Development

The present study describes the development and subsequent validation of Reverse phase HPLC (RP-HPLC) method for the analysis of Imeglimin hydrochloride. A novel economic, simple, rapid, accurate, reproducible, and precise Reverse Phase High Performance Liquid Chromatography (RP-HPLC) method for Imeglimin hydrochloride. The method was performed on a YOUNG LIN-HPLC system-ACME9000. The method developed for Imeglimin hydrochloride was quantitatively measured using an isocratic RP-HPLC methodology. The chromatographic separation of Imeglimin hydrochloride was achieved on RP-HPLC equipped with Hypersil BDS C18 (250mm x 4.6mm, 5 um) column using isocratic elution with a mobile phase consisting of MeOH: Buffer in a ratio of (70:30% v/v) at a flow rate of 1.0ml/min with an injection volume of 20µl, where detection was carried out by UV- 730D detector at 239nm The retention time for Imeglimin hydrochloride was found to be 3.47 min. The developed method was successfully with results falling within acceptable criteria validated for different validation parameters as per (ICH-Q2 (R1)) guidelines. The linear regression equation was found to be y = 27.83x - 8.512 with a correlation coefficient (R2) > 0.999 which shows excellent linear correlation. Accuracy, precision, specificity, system suitability, robustness, linearity, LOD and LOQ were determined for method validation. The results were found to be well within recommended limits as per ICH guidelines. Stability studies of Imeglimin hydrochloride were carried out under acidic, basic, peroxide, photolytic and thermal conditions. Degradation was observed in acidic, basic, and oxidative conditions, but not in photolytic and thermal conditions.  

The purpose of this research is to develop and validate a precise method for UV-Vis spectrophotometric and Reverse-Phase High Performance Liquid Chromatography (RP-HPLC) for determination of Octenidine dihydrochloride in bulk and pharmaceutical preparation. According to the relevant experiment the maximum wavelength was found to be 285nm and it is used for further process of development of method and its validation. The developed methods used for quantitative estimation of Octenidine dihydrochloride in pharmaceutical preparation and bulk drug which shows the satisfactory results as per ICH guidelines, so these developed and validated methods are found very simple, sensitive and rapid according to the ICH guideline and can be successfully applied to estimate the ODCL in bulk and pharmaceutical dosage form.

A novel Quality by Design methodology was used to develop and validate a rapid, accurate, precise, simple, efficient and reproducible isocratic Reversed Phase-High Performance Liquid Chromatographic (RP-HPLC) method for the estimation of Luliconazole in bulk and pharmaceutical dosage form. Luliconazole was separated using Kromasil C18 column (250mm×4.6 mm, 5µm particle size), Shimadzu LC2030 HPLC system having UV detector and the mobile phase contained a mixture of 0.01M Ammonium acetate buffer and Acetonitrile (35:65). The flow rate was set to 1.2 ml/min with the responses measured at 294nm. The retention time of Luliconazole was found to be 3.092 min. Central composite design employed for design of experiment and optimization. Desirability value was found to be 0.723 and overall model was found to significant. Linearity was established for Luliconazole in the range of 20-120 µg/ml with correlation coefficient (r2=0.9995). Limit of detection (LOD) and limit of quantitation (LOQ) were evaluated and found to be 1.1700 and 3.5455 respectively. The accuracy values were found to be in the range of 98 –102% and every parameter found with in limit. Validation parameters were evaluated for the method according to the International Conference on Harmonization (ICH) Q2 R1 guidelines. This method can be used for the estimation and analysis of Luliconazole drug in active pharmaceutical ingredients and pharmaceuticals.

To develop and validate simple, rapid, linear, accurate, precise and economical UV Spectroscopic method for estimation of Climbazole in Climbazole shampoo. The drug is freely soluble in organic solvents such as Chloroform and Methanol. The drug was identified in terms of solubility studies and on the basis of melting point done on Melting Point Apparatus of Equiptronics. It showed absorption maxima were determined in Methanol: Water (50:50). The drug obeyed the Beer’s law and showed good correlation of concentration with absorption which reflect in linearity. The UV spectroscopic method was developed for estimation of Climbazole in shampoo dosage form and also validated as per ICH guidelines. The drug is freely soluble in organic solvents such as Methanol, Chloroform. So, the Analytical Grade Methanol: Water is used as a diluent in equal proportion for method. The melting point of Climbazole was found to be 93-94?C (uncorrected). It showed absorption maxima 256 nm in Methanol: Water (50:50). On the basis of absorption spectrum the working concentration was set on 6µg/ml (PPM). The linearity was observed between 2-10 μg/ml (PPM). The results of analysis were validated by recovery studies. The recovery was found to be 98.75, 98.00 and 99.17% for three levels respectively. The % RSD for precision was found to be 0.47%. A simple, rapid, linear, accurate, precise and economical UV Spectroscopic method has been developed for estimation of Climbazole in shampoo dosage form. The method could be considered for the determination of Climbazole in quality control laboratories.

To develop and validate simple, rapid, linear, accurate, precise and economical UV Spectroscopic method for estimation of Fluconazole in tablet dosage form. The drug is freely soluble in organic solvents such as ethanol, DMSO, and dimethyl formamide. The drug was identified in terms of solubility studies and on the basis of melting point done on Melting Point Apparatus of Equiptronics. It showed absorption maxima were determined in Ethanol. The drug obeyed the Beer’s law and showed good correlation of concentration with absorption which reflect in linearity. The UV spectroscopic method was developed for estimation of Fluconazole in tablet dosage form and also validated as per ICH guidelines. The drug is freely soluble in organic solvents such as Ethanol, DMSO, and Dimethyl Formamide. So, the Analytical Grade Ethanol is used as a diluent in method. The melting point of Fluconazole was found to be 139-140?C (uncorrected). It showed absorption maxima 252 nm in Ethanol. On the basis of absorption spectrum the working concentration was set on 60µg/ml (PPM). The linearity was observed between 20-100 μg/ml (PPM). The results of analysis were validated by recovery studies. The recovery was found to be 98.75, 101.00 and 100.83% for three levels respectively. The % RSD for precision was found to be 0.78%. A simple, rapid, linear, accurate, precise and economical UV Spectroscopic method has been developed for estimation of Fluconazole in tablet dosage form. The method could be considered for the determination of Fluconazole in quality control laboratories.

To develop and validate simple, rapid, linear, accurate, precise and economical UV Spectroscopic method for estimation of Valsartan in tablet dosage form. The drug is freely soluble in analytical grade Ethanol, Methanol and Acetonitrile. The drug was identified in terms of solubility studies and on the basis of melting point done on Melting Point Apparatus of Equiptronics. It showed absorption maxima were determined in diluent Methanol: Water (50:50) ratio. The drug obeyed the Beer’s law and showed good correlation of concentration with absorption which reflect in linearity. The UV spectroscopic method was developed for estimation of Valsartan in tablet dosage form and also validated as per ICH guidelines. The drug is freely soluble in analytical grade Ethanol, Methanol, Acetonitrile and sparingly soluble in water. So, the analytical grade Methanol: water (50:50) is used as a diluent in method. The melting point of Valsartan was found to be 115-116?C (uncorrected). It showed absorption maxima 250 nm in Methanol: Water (50:50) ratio. On the basis of absorption spectrum the working concentration was set on 20µg/ml (PPM). The linearity was observed between 10-30 μg/ml (PPM). The results of analysis were validated by recovery studies. The recovery was found to be 98.75, 101.00 and 99.17% for three levels respectively. The % RSD for precision was found to be 0.35%. A simple, rapid, linear, accurate, precise and economical UV Spectroscopic method has been developed for estimation of Valsartan in tablet dosage form. The method could be considered for the determination of Valsartan in quality control laboratories. Keywords: Valsartan, Development, UV Spectrophotometer, Melting Point, Assay Method, Validation, Accuracy, Linearity, Ruggedness, Precision.

In this article forced degradation is a degradation of drug product and new drug substance at different condition more severe accelerated condition. The forced degradation studies ensure chemical behavior of the molecule which in turn helps the development of formulation and packaging. The HPLC is an essential analytical tool in assessing drug and product stability. It insists various conditions like humidity, temperature, light and environmental factors which may affects the drug substance and drug product.

Compendia methods from the USP (United States pharmacopoeia) are widely used in Pharmaceutical drug product testing. However USP methods are under uninterrupted revision to improvement. Donepezil USP monograph is having two methods to quantify donepezil Related substance. The present research work is a single, simple and economic stability indicating impurity profiling method has been developed for scrutiny of Donepezil hydrochloride. Successfully Chromatographic separation has been achieved on an Inertsil C8 3v (150mm x 4.6mm) 3μm with buffered mobile phase consisting of solvent A (mixture of 0.1M phosphate (pH 2.8) buffer and methanol in the ratio 90: 10 (v/v); respectively) and Solvent B (mixture of 0.1 molar (M) phosphate ( pH 2.8) buffer , Acetonitrile and methanol in the ratio 20:20: 60 (v/v); respectively) delivered at flow rate of 1.0 mL/min and the detection wavelength is 215 nm. The drug was subjected to the stress conditions. Donepezil hydrochloride was found to deteriorate significantly in basic, oxidative stress conditions and stable other degradation conditions. One degradant was observed in the stability studies, Which is crossing Identification threshold .the same was isolated and structural elucidation was carried out by H-NMR, Mass spectroscopy. The developed method was corroborated as per ICH guidelines.

The solubility of a substance becomes especially important in the pharmaceutical field because it often represents a major factor that controls the bioavailability of a drug substance. Moreover, solubility and solubility-related properties can also provide important information regarding the structure of drug substances, and in their range of possible intermolecular interactions. For these reasons, a comprehensive knowledge of solubility phenomena permits pharmaceutical scientists to develop an optimal understanding of a drug substance, to determine the ultimate form of the drug substance, and to yield information essential to the development and processing of its dosage forms.

A simple, precise and accurate RP-HPLC method was developed and validated for rapid assay of Dosulepin tablet dosage form. Isocratic elution at a flow rate of 1mL/min was employed on a symmetry Chromosil C18 (250x4.6mm, 5µm in particle size) at ambient temperature. The mobile phase consisted Methanol: Acetonitrile: 0.01M Phosphate buffer in the ratio of 55:20:25 (v/v/v). The UV detection wavelength was 230nm and 20 μL sample was injected. The retention time for Dosulepin was 3.46min. The percentage RSD for precision and accuracy of the method was found to be less than 2%. The method was validated as per the ICH guidelines. The method was successfully applied for routine analysis of Dosulepin tablet dosage form and bulk drug.