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Dash R.N.,Alliance Institute of Advanced Pharmaceutical and Health science | Habibuddin M.,Adept Pharma and Bioscience Excellence Private Ltd | Sahoo A.,Alembic Research Center
Current Pharmaceutical Analysis | Year: 2013

This paper describes the development and validation of a most economical and sensitive isocratic stability indicating HPLC method for the assay of recombinant human insulin (RHI) from yeast origin (Hansenula polymorpha). The method employs a Thermo Biobasic, C-18 (250×4.6 mm, 300 A°, 5 μm) column with a mobile phase of acetonitrile potassium dihydrogen phosphate (pH 2.5; 50 mM) (35:65, v/v) and UV detection at 242 nm. Factorial design was used to facilitate method development. Buffer pH and concentration of acetonitrile were considered as the independent variable to study capacity factor of RHI. Sixteen experiments were undertaken, and a quadratic model was derived for the capacity factor of RHI. The method produced well defined, sharp peaks having lower tailing factor (1.114). A linear response with a correlation coefficient (r2) of 0.999 was observed over the range of 0.025 2.0 IU mL-1. Developed method was employed to analyze RHI samples from forced degradation and stability study. Degradation of RHI under different ICH prescribed stress conditions was carried out. Four batches of RHI formulation were exposed to different conditions of temperature and humidity for forty-five days. Degradation of RHI during stability study followed first-order kinetics. Data obtained from degradation kinetics were employed to find out the rate constant; time left for 50% potency, and time left for 90% potency. Rate constants obtained from different conditions were employed to plot the Arrhenius plot. © 2013 Bentham Science Publishers. Source


Sahu P.K.,Alliance Institute of Advanced Pharmaceutical and Health science | Sankar K.R.,Aurobindo Pharma Ltd | Annapurna M.M.,Roland Institute of Pharmaceutical science Khodasinghi
E-Journal of Chemistry | Year: 2011

An RP-HPLC analytical method for estimation of valdecoxib in human plasma was developed and validated. Protein precipitation and valdecoxib extraction from plasma (200 μL) was carried out by adding 800 μL perchloric acid (5%, v/v in water) containing nimesulide as the internal standard followed by vortex mixing and centrifugation. The supernatant (20 μL) was then injected onto an ODS C18 (25 cm×4.6 mm) column from Shimadzu. The mobile phase comprised of acetonitrile and water (35: 65) with a total run time of 12 min and the wavelength of the detector was set at 244 nm. The extraction recovery of valdecoxib from plasma was >95% and the calibration curve was linear (r 2 = 0.999) over valdecoxib concentrations ranging from 20 to 1400 μg/mL (n = 10). The method had an accuracy of >92% and LOD and LLOQ of 3.58 μg/mL and 13.45 μg/mL respectively. The method reported is simple, reliable, precise, accurate and has the capability of being used for determination of Valdecoxib in clinical settings. Source


Bhanu Teja B.,M s. TherDose Pharma Pvt. Ltd | Swaroop Kumar V.,M s. Incogen Therapeutics Ltd | Habibuddin M.,Alliance Institute of Advanced Pharmaceutical and Health science
Oriental Journal of Chemistry | Year: 2010

A simple and isocratic reverse phase high performance liquid chromatography (RP-HPLC) method was developed and validated for quantitative determination of Pemetrexed Disodium in bulk drug samples and formulations. The method was validated for system suitability, accuracy, precision, linearity, specificity, solution stability, limit of detection and limit of quantitation. Pemetrxed Disodium was analyzed by using Zorbax SB - C18 (250 mm × 4.6 mm, 5 μm) at ambient temperature, with isocratic elution of Buffer:Acetonitrile (90:10). The flow rate was set at 0.9 ml/min and the analysis was performed at a wavelength of 265 nm using Photo Diode Array (PDA) detector. Efficient UV detection at 265 nm enabled determination of Pemetrexed disodium without any interference from injectable solution excipients or solvents. The retention time (RT) for Pemetrexed disodium was around 6 min. The calibration curves were linear over a concentration range from 0.06248 mg to 0.49984 mg/ml. Limit of detection (LOD) for Pemetrexed disodium was 0.00002522 mg/ml and Limit of quantitation (LOQ) was 0.0001261 mg/ml. The developed method was successfully applied to estimate the amount of Pemetrexed disodium in formulations. Source


Dash R.N.,Alliance Institute of Advanced Pharmaceutical and Health science | Habibuddin M.,Adept Pharma and Bioscience Excellence Private Ltd | Humaira T.,Adept Pharma and Bioscience Excellence Private Ltd | Patel A.A.,King Khalid University
Journal of Liquid Chromatography and Related Technologies | Year: 2015

This paper describes the optimization of an isocratic stability indicating HPLC method for Ezetimibe (EZM). A five factor, three-level Box-Behnken experimental design optimized the method. The responses were (1) retention time, (2) tailing factor, and (3) theoretical plates. The quadratic effect of percentage (v/v) acetonitrile was the most significant (p < 0.001) factor to affect retention time and tailing factor, while interactions between percentage (v/v) acetonitrile and buffer pH had the most significant (p < 0.05) effect upon theoretical plates. The developed models for each response found to be well predictive bearing an acceptable adjusted correlation coefficient (0.9752 for retention time, 0.8557 for tailing factor, and 0.8336 for theoretical plates). The models were found to be significant (p < 0.001) having a high F value for each response (89.63 for retention time, 14.34 for tailing factor, and 12.27 for theoretical plates). The global desirability found to be 0.93 for the optimum chromatographic condition that achieved at a temperature of 35 ± 2°C using acetonitrile-potassium dihydrogen phosphate (pH 3.5; 20 mM) (45:55, v/v). The flow rate and injection volume kept at 0.8 mL min-1 and 20 L, respectively. The optimized chromatographic method subsequently applied to quantify EZM from a novel supersaturable self-nanoemulsifying formulation. © 2015 Taylor and Francis Group, LLC. Source


Ramesh D.,Alliance Institute of Advanced Pharmaceutical and Health science | Habibuddin M.,Adept Pharma and Bioscience Excellence Private Ltd
Current Pharmaceutical Analysis | Year: 2012

A novel liquid chromatographic-electrospray ionization mass spectrometric (LC-ESI-MS) method has been developed for the determination of Armodafinil in human plasma using carbamazepine as internal standard. The sample was prepared by employing liquid-liquid extraction method from human plasma using ethyl acetate as a solvent. The chromatographic separation was achieved within 3.0 min by using 0.2% formic acid: methanol (15:85) as mobile phase on hypurity advance C-18 column (5μ; 100 × 4.6 mm) at a flow rate of 1.0 ml/min. Ion signals m/z "274.1/167.3, 237.0/192.0" for armodafinil and internal standard respectively were measured in the positive ion mode. A detailed validation of the method was performed as per US-FDA guidelines (ICH Q2B). The results of all validation parameters were found to be within the acceptance limits. The drug concentration range from 50-10000 ng/mL was shown to be linear (r2 = 0.9989). Accuracy of the method was found to be >94%, and lower limit of quantification was found at 50 ng/mL. The extraction recoveries were found to be 70.6±0.96% and 67.7±1.32% for ARM and IS, respectively. The recoveries of the stability of sample at different conditions were found to be more than 95%. From the results, it is suggested that the proposed method is simple, reproducible, accurate and precise. So, this method can be applied for the future investigative studies of ARM in human plasma. © 2012 Bentham Science Publishers. Source

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