Validation

The aim of the research study was the development and validation of a simple, rapid, accurate and precise reversed-phase high performance liquid chromatography (RP-HPLC) stability-indicating method for the determination of aceclofenac in bulk and pharmaceutical dosage forms. The RP-HPLC studies was performed on the instrument Jasco HPLC system with Jasco UV 2010 photo diode array detector, ODS C18 RP-column (Intersile 250 mm × 4.6 mm; i.d. 10 μm), Rheodyne injection syringe with 20µL loop volume and windows based chrompass software was used for separation. The isocratic elution was performed using the mobile phase ratio of methanol: water (65:35 v/v) and UV detection wavelength at 263 nm. The overall run time of the analysis was 20 minutes and the flow rate was 1.0 mL/min. The RP-HPLC method developed for analysis of aceclofenac was validated as per the ICH guidelines with respect to specificity, selectivity, linearity, accuracy, precision and robustness. The linearity for developed method was observed in the concentration range of 5-50 μg/mL with the correlation coefficient (r2) of 0.9992. The percentage accuracy of aceclofenac ranged from 99.40 to 100.79%. The relative standard deviation for inter-day precision was lower than 2.0%. The assay of aceclofenac was determined in tablet dosage form was found to be within limits. Aceclofenac was subjected to stress conditions such as neutral, acidic, alkaline, oxidation, and photolysis degradations as per ICH guidelines. The results of degradation studies revealed that the drug degraded a maximum (32.68%) in acidic conditions followed by alkaline conditions (15.05%). The drug was found to be resistant towards neutral, acidic and photolytic degradation conditions.

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.

To develop and validate simple, rapid, linear, accurate, precise and economical UV Spectroscopic method for estimation of Ivabridine HCl in tablet dosage form. The drug is freely soluble in analytical grade water. 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 analytical grade water. 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 Ivabridine HCl in tablet dosage form and also validated as per ICH guidelines. The drug is soluble in analytical grade water, slightly soluble in methanol and freely soluble in ethanol. So, the analytical grade water is used as a diluent in method. The melting point of Ivabridine HCl was found to be 194-195?C (uncorrected). It showed absorption maxima 260 nm in analytical grade water. 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, 98.33 and 101.25% for three levels respectively. The % RSD for precision was found to be 0.54%. A simple, rapid, linear, accurate, precise and economical UV Spectroscopic method has been developed for estimation of Ivabridine HCl in tablet dosage form. The method could be considered for the determination of Ivabridine HCl in quality control laboratories. Keywords: Ivabridine HCl, UV Spectrophotometer, Melting Point, Assay Method, Validation, Accuracy, Linearity, Ruggedness, Precision.

To develop and validate simple, rapid, linear, accurate, precise and economical UV Spectroscopic method for estimation of Guaifenesin in tablet dosage form. The drug is freely soluble in analytical grade 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 analytical grade Methanol. 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 Guaifenesin in tablet dosage form and also validated as per ICH guidelines. The drug is freely soluble in analytical grade Methanol, moderately soluble in Benzene and soluble in Chloroform, Glycerol. So, the analytical grade Methanol is used as a diluent in method. The melting point of Guaifenesin was found to be 78-79ËšC (uncorrected). It showed absorption maxima 269 nm in analytical grade Methanol. On the basis of absorption spectrum the working concentration was set on 10µg/ml (PPM). The linearity was observed between 6-14 μg/ml (PPM). The results of analysis were validated by recovery studies. The recovery was found to be 98.75, 101 and 99.17% for three levels respectively. The % RSD for precision was found to be 0.97%. A simple, rapid, linear, accurate, precise and economical UV Spectroscopic method has been developed for estimation of Guaifenesin in tablet dosage form. The method could be considered for the determination of Guaifenesin in quality control laboratories.

To develop and validate simple, rapid, linear, accurate, precise and economical UV Spectroscopic method for estimation of Lansoprazole in Capsule dosage form. The drug is soluble in analytical grade 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 analytical grade Methanol. 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 Lansoprazole in Capsule dosage form and also validated as per ICH guidelines. The drug is freely soluble in Dimethylformamide, soluble in analytical grade Methanol, sparingly soluble in Ethanol, slightly soluble in Ethyl Acetate, Dichloromethane and Acetonitrile. So, the analytical grade Methanol is used as a diluent in method. The melting point of Lansoprazole was found to be 179-180ËšC (uncorrected). It showed absorption maxima 285 nm in analytical grade Methanol. On the basis of absorption spectrum the working concentration was set on 10µg/ml (PPM). The linearity was observed between 6-14 μg/ml (PPM). The results of analysis were validated by recovery studies. The recovery was found to be 98.75, 99.00 and 100.80 % for three levels respectively. The % RSD for precision was found to be 0.9039 %.A simple, rapid, linear, accurate, precise and economical UV Spectroscopic method has been developed for estimation of Lansoprazole in Capsule dosage form. The method could be considered for the determination of Lansoprazole in quality control laboratories.

A simple Reverse phase liquid chromatographic method has been developed and subsequently validated for estimation of lansoprazole in tablet dosage form. The separation was carried out using a mobile phase consisting of Methanol and 0.1% OPA (Ortho Phosphoric Acid) in the ratio of 70:30. The column used was C18 and 250 mm length with flow rate of 1.2 ml / min using UV detection at 285nm. The described method was linear over a concentration range of 10-50 μg/ml for the assay of Lansoprazole. The retention time of Lansoprazole was found to be 6.6 min, and all the results of analysis were validated statistically. The results of the study showed that the proposed RP-HPLC method is simple, rapid, precise and accurate, which is useful for the routine determination of Lansoprazole in tablet dosage form and in its pharmaceutical dosage forms.

To develop and validate simple, rapid, linear, accurate, precise and economical UV Spectroscopic method for estimation of Acebrophylline in tablet dosage form. The drug is freely soluble in analytical grade Ethanol. 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 analytical grade 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 acebrophylline in tablet dosage form and also validated as per ICH guidelines. The drug is freely soluble in analytical grade Ethanol, slightly soluble in methanol and water. So, the analytical grade Ethanol is used as a diluent in method. The melting point of acebrophylline was found to be 213-214ËšC (uncorrected). It showed absorption maxima 251 nm in analytical grade Ethanol. On the basis of absorption spectrum the working concentration was set on 10µg/ml (PPM). The linearity was observed between 2-18 μg/ml (PPM). The results of analysis were validated by recovery studies. The recovery was found to be 98.75, 101 and 99.17% for three levels respectively. The % RSD for precision was found to be 0.95%. A simple, rapid, linear, accurate, precise and economical UV Spectroscopic method has been developed for estimation of Acebrophylline in tablet dosage form. The method could be considered for the determination of Acebrophylline in quality control laboratories.

A new, simple, rapid, selective, precise and accurate isocratic reverse phase high performance liquid Chromatography assay method has been developed for simultaneous estimation of Isoniazid and Pyridoxine tablet formulations. The separation was achieved by using column Hypersil BDS, (250 x 4.6 mm, 5 µ) (Make: Thermo), in mobile phase consisted of pH4.0 phosphate buffer and Acetonitrile in the ratio of 75:25 v/v. The flow rate was 1.0 mL/min, column oven temperature 30° C, the injection volume was 10 μL, and detection was performed at 267 nm using a photodiode array detector (PDA), Run time 6 minutes. The retention time of Isoniazid and Pyridoxine, was noted to be 3.5 minutes and 4.3 minutes respectively, indicative of rather shorter analysis time. The method was validated as per ICH guidelines. The proposed method was found to be accurate, reproducible, and consistent.