scholarly journals DEVELOPMENT AND VALIDATION OF STABILITY INDICATING CHROMATOGRAPHIC METHOD FOR SIMULTANEOUS ESTIMATION OF SACUBITRIL AND VALSARTAN IN PHARMACEUTICAL DOSAGE FORM

2017 ◽  
Vol 9 (5) ◽  
pp. 1
Author(s):  
Shweta Mishra ◽  
C. J. Patel ◽  
M. M. Patel
Keyword(s):  
Dosage Form ◽  
Degradation Products ◽  
Potassium Phosphate ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Development And Validation ◽  
Tablet Dosage

Objective: This study aims to develop and validate a stability indicating HPLC method for simultaneous estimation of sacubitril and valsartan in pharmaceutical dosage form.Methods: Sacubitril and valsartan separation were achieved by LC-20 AT C18 (250 mm x 4.6 mm) column and buffer (potassium phosphate, pH 3.0): methanol (50:50) as mobile phase, at a flow rate of 1 ml/min (millilitre per minute). Detection was carried out at 224 nm (nanometer). The different HPLC experimental parameters were optimized and the method was validated according to the standard guideline. Forced degradation experiments were carried out by exposing sacubitril and valsartan standard and sample for thermal, photolytic, oxidative and acid-base hydrolytic stress conditions.Results: Retention time of sacubitril and valsartan were found to be 4.170 min (minute) and 6.530 min (minute) respectively. The method has been validated for linearity, accuracy, precision, LOD, and LOQ. Linearity observed for sacubitril is 12.25-36.75 μg/ml (microgram per milliliter) and for valsartan is 12.75-38.25 μg/ml (microgram per milliliter). The results showed that sacubitril and valsartan and the other degradation products were fully resolved and thus the proposed method is stability-indicating.Conclusion: The proposed HPLC method was found to be simple, specific, precise, accurate, rapid and economical for simultaneous estimation of valsartan and sacubitril in bulk and tablet dosage form. Thus the validated economical method was applied for forced degradation study of sacubitril and valsartan tablet.

scholarly journals Validation of a Stability-Indicating RP-HPLC Method for the Determination of Entecavir in Tablet Dosage Form

2010 ◽  
Vol 93 (2) ◽  
pp. 523-530 ◽  
Author(s):  
Sérgio Luiz Dalmora ◽  
Maximiliano da Silva Sangoi ◽  
Daniele Rubert Nogueira ◽  
Lucélia Magalhães da Silva
Keyword(s):  
Dosage Form ◽  
Potassium Phosphate ◽  
Hplc Method ◽  
Forced Degradation ◽  
Photodiode Array Detection ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Forced Degradation Studies ◽  
Tablet Dosage

Abstract An RP-HPLC method was validated for the determination of entecavir in tablet dosage form. The HPLC method was carried out on a Gemini C18 column (150 4.6 mm id) maintained at 30C. The mobile phase consisted of acetonitrilewater (95 + 5, v/v)/potassium phosphate buffer (0.01 M, pH 4; 9 + 91, v/v) pumped at a flow rate of 1.0 mL/min. Photodiode array detection was at 253 nm. The chromatographic separation was obtained with a retention time of 4.18 min, and the method was linear in the range of 0.5200 g/mL (r2 0.9998). The specificity and stability-indicating capability of the method was proven through forced degradation studies, which also showed that there was no interference of the excipients and an increase of the cytotoxicity only by the basic condition. The accuracy was 101.19, with bias lower than 1.81. The LOD and LOQ were 0.39 and 0.5 g/mL, respectively. Method validation demonstrated acceptable results for precision and robustness. The proposed method was applied for the analysis of tablet formulations, to improve QC and assure therapeutic efficacy.

scholarly journals Stability indicating RP-HPLC method development and validation for the simultaneous estimation of Grazoprevir and Elbasvir in bulk and pharmaceutical dosage form

2018 ◽  
Vol 1 (1) ◽  
pp. 1-7
Author(s):  
V. Pavan Kumar ◽  
A. Vijaya Kumar ◽  
B Sivagami ◽  
R. Charan Kumar ◽  
M. Niranjan Babu
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Regression Equations ◽  
Pharmaceutical Dosage Form ◽  
Potassium Hydrogen ◽  
Hplc Method Development ◽  
Development And Validation ◽  
Tablet Dosage

A simple, Accurate and precise method was developed for the simultaneous estimation of the Grazoprevir and Elbasvir in Tablet dosage form. Chromatogram was run through Kromosil C18 (250 x 4.6 mm), 5m. Mobile phase containing Buffer: Acetonitrile taken in the ratio 45:55 was pumped through column at a flow rate of 1 ml/min. Buffer used in this method was Di Potassium Hydrogen ortho Phosphate. Temperature was maintained at 30°C. Optimized wavelength selected was 215 nm. Retention time of Elbasvir and Grazoprevir and were found to be 2.503 min and 3.004. %RSD of the Elbasvir and Grazoprevir were and found to be 0.3 and 0.4 respectively. %Recovery was obtained as 98.17% and 99.83% for Grazoprevir and Elbasvir respectively. LOD, LOQ values obtained from regression equations of Grazoprevir and Elbasvir were 0.24, 0.73 and 0.06, 0.19 respectively. Retention times were decreased and run time was decreased, so the method developed was simple and economical that can be adopted in regular Quality control test in Industries.

scholarly journals Development of Stability Indicating RP-HPLC Method for Simultaneous Estimation of Amlodipine and Olmesartan in Pure and Pharmaceutical Dosage Form

2018 ◽  
Vol 10 (05) ◽  
Author(s):  
Dhiraj Kumar ◽  
Susanta Kumar Panda ◽  
Sudhir Kumar Sahoo
Keyword(s):  
Dosage Form ◽  
Degradation Products ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Standard Curve ◽  
Stress Studies ◽  
Rp Hplc ◽  
Limit Of Quantitation

A precise, accurate, economical and simple stability indicating RP-HPLC method was developed for the estimation of Amlodipine (AML) and Olmesartan (OLM) in bulk and pharmaceutical dosage form. Method was performed on a octadecyl silane column with dimensions 4.6 x 250 mm having particle size 5 micron. The mobile phase used in the method is TEA Buffer (pH 3.0) and acetonitrile in proportion of 25:75 respectively. The flow rate was maintained at 1.0 ml/ min and effluent was monitored at 258 nm. The drug was subjected to acid and alkali hydrolysis, oxidation, photolysis and heat as stress conditions. The method was validated for specificity, linearity, precision, accuracy, robustness and system suitability. The retention times were observed at 2.39 min and 3.33 min for AML and OLM respectively. The standard curve was found linear over a range of 05–35 μg/ml for AML and OLM. Similarly an average correlation coefficient was also obtained at 0.999 for AML and OLM. The limit of quantitation (LOQ) of this method was 2μg/ml for Amlodipine and Olmesartan. The absolute recovery was 100% for Amlodipine and 100.3 for Olmesartan. Degradation products produced as a result of stress studies did not interfere with the detection of AML and OLM and the assay can thus be considered stability-indicating.

scholarly journals Development and validation of stability-indicating RP-UPLC method for simultaneous estimation of thiocolchicoside and aceclofenac in combined dosage form

2014 ◽  
Vol 3 (7) ◽  
pp. 296-300 ◽  
Author(s):  
Paramasivam Balan ◽  
Nagappan Kannappan
Keyword(s):  
Dosage Form ◽  
Pharmaceutical Journal ◽  
Detector Response ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Stability Indicating ◽  
The Stability ◽  
Development And Validation ◽  
Tablet Dosage

A stability indicating RP-UPLC method was developed and validated for the simultaneous determination of Thiocolchicoside (TCC) and Aceclofenac (ACF) in tablet dosage form. The chromatographic separation was carried out by Thermo Scientific UPLC Instrument, Accela 1250 Pump, auto sampler with PDA detector, using column Thermo Scientific hypersil gold C18, (50 x 2.1mm) particle size 1.9µm using 5% ammonium acetate buffer and methanol in the ratio of 40:60, pH was adjusted to 5 with ortho phosphoric acid as mobile phase at a flow rate of 250 µl/min with the detection at 276nm. The run times of the TCC and ACF were about 0.697 and 1.125 minutes, respectively. The detector response is linear from 4.8 µg/ml to 7.2 µg/ml and 63.8 µg/ml to 96 µg/ml concentrations for TCC and ACF respectively. The linear regression equation was found to be y = 20620x-677.68 (r2 = 0.9996) for TCC and y= 50931x-319.3 (r2 = 0.9997) for ACF. The detection limit and quantification limit was 0.076µg and 0.23µg for TCC and 0.27µg and 0.71µg for ACF. The percentage of assay of TCC and ACF were about 99.50% and 99.96% respectively. The stability indicating capability was established by forced degradation experiments. The method was satisfactorily validated as per the ICH guidelines.DOI: http://dx.doi.org/10.3329/icpj.v3i7.19078 International Current Pharmaceutical Journal, June 2014, 3(7): 296-300

scholarly journals Development of Stability Indicating RP-HPLC Method for Ertapenem in Bulk Drug and Pharmaceutical Dosage Form

2017 ◽  
Vol 16 (1) ◽  
pp. 21-28
Author(s):  
Ruchi Jain ◽  
Nilesh Jain ◽  
Deepak Kumar Jain ◽  
Avineesh Singh ◽  
Surendra Kumar Jain
Keyword(s):  
Dosage Form ◽  
Degradation Products ◽  
Hplc Method ◽  
Stress Conditions ◽  
Assay Method ◽  
Main Peak ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Bulk Drug

A simple, inexpensive, rapid and novel stability indicating isocratic HPLC method has been developed and validated for quantitative analysis of ertapenem sodium in the bulk drug and in pharmaceutical dosage form. An isocratic separation of ertapenem sodium was achieved on Hypersil BDS C18 column (4.6 x 250 mm, 5 ? particle size) as the stationary phase with a flow rate of 1.2 ml/min and using a UV detector to monitor the eluate at 298 nm. The mobile phase consisted of acetonitrile : water (60:40v/v) and pH adjusted 2.9 by othophosphoric acid enabled separation of the drug from its degradation products. The method was validated for linearity, accuracy (recovery), precision, specificity and robustness. The linearity of the method was satisfactory over the range 2-10 ?g/ml (correlation coefficient 0.999). Recovery of ertapenem sodium from the pharmaceutical dosage form ranged from 99.97 to 103.7%. Ertapenem sodium was subjected to stress conditions [hydrolysis (acid, base), oxidation, photolysis and thermal degradation] and the samples were analyzed by this method. The forceddegradation study with ertapenem sodium showed that it was degraded under basic condition. The drug was stable under the other stress conditions investigated. Ertapenem sodium was found to be less stable in solution state, whereas it was comparatively much stable in solid state. The degradation products were well resolved from main peak. The forced degradation study prove the stability indicating power of the method and therefore, the validated method may be useful for routine analysis of ertapenem sodium as bulk drug, in respective dosage forms, for dissolution studies and as stability indicating assay method in pharmaceutical laboratories and industries.Dhaka Univ. J. Pharm. Sci. 16(1): 21-28, 2017 (June)

scholarly journals Stability-Indicating RP-HPLC Method for Simultaneous Estimation of Enrofloxacin and Its Degradation Products in Tablet Dosage Forms

2015 ◽  
Vol 2015 ◽  
pp. 1-11 ◽  
Author(s):  
V. Ashok Chakravarthy ◽  
B. B. V. Sailaja ◽  
Avvaru Praveen Kumar
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Dosage Forms ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Column Temperature ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Tablet Dosage

The present work was the development of a simple, efficient, and reproducible stability-indicating reverse-phase high performance liquid chromatographic (RP-HPLC) method for simultaneous determination enrofloxacin (EFX) and its degradation products including ethylenediamine impurity, desfluoro impurity, ciprofloxacin impurity, chloro impurity, fluoroquinolonic acid impurity, and decarboxylated impurity in tablet dosage forms. The separation of EFX and its degradation products in tablets was carried out on Kromasil C-18(250×4.6 mm, 5 μm) column using 0.1% (v/v) TEA in 10 mM KH2PO4(pH 2.5) buffer and methanol by linear gradient program. Flow rate was 1.0 mL min−1with a column temperature of 35°C and detection wavelength was carried out at 278 nm and 254 nm. The forced degradation studies were performed on EFX tablets under acidic, basic, oxidation, thermal, humidity, and photolytic conditions. The degraded products were well resolved from the main active drug and also from known impurities within 65 minutes. The method was validated in terms of specificity, linearity, LOD, LOQ, accuracy, precision, and robustness as per ICH guidelines. The results obtained from the validation experiments prove that the developed method is a stability-indicating method and suitable for routine analysis.

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