP-HPLC method has been developed for the quantitative estimation of lamotrigine in bulk and pharmaceutical formulations. UV spectrophotometric method which involves the determination of Lamotrigine in bulk and in bulk drug and pharmaceutical formulation has maximum absorption at 307.5nm in methanol. It obeys Beer’s and Lambert’s law in the concentration range of 5-45 µg/ml. A rapid and sensitive RP- HPLC Method with UV detection (270 nm) for routine analysis of Lamotrigine formulation was developed. Chromatography was performed with mobile phase containing a mixture of methanol and Phosphate buffer (65:35v/v) with flow rate 1.0 ml/min. In the range of 20-100 µg/ml, the linearity of lamotrigine shows a correlation co-efficient of 0.9998. The proposed method was validated by determining sensitivity and system suitability parameters.

Development of a rapid and reliable high-performance liquid chromatography method for determination of water-soluble vitamins in veterinary feed premix

Background and Aim: Determination of trace amounts of vitamins in multi-component feed premix is a troublesome analytical procedure. In this study, a simple and rapid high-performance liquid chromatography (HPLC) method was developed and validated for the concurrent detection and quantitation of four water-soluble vitamins such as thiamine, riboflavin, pyridoxine, and cyanocobalamin in veterinary feed premixes. Materials and Methods: The chromatographic separation of the vitamins was carried out at 35°C temperature on a reversed-phase C18 column using a gradient pump mode. Mobile phase constituents were solvent (a): 25 mM Potassium dihydrogen phosphate and 5 mM sodium hexanesulfonate in deionized water having pH-4.0 and solvent and (b) 5 mM sodium hexanesulfonate in methanol. Detection was performed with HPLC ultraviolet/visible detection set at 278 and 361 nm wavelength in two different channels. The flow rate was 1.2 mL/min and the total run time was 25 min. Results: The method was validated according to the International Conference on Harmonization and Food and Drug Administration guidelines and acceptance criteria for system suitability, precision, linearity, and recovery were met in all cases. The relative standard deviation for system suitability and precision was <2% for all vitamins. The linearity of the calibration curves was excellent (R2>0.999) at concentration of 5, 10, 15, 20, 25, and 30 μg/mL for all vitamins. The limits of detection values were 0.0125, 0.0017, 0.0064, and 0.0065 μg/mL for thiamine, riboflavin, pyridoxine, and cyanocobalamin, respectively, and the limits of quantification values were 0.0378, 0.0051, 0.0213, and 0.0198 μg/mL for thiamine, riboflavin, pyridoxine, and cyanocobalamin, respectively. The recovery percentages ranged from 88% to 115%. Conclusion: The overall parameters of the proposed method met the validation criteria and this method could be a highly desirable technique for routine analysis of water-soluble vitamins in veterinary feed premix.