Pharmaceutical Methods最新文献

{"title":"A New Force Indicating RP-HPLC Method Development and Validation for the Simultaneous Estimation of Pibrentasvir and Glecaprevir in Bulk and its Tablet Dosage Form","authors":"D. Babu, C. Chetty, S. Mastanamma","doi":"10.5530/phm.2018.2.14","DOIUrl":"https://doi.org/10.5530/phm.2018.2.14","url":null,"abstract":"","PeriodicalId":19960,"journal":{"name":"Pharmaceutical Methods","volume":"158 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2018-08-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76347781","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Development and Validation of RP-HPLC Method for the Simultaneous Estimation of Lamivudine, Tenofovir Alafenamide and Dolutegravir Bulk and their Combined Dosage Form","authors":"Sk. Mastanamma, J. Jyothi, P. Saidulu, M. Varalakshmi","doi":"10.5530/PHM.2018.2.10","DOIUrl":"https://doi.org/10.5530/PHM.2018.2.10","url":null,"abstract":"Introduction: A simple and Rapid High Performance Liquid Chromatographic method was developed and validated for simultaneous estimation of lamivudine, tenofovir alafenamide and dolutegravir in their tablet dosage form. Method: The method was established using Agilent C18 (250 × 4.6 mm, i.d., 5 μm) column, a mobile phase consisting of 0.05M phosphate buffer pH 6.2 (solvent A) and acetonitrile (solvent B) 60:40 v/v at a flow rate of 1 mL/min with isocratic elution, injecting 10 μL sample into the chromatographic system. The eluted compounds were detected by using PDA Detector at a detection wavelength of 260 nm and the temperature was maintained at 30°C. Result: Retention times for the three compounds were found to be 3.09 min, 6.19 min and 9.61min for lamivudine, tenofovir alafenamide, and dolutegravir respectively. The linearity range was 10-80 μg/ml for three drugs with values of LOD found to be 0.56, 0.39μg, 1.35μg and LOQ were found to be 1.50μg, 0.99μg and 3.61 μg for lamivudine, tenofovir alafenamide and dolutegravir respectively which were linear enough showing correlation coefficient 0.999 in all the cases. Conclusion: The proposed method is therefore, suitable for the purpose in quality-control laboratories for quantitative analysis of the drugs individually and in the combined dosage form. The method was found to be as it is simple and rapid with tremendous precision and accuracy. The method can be used as a routine quality control method for triple combined dosage forms.","PeriodicalId":19960,"journal":{"name":"Pharmaceutical Methods","volume":"47 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2018-08-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"88571173","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"New Strategy for Solubilization and Refolding of Recombinant Human Interferon α2b Inclusion Bodies from E. coli Gene Overexpression System","authors":"C. Yon, Pak Yong-Ju, Song-Jin Yun","doi":"10.5530/phm.2018.2.15","DOIUrl":"https://doi.org/10.5530/phm.2018.2.15","url":null,"abstract":"Objective: New Strategy for solubilization and refolding of recombinant human Interferon α2b inclusion bodies was established to obtain a high solubilization and refolding rate of recombinant human Interferon α2b inclusion bodies from E. coli Gene Overexpression System.Method: The IFN-α2b inclusion bodies were solubilized with solubilizing buffer of 2mol/L urea. Refolding was performed via two steps, diluting by pulse adding the solubilized IFN α2b sample and dialysing it slowly using ultrafiltration 5K step by step. Finally refolded IFN α2b was purified through Cu2+ chelate affinity chromatography. Results: The urea concentration of 2mol/L in the solubilizing buffer gave the solubilization rate of 89.73%. Diluting the solubilized IFN α2b sample by pulse adding gave the refolding rate of 78.53%. The multi steps dialysis through ultrafiltration membrane 5K gave the antiviral activity recovery of 98.73%. The purification through one step Cu2+ chelate affinity chromatography raised the specific activity of IFN sample to 1.4×108U/mg protein and 12% SDS-PAGE showed single band of purified IFNα2b at expected MW height, whose purity was 99.8%. Conclusion: Large-scale production of recombinant human Interferon α2b (IFN-α2b) in E. coli with a thermoinducible overexpression system was established by applying an effective solubilizing and refolding processes of interferon α2b inclusion bodies (IBs). Solubilization and refolding rate of IFN-α2b IBs were 89.71% and 79.87% respectively. Refolded IFN-α2b was purified through one-step immobilized metal affinity chromatography to give a pure bioactive IFN-α2b with the specific activity of 1.4×108 IU/mg protein and with the recovery rate over 52.89%.","PeriodicalId":19960,"journal":{"name":"Pharmaceutical Methods","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2018-08-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78739362","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Science based Development of Viscous Eye Drop of Dorzolamide Hydrochloride and Timolol Maleate using Full Factorial Design","authors":"Purvi A. Shah, Niketa Ratilal Gevariya, J. Christian, K. Patel, V. Thakkar, M. Gohel, T. Gandhi","doi":"10.5530/PHM.2018.2.13","DOIUrl":"https://doi.org/10.5530/PHM.2018.2.13","url":null,"abstract":"","PeriodicalId":19960,"journal":{"name":"Pharmaceutical Methods","volume":"40 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2018-08-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"89226289","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Comparison of Analytical Spectrophotometric Methods for the Determination of Tetrabenazine in Tablets","authors":"K. P. Kumar, C. Swetha, J. Tejaswini, V. P. K. Reddy, D. Subramanyam, Chinnagollareddy Rupavani, Kothuru Renuka","doi":"10.5530/phm.2018.1.7","DOIUrl":"https://doi.org/10.5530/phm.2018.1.7","url":null,"abstract":"Background: Tetrabenazine was approved in the year of 2008 by USFDA. It was indicated mainly as an antipsychotic drug but now-a-days it is used for the treatment of hyperkinetic disorders. Objective: The objective of the study was to develop a simple and cost-effective spectrophotometric methods for the determination of tetrabenazine in tablets. Materials and Methods: The UV-Visible spectrophotometric studies carried out by Shimadzu UV 1800 with UV probe software and FT-IR studies using bruker alpha with opus software. The UV spectrum at 284 nm (Method A) and visible spectrum at 454 nm (Method B) are recorded. The FT-IR band of carbonyl group in tetrabenazine appeared at 1700 cm−1 with two-point baseline between 1650-1750 cm−1 (Method C). Results: Method A: The UV method was proved linear over the range of 10–50 μg/mL with correlation coefficient r2=0.9988 and mean recovery of 99.02% to 101.54%. Method B: The colorimetric method involves oxidative reaction of tetrabenazine and it yields green color chromogen. The linear concentrations over the range of 3-15 μg/mL with correlation coefficient of r2=0.9981 and mean recovery of 99.93% to 100.50%. Method C: The FT-IR method was showed linear over the range of 5-25 μg/mg, with correlation coefficient r2=0.9998 and mean recovery of 100.75% to 100.91%. The results of tetrabenazine tablets showed good agreement with their label claim. The results of ANOVA declare there was no significant difference between these spectrophotometric methods. Conclusion: Hence, these spectroscopic methods can be used for routine quality testing analysis of tetrabenazine in pharmaceutical laboratories.","PeriodicalId":19960,"journal":{"name":"Pharmaceutical Methods","volume":"6 1","pages":"34-39"},"PeriodicalIF":0.0,"publicationDate":"2017-10-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"85417064","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Novel RP-HPLC Method for the Determination of Paroxetine in Pure Form and in Tablet Formulation","authors":"Vijayalakshmi Marella, K. Lalitha, M. Pravallika, B. N. Nalluri","doi":"10.5530/PHM.2018.1.9","DOIUrl":"https://doi.org/10.5530/PHM.2018.1.9","url":null,"abstract":"Aim: To provide simple, rapid, reproducible reverse phase HPLC method for the estimation of paroxetine in pure form and tablet formulation. Method: The method is optimised using an inertsil column C18 (250x4.6 mm, 5μm) with the mobile phase consists of 10mM ammonium formate and acetonitrile in the ratio of 50:50v/v at an isocratic flow rate of 1ml/min. The detection is carried out at 220nm. Results: The calibration curve is linear in the concentration range of 5-25 μg/ml. The method is statistically validated for its linearity, precision, accuracy, stability and specificity as per ICH Q2R1 guidelines and the method is found to be robust. The LOD and LOQ values were found to be 0.748 and 2.62 μg/ml respectively. Conclusion: Hence the proposed method was found to be precise, accurate, LCMS compatible and can easily adaptable for quality control of paroxetine in dosage forms , biological fluids, dissolution studies.","PeriodicalId":19960,"journal":{"name":"Pharmaceutical Methods","volume":"17 1","pages":"45-48"},"PeriodicalIF":0.0,"publicationDate":"2017-10-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"82451214","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Simple and Economical UV Spectrophotometric Area under Curve Method for Estimation of Eletriptan Hydro bromide","authors":"Mahesh Deshpande, V. Kasture, M. Mohan","doi":"10.5530/PHM.2018.1.6","DOIUrl":"https://doi.org/10.5530/PHM.2018.1.6","url":null,"abstract":"Objective: Simple and economical area under curve method was developed and validated for the estimation of Eletriptan Hydrobromide. Method: The solvent implemented for estimation of Eletriptan Hydrobromide was water. The λmax was found to be 221 nm.The area under curve of UV spectrum between 216 to 226 nm. The method is validated according to ICH guideline Q2(R1). Results: The linearity range of Eletriptan HBr was found to be 5-25 μg/ml. The correlation coefficient was found to be 0.999. The values of %RSD for inter and intra-day precisions were within the acceptable limit. LOD and LOQ were found to be 5.77 μg/ml and 1.90 μg/ml respectively. % Recovery of Eletriptan HBr was 99.66 to 99.95.The values of ruggedness shows the method is rugged. Conclusion: The developed method can be implemented for routine analysis of Eletriptan HBr in bulk as well as formulation as per ICH Q2 (R1) guidelines.","PeriodicalId":19960,"journal":{"name":"Pharmaceutical Methods","volume":"4 1","pages":"30-33"},"PeriodicalIF":0.0,"publicationDate":"2017-10-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"88865451","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"RP-HPLC Forced Degradation Studies of Aztreonam in Pharmaceutical Dosage Form","authors":"V. Prakash, J. Suresh, Sarif Niroush Konari","doi":"10.5530/PHM.2018.1.8","DOIUrl":"https://doi.org/10.5530/PHM.2018.1.8","url":null,"abstract":"Introduction: Aztreonam belongs to the monobactam class of antibiotic used to treat infectious diseases produced by gram-negative bacteria. This work presents the development of LC methods for the estimation of Titled drug in pharmaceutical dosage form and forced degradation studies on four different stress conditions. Method: A waters HPLC Inspire (4.6 x 250mm, 5μm) in isocratic mode, with mobile phase containing buffer: Acetonitrile (40:60 %v/v) pH 3 adjusted with orthophosphoric acid were used. The flow rate was 1ml/min and linearity range was established at 525 μg/ml. Conclusion: Degradation studies disclose method abilities on various stress conditions. Forced degradation results can be used for the development of stable dosage form and for the designing of proper storage requirement. The proposed method is accurate, precise, specific and rapid for the estimation of aztreonam injection.","PeriodicalId":19960,"journal":{"name":"Pharmaceutical Methods","volume":"101 1","pages":"40-44"},"PeriodicalIF":0.0,"publicationDate":"2017-10-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"80402191","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"An Insight into the Analytical Techniques","authors":"R. Verma","doi":"10.5530/PHM.2018.1.1","DOIUrl":"https://doi.org/10.5530/PHM.2018.1.1","url":null,"abstract":"Pharmaceutical field is related to the discovery of novel molecules, their formulation for the treatment of disease, but the presence of impurities in pharmaceuticals may cause serious side effects and physical and chemical incompatibilities. Hence, the use of various analytical techniques reduces or eliminate the impurities at various levels of pharmaceuticals development. Here, some analytical techniques are given along with their advantages which are used in research as well as also at various steps of pharmaceuticals manufacturing.1 1. Titration: This analysis involves acid base titration, redox titration, precipitation titration, complexometric and non-aqueous titration. Application: a. Functional group analysis. b. Estimation of drugs. c. Analysis of degradation products of pharmaceuticals. Advantages: a. Saves time and labor. b. Precise. 2. Thin layer chromatography: It is a very simple, popular and basic technique which has a wide applicability. Application: a. Any impurity in drugs could be screened. b. Can be used for quantitative analytical methods. c. Provides information about degradation products of pharmaceuticals. Advantages: a. Less sample application is required and is cheap. b. Number of mobile phases can be selected. c. High amount of sample can be loaded. d. Sample distinction is possible.2 3. High performance thin layer chromatography (HPTLC): It is a very important separation technique which could be used for large number of samples. Application: Used for quantitative analysis of drugs such as alfuzosin and pentazocine. Advantages: a. Reduced time. b. Easy to handle. c. Number of parameters could be studied. c. Results are reliable. 4. High-performance liquid chromatography (HPLC): This is a very precise, accurate method of separating complex molecules mixture. Application: a. Useful in method development of Pharmaceutical drugs. b. To detect the contents of formulations. c. To estimate the drug content in biological fluids. d. To analyze the impurity in the sample.3 e. To analyze the degradation products. Advantage: DOI: 10.5530/phm.2018.1.1 Address for correspondence: Ruchi Verma, Manipal College of Pharmaceutical Sciences, Manipal University, Karnataka, INDIA. E-mail: ruchi.verma@manipal.edu a. Sensitive, reliable, precise method for analysis. 5. Gas Chromatography (GC): It is a very useful and accurate chromatographic technique for the analysis of volatile compounds. Application: a. Quantitative analysis of drugs, complex mixtures. b. Estimation of impurity in the samples. 6. UV visible spectroscopy: It is a very economical method which involves less manpower. This method is used to analyze pharmaceuticals which involves assay of drugs and estimation of active pharmaceutical constituent in formulation.4 7. Fluorimetry and phosphorimetry: These techniques utilize micro samples to test the formulation and biological samples. 8. Near Infrared spectroscopy (NIR) and Nuclear magnetic spectroscopy (NMR):NIR finds its applicat","PeriodicalId":19960,"journal":{"name":"Pharmaceutical Methods","volume":"7 1","pages":"01-01"},"PeriodicalIF":0.0,"publicationDate":"2017-10-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77109640","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Application of Box-Behnken Design for Validation of High-Performance Thin-Layer Chromatography/Densitometry Method for Robustness Determination of Apremilast in Bulk and in house Tablets","authors":"Suraj R. Chaudhari, A. Shirkhedkar","doi":"10.5530/PHM.2018.1.3","DOIUrl":"https://doi.org/10.5530/PHM.2018.1.3","url":null,"abstract":"Background: Apremilast is small molecule inhibitor of phosphodiesterase-4 (PDE-4) and an immunomodulating agent which is used for management of refractory psoriatic arthritis. Material and Methods: HighPerformance Thin-Layer Chromatography (HPTLC) method for the analysis of apremilast was developed and validated as per ICH guidelines. Apremilast was chromatographed on silica gel 60 F254 TLC plates using toluene: methanol (8:2 v/v) as a mobile phase. A Compact spot for apremilast was observed with Rf 0.64 ± 0.05, when the densitometric scanning was implemented at 230 nm. The linear regression analysis data for the calibration plots showed r2 > 0.99 with a concentration range from 250 – 1500 ng/band. ‘Design of Experiments’ (DoE) employing ‘Box-Behnken Design’ (BBD) and ‘Response Surface Methodology’ (RSM) were studied as an advancement to traditional ‘One Variable at Time’ (OVAT) approach to assess the effects of variations in selected factors particularly (development distance, saturation time, activation time of plate and mobile phase ratio) as graphical interpretation for robustness. The statistical insight was achieved with Multiple Linear Regression (MLR) and ANOVA. Results: The method was validated for precision, accuracy, detection limit and quantitation limit, and robustness. Conclusion: The method was successfully employed for the determination of apremilast from its in-house tablet formulation.","PeriodicalId":19960,"journal":{"name":"Pharmaceutical Methods","volume":"1 1","pages":"09-15"},"PeriodicalIF":0.0,"publicationDate":"2017-10-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"88236987","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}