Stability indicating

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.

A simple, precise and accurate stability indicating RP-HPLC method has been developed and subsequently validated for the simultaneous estimation of Sildenafil citrate and Estradiol valerate in bulk and pharmaceutical formulation. The separation was carried out using C18 column (150mm x 4.6mm, 5μm), mixture of acetonitrile and water 80:20 % v/v as a mobile phase with a flow rate of 1 ml/min and the effluent was monitored at 290 nm using PDA detector. The retention time of Sildenafil citrate and Estradiol valerate were 2.55 min and 5.56 min respectively. The method is linear over the range of 125 - 750 μg/ml and 5 - 30 μg/ml for Sildenafil citrate and Estradiol valerate respectively. The method was found to be precise, accurate and specific during the study. The percentage assay was found to be 100.68 % and 99.58 % for Sildenafil citrate and Estradiol valerate respectively from the tablet formulation. Sildenafil citrate and Estradiol valerate were subjected to stress condition to check the degradation behaviour of them. The drugs undergo degradation under acidic, basic, oxidative and thermal condition. The proposed method enables rapid quantification and simultaneous analysis of both drugs from commercial formulations without any interference of excipients. So, the method can be used for routine analysis of Sildenafil citrate and Estradiol valerate in combined tablet formulation.

A simple, precise, accurate, simultaneous and stability-indicating HPLC method developed with an effective resolution of active pharmaceutical ingredients. The present method effectively separates all the related substances of Diphenhydramine hydrochloride and acetaminophen along with impurities. Chromatographic separation has been obtained on Inertsil C18 (250 X 4.6mm, 5µ) column using a gradient elution with a mixture of phosphate buffer pH3.0 and acetonitrile. At 220 nm compounds will be eluted and monitored. Diphenhydramine hydrochloride and acetaminophen were subjected to the stress conditions of acid, base, peroxide, thermal, photolytic, humidity and water degradation. The degradation products were well resolved from main peak and its impurities, proving the stability-indicating ability of the method. The developed method was validated as per International Conference on Harmonization (ICH) guidelines and validation acceptance criteria were met in all cases. The current method has proven good linearity and accuracy over the range of all known impurities from LOQ to 150% of the target concentration. The degree of reproducibility, as results obtained by deliberate changes in the method parameter and variety of condition has proven that the method is robust and rugged.

A sensitive and selective RP-HPLC method is described for the determination of stability in Acetaminophen and Tramadol dosage forms. Chromatographic separation was achieved on a C18 column using mobile phase consisting of a mixture of mixed Phosphate buffer pH: 3.4 Acetonitrile (30:70v/v/v), with detection of 236nm and flow rate at 1mL/min. Linearity was observed in the range 100-300 µg /ml for Acetaminophen (r2 =0.994) & 10-30µg /ml for Tramadol (r2 =0.994) for the amount of drugs estimated by the proposed methods was in good agreement with the label claim. No chromatographic interference from tablet excipients was found. The proposed methods were validated. The force degradation of the drugs was assessed by different environmental conditions. Recovery experiments indicated the absence of interference from commonly encountered pharmaceutical additives. The method was found to be precise as indicated by the repeatability analysis, showing %RSD less than 2. All statistical data proves validity of the methods and can be used for routine analysis of pharmaceutical dosage form.

A novel, simple, rapid and stability-indicating reversed-phase ultra performance liquid chromatographic and mass spectrometric method was developed and subsequently validated for quantitation of Efavirenz (EFV) from drug substance matrix. The separation was achieved in 2.5 minutes on Waters ACQUITY UPLC BEH C18 (50 x 2.1) mm, 1.7µm column in isocratic mode with flow rate 0.4 mL/min. Mobile phase used was 0.01 M ammonium acetate buffer pH 7.5 and acetonitrile in ratio 50:50 v/v. Detection was carried out at the maximum wavelength of 247 nm using a photodiode array detector. The retention time of Efavirenz was found 1.8 minutes. Specificity of the method was established on drug substance by hydrolytic and oxidative stress conditions. Validation of analytical method was carried out as per the current ICH guidelines for linearity, recovery, precision, limit of detection, limit of quantification and robustness parameters.

Terbinafine hydrochloride (TFH), is a potent antifungal agent of the allylamine class with broad spectrum activity against yeasts, dimorphic fungi, molds, and dermatophytes. A new, simple, rapid, selective, precise, accurate, and stability indicating high performance liquid chromatographic method has been developed for the determination of terbinafine hydrochloride (TFH) in pharmaceuticals. The assay was performed using an Zorbax Eclips XDB C-18 (3.5 µm, 4.6 × 150 mm i.d.,) column at 30ºC temperature with UV-detection at 222 nm. A mobile phase consisting of buffer (1000 mL water, 2 mL triethylamine, pH 3.4 adjusted with trifluoroacetic acid.), isopropyl alcohol and methanol (40:12:48, v/v/v), was used in the assay at a flow rate of 1 mL min-1. The method was validated and system suitability parameters were investigated. An excellent linearity was obtained over the concentration range 1 - 80 μg mL-1 TFH with limits of detection (LOD) and quantification (LOQ) values of 0.3 and 1.0 mg mL-1, respectively. The proposed method were applied successfully to the determination of TFH in tablets. The results obtained were in good agreement with those obtained by a reference method, with high precision and without any detectable interference from tablets excipients. The validity and reliability of the proposed methods were further assessed by the recovery studies via a standard addition method. In addition, forced degradation of TFH was conducted in accordance with the ICH guidelines. Acidic, basic water hydrolysis, thermal stress, peroxide and photolytic degradation were used to assess the stability indicating power of the method. Slight degradation was observed during oxidative degradation and no degradation was observed under other stress conditions.

A novel stability indicating RP-HPLC method was developed for simultaneous estimation of Ethylhexyl triazone and Bemotrizinol in sun care formulations. Separation of Ethylhexyl triazone, Bemotrizinol and their degradation products was achieved on Waters symmetry C18 (150 × 3.9 mm, 5µ) as stationary phase and mixture of pH 4.50 ammonium formate buffer and 1,4-dioxane (20:80, v/v) as mobile phase. Both analytes were simultaneously measured at UV detection of 311 nm. Method was validated for specificity, method precision (Intra-day and inter-day), linearity, accuracy and robustness as per ICH guideline. Ethylhexyl triazone and Bemotrizinol were linear in the concentration range of 0.10-225 µg/mL and 0.12-225 µg/mL respectively with correlation coefficient of > 0.999. This method can be utilized in cosmetic industries to monitor both analytes in sun care formulations to assure the quality of the products.

This study is aimed at Developing and validating an UPLC method for Bosentan and its related substances that might coexist in bulk drugs and its tablet formulations as impurities that may originate from synthesis process or degradation. A chromatographic system consisting Waters Acquity UPLC HSS PFP, 2.1x 50mm (2.5 µm) column, mobile phase of 0.02M KH2PO4with pH 2.0 as Buffer phase and Acetonitrile: Methanol in 1:1 ratio as organic phase, with gradient elution at flow of 0.6 mL/min and UV detector set at 220 nm has shown a good chromatographic separation for Bosentan and its related substances. The developed method was validated as per ICH Guidelines and shown equivalency with API Vendor method. The developed UPLC method has run time of only 13 minutes making the method productive and may be applied for Quality control Testing.

This study is aimed at Developing and validating an UPLC method for Sildenafil citrate, Bosentan and its related substances that might coexist in bulk drugs and its tablet formulations as impurities that may originate from synthesis process or degradation. A chromatographic system consisting Waters Acquity UPLC HSS PFP, 2.1x 50mm (2.5 µm) column, mobile phase of 0.02M KH2PO4with pH 2.0 as Buffer phase and Acetonitrile: Methanol in 1:1 ratio as organic phase, with gradient elution at flow of 0.4 mL/min and UV detector set at 220 nm has shown a good chromatographic separation for sildenafil citrate, Bosentan and its related substances. The developed method was validated as per ICH Guidelines. The developed UPLC method has run time of only 20 minutes making the method productive and may be applied for Quality control Testing.

This study is aimed at Developing and validating an UPLC method for determination of Sildenafil and tadalafil content in API and formulations. A chromatographic system consisting Waters  Acquity UPLC BEH C8(1.8 µm)column, mobile phase of  0.2 M ammonium acetate and Acetonitrile with gradient elution at flow of 0.3 mL/min and UV detector set at 245 nm has shown a good chromatographic separation for Sildenafil tadalafil. The developed method was validated as per ICH Guidelines, the developed UPLC method has run time of only 10 minutes making the method productive and tested by spiking all the impurities of sildenafil and tadalafil. It may be applied for Quality control Testing.