Objective: The aim of the research work to develop a simple, sensitive, rugged, robust and specific novel gradient stability indicating reverse phase HPLC method for quantitative determination of known and unknown impurities profiling of Carvedilol pharmaceutical dosage forms (Tablets). Methods: Chromatographic separation has been achieved on an Inertsil ODS 3V column (150 mm x 4.6 mm, 5μm) with mobile phase consisting Mobile phase-A (Water, Acetonitrile and Trifluroacetic acid in the ratio of 80:20:0.1 v/v/v respectively and pH adjusted to 2.0 with dilute potassium hydroxide solution) and Mobile phase-B (Water and acetonitrile in the ratio of 100:900 v/v respectively) delivered at flow rate of 1.0 ml min-1 and the detection wavelength 240 nm. The column compartment temperature maintained at 40 °C. Results: Resolution between Carvedilol and its impurities has been achieved greater than 1.5. The developed method was validated as per ICH guidelines. Analytical method found Precise, Linear, accurate, specific, rugged and robust. Conclusion: Developed and validated novel analytical method can be used to for impurity profile analysis of Carvedilol Pharmaceutical dosage form (Tablets).

The main objective of this research work was to develop and validate, a new gradient, highly sensitive, specific and stability indicating Reverse Phase HPLC method for quantitative determination of known, unknown impurities and degradant impurities profiling for Cholecalciferol tablets. No Pharmacopoeial method is available to quantify known, unknown impurities and degradants profiling for Cholecalciferol tablets. The impurities were separated on the Hypersil BDS column (150 mm x 4.6mm, 3µm) with a mobile phase of mixture of Trifluoroacetic acid buffer and acetonitrile with flow rate of 1.5 mL minute -1. The column compartment was maintained at 40°C and the detection wavelength was at 265nm. Cholecalciferol, its known impurity and unknown impurities have been well resolved from each other. Recovery of the known and unknown impurities found between 80% to 120% as per ICH guideline. Method found linearity over the working concentration range with acceptance criteria of correlation coefficient greater than 0.99. Method precision and intermediate precision results found with percentage relative standard deviation of impurity content less than 10% for replicated analysis of test samples. A stress study was conducted with a drug product that was exposed to different conditions of acid, base, oxidation, heat, humidity and photolytic degradation. Cholecalciferol was found to degrade significantly under Photolytic, Thermal and Alkaline stress conditions. The degradation products were well resolved from Cholecalciferol and its impurities. For each stress condition, peak purity of Cholecalciferol was assessed using the Photodiode Array detector and found homogeneous in nature. The mass balance for stress study was found in between 95% and 105%. Thus, proving the stability indicating nature of the analytical method. The developed method was validated as per ICH guidelines. The method found accurate, precise, linear, robust, rugged, specific and stability indicating in nature.

Background A novel gradient, high-sensitive and specific stability-indicating reverse-phase HPLC method was developed and validated for quantitative purpose of known, unknown and degradant impurities profiling for diltiazem hydrochloride tablets. The impurities were separated on the Zorbax RX C8 column (150 mm × 4.6 mm, 5 μm) with mobile phase-A consisting of a mixture of 0.05 M sodium dihydrogen phosphate monohydrate buffer pH 3.0 and methanol in the ratio 800:200v/v and mobile phase-B consisting of acetonitrile with a flow rate of 1.0 mL min−1. The column compartment was maintained at 35 °C, and the detection wavelength was 240 nm. Diltiazem hydrochloride, its known impurities and unknown impurities have been well resolved from each other. Results The linearity of the method has been demonstrated across the concentration range of 0.18 to 5.65 µg mL−1 for EP impurity-F with correlation coefficient R2 greater than 0.99. Recovery of method was proved from LOQ to 150% for known and unknown impurities with respect to test concentration and found in between 80 and 120%. Forced degradation study and specificity experiment results with mass balance proved the stability-indicating nature of the method and separated all known, unknown impurities and degradants from each other as well as from main drug component (diltiazem hydrochloride). The mass balance for stress study was found in between 95 and 105%. Conclusion Newly developed analytical method was validated as per ICH Q2 (R1) guidelines “Validation of analytical procedure” and found linear, accurate, specific, robust and precise in the established working range.

Objective: The aim of the research work to monitor impurities profiling and degradation kinetics of Carvedilol Pharmaceutical Dosage Form (Tablets) through stress degradation study. Methods: To study impurity profiling and degradation kinetics Chromatographic condition used as, Inertsil ODS 3V column (150 mm x 4.6 mm, 5μm) with mobile phase consisting Mobile phase-A (Water, Acetonitrile and Trifluroacetic acid in the ratio of 80:20:0.1 v/v/v respectively and pH adjusted to 2.0 with dilute potassium hydroxide solution) and Mobile phase-B (Water and acetonitrile in the ratio of 100:900 v/v respectively) delivered at flow rate of 1.0 ml min-1 and the detection wavelength 240 nm. The column compartment temperature maintained at 40 °C. Results: Stress degradation study conducted using Acid, Alkali, Oxidation, Humidity, Thermal and Photolytic stress degradation conditions. Known, unknown and degradant impurities nature and degradation kinetics in different stressed degradation conditions were monitored through stability indicated method reverse phase HPLC method. Carvedilol molecule found sensitive to Oxidation and Alkali conditions. Impurity-A significantly increased from its not detected level. Carvedilol molecule found stable in Acid, Humidity, Thermal and Photolytic stress degradation condition. In all stressed conditions, mass balance was found between 95% to 105% and peak purity of carvedilol peak was found pure. Conclusion: Stress degradation study is required to know the degradation pathway of product and to prove the stability indicating nature of the analytical method. Study provide information pertaining to the intrinsic stability of drug product.

: Surfactants enhances complexation of triphenylmethane dyes by formation of a new dye : surfactant complex which is as an intermediate stable complex. Addition of quaternary salts of surfactants to the deeply colored solution of dyes causes a marked change in its λmax. The absorption spectra of Eriochrome AzurolB ,EAB; a triphenylmethane dye , has been studied in the presence as well as in the absence of sodium lauryl sulphate, SLS . At different pH values ranging from pH 1.00 to 12.00, the spectra is studied.Hypsochromic shift is observed in the absorption spectra in the presence of surfactant. Dissociation constant has been evaluated both in the presence and absence of surfactant. Decrease in the values of dissociation constant, pK values in the presence of surfactant is observed which indicated formation of water soluble, stable, dye-surfactant complex. Composition of stable dyesurfactant complex is determined and effect of foreign ions such as Chlorides i.eNaCl, KCl, NH 4 Cl; the nitrates i.e KNO 3 , NaNO 3 , NH 4 NO 3; andsulphatesi.e K 2 SO 4, ,Na 2 SO 4 and (NH 4 ) 2 SO 4 has been studied in detail. It is found out that the Binary submicellar aggregates can be proposed as the active species in ternary complex formation with metal ions and hence can be termed as modified reagents, as EAB-SLS.