VALIDATED STABILITY INDICATING UPLC METHOD FOR AFATINIB AND ITS IMPURITIES IN PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2021 ◽  
Vol 57 (11) ◽  
pp. 27-39
Author(s):  
Ramu Ivaturi ◽  
Sastry T Manikya ◽  
Satyaveni S
Keyword(s):  
Dosage Form ◽  
Forced Degradation ◽  
Good Resolution ◽  
Mobile Phase Flow Rate ◽  
Pharmaceutical Dosage Form ◽  
Column Temperature ◽  
Stability Indicating ◽  
Related Impurities ◽  
Short Run ◽  
Run Time

A novel, simple, selective, rapid stability-indicating and LC-MS compatible short run time UPLC method was developed and validated for the determination of afatinib and its related substances in bulk and finished dosage form. A reverse phase gradient mode short run time method has been developed by using UPLC to separate all the five known impurities of Afatinib. The chromatographic separation of afatinib and its related impurities was achieved by using Acquity UPLC HSS PFP column 100*2.1 mm, 1.8 μm using 0.1% v/v formic acid in Milli-Q water and acetonitrile as a co-solvent with a run time of 12 minutes. The column temperature was maintained at 30°C. The mobile phase flow rate was 0.4 mL/min and the UV detection was carried out at a wavelength of 258 nm. The proposed method was validated in terms of specificity (forced degradation), linearity, accuracy, precision, robustness and ruggedness as per ICH quality guidelines Q2 (R1). Forced degradation was performed using hydrolysis, oxidation, thermal and photolytic conditions with good resolution between degradants and analyte. Degradation peaks neither co-elute with the main analyte nor with the known impurities, indicating that the proposed method as is stability indicating. Limit of quantification for all the five known impurities and analyte were in the range of 0.02 ppm to 0.05 ppm, indicating that the method is sensitive. Recovery of the impurities and analyte at various levels ranging from LOQ level to 200% level was in the range of 96.9 to 101.8%, indicating that the method was accurate and precise. Hence the validated method can be successfully applied for the quantitative estimation of afatinib and its related impurities in bulk and tablet dosage form.

HPLC METHOD DEVELOPMENT, VALIDATION, AND FORCED DEGRADATION FOR SIMULTANEOUS ANALYSIS OF OXYCODONE AND NALTREXONEIN PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (02) ◽  
pp. 31-38
Author(s):  
R. S. Ch Phani ◽  
◽  
K. R. S. Prasad ◽  
R. M Useni
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Hplc Method ◽  
Forced Degradation ◽  
Solution Stability ◽  
Pharmaceutical Dosage Form ◽  
Column Temperature ◽  
Degradation Study ◽  
Ich Guidelines ◽  
Hplc Method Development

A simple, precise and stability-indicating RP-HPLC method was developed for simultaneous quantification of oxycodone (OXCD) and naltrexone (NTRX) in combined dosage form. The developed method was validated with respect to precision, linearity, accuracy, robustness, ruggedness, sensitivity and solution stability. The method was developed with ammonium di hydrogen phosphate buffer (pH 5.0) and acetonitrile in a ratio of 55:45 (v/v) as mobile phase at a flow rate of 1.0 mL/minute over Intersil ODS C18 column (250 mm × 4.6 mm×5μ).The UV detection wavelength was fixed at 235 nm. The column temperature was maintained at ambient temperature. The method showed good linearity with correlation coefficient values of 0.9990 and 0.9994 for OXCD and NTRX. The percent recoveries of the two drugs found within the limits of 98.0–102.0%. The LOQ concentrations of OXCD and NTRX are 0.625 μg/ mL and 0.075 μg/mL, respectively. The LOD concentrations of OXCD and NTRX are 0.3125 μg/mL and 0.0375 μg/mL, respectively. According to ICH guidelines forced degradation study was validated.

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 NEW STABILITY-INDICATING ULTRA PERFORMANCE LIQUID CHROMATOGRAPHY METHOD DEVELOPMENT AND VALIDATION OF LENVATINIB MESYLATE IN BULK DRUG AND PHARMACEUTICAL DOSAGE FORMS

2018 ◽  
Vol 11 (9) ◽  
pp. 140
Author(s):  
Jahnavi Bandla ◽  
S. Ganapaty
Keyword(s):  
Liquid Chromatography ◽  
Dosage Form ◽  
Ultra Performance Liquid Chromatography ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Relative Standard ◽  
Validation Parameters ◽  
Bulk Drug

Objective: The objective of the present study was to develop and validate a new stability-indicating method for the quantification of lenvatinib mesylate in bulk drug and pharmaceutical dosage form using ultra performance liquid chromatography (UPLC).Methods: The optimized chromatographic conditions for elution of drug included UPLC HSS C18 (100 mm × 2.1 mm, 1.8 m) column, mixture of 0.1% orthophosphoric acid and acetonitrile (50:50 v/v%) mobile phase run on an isocratic mode at a flow rate of 0.3 mL/min, 240 nm detection wavelength, and column oven temperature maintained at 30°C.Results: The retention time for lenvatinib was found to be 1.24 min. The developed method was validated for various validation parameters in accordance with the International Conference on Harmonization guidelines. The method obeyed Beer’s law in the concentration range of 2.5– 15 μg/mL with a correlation coefficient of 0.9996. The percentage relative standard deviation and percentage recovery were determined to be 0.4 and 99.66–100.30%, respectively. The developed method was found to be accurate, precise, specific, linear, rugged, and robust. Forced degradation studies were conducted by exposing the drug to diverse stress conditions such as acidic, basic, peroxide, neutral, photolytic, and thermal conditions. The net degradation was obtained within the limits.Conclusion: The developed method for the estimation of lenvatinib can be employed to routine analysis of pharmaceutical dosage form.

scholarly journals STABILITY-INDICATING METHOD DEVELOPMENT AND VALIDATION FOR THE ESTIMATION OF CABOZANTINIB IN PHARMACEUTICAL DOSAGE FORMS BY ULTRA-PERFORMANCE LIQUID CHROMATOGRAPHY

2018 ◽  
Vol 11 (10) ◽  
pp. 238
Author(s):  
Gorja Ashok ◽  
Sumanta Mondal
Keyword(s):  
Liquid Chromatography ◽  
Dosage Form ◽  
Method Development ◽  
Thermal Conditions ◽  
Ultra Performance Liquid Chromatography ◽  
Forced Degradation ◽  
Solution Stability ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating

Objective: The proposed study aimed to develop a stability-indicating ultra-performance liquid chromatography (UPLC) method for the estimation of cabozantinib in pharmaceutical dosage form and validate the method in accordance with the International Conference on Harmonization guidelines.Methods: The optimized conditions for the developed UPLC method are Acquity UPLC Hibar C18 (100 mm × 2.1 mm, 1.7 μ) column maintained at 30°C with mobile phase consisting of 0.1% orthophosphoric acid and acetonitrile in the ratio of 55:45% v/v on isocratic mode at flow rate of 0.3 mL/ min. The sample was detected at 244 nm.Results: The retention time for cabozantinib was deemed 1.3 min. The developed method was validated for accuracy, precision, specificity, ruggedness, robustness, and solution stability. The method obeyed Beer’s law in the concentration range of 20 μg/mL and 120 μg/mL with correlation coefficient of 0.9997. Forced degradation studies were conducted by exposing the drug solution to numerous stress conditions such as acidic, basic, peroxide, neutral, photolytic, and thermal conditions. The net degradation was considered within the limits, indicating that drug is stable in stressed conditions.Conclusion: The developed method for the estimation of cabozantinib can be utilized for the routine analysis of pharmaceutical dosage form.

scholarly journals STABILITY INDICATING METHOD DEVELOPMENT AND VALIDATION FOR THE ESTIMATION OF PANOBINOSTAT LACTATEIN PHARMACEUTICAL DOSAGE FORMS BY UPLC

2018 ◽  
Vol 10 (11) ◽  
pp. 60
Author(s):  
Ashok Gorja ◽  
Sumanta Mondal
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Thermal Conditions ◽  
Ultra Performance Liquid Chromatography ◽  
Forced Degradation ◽  
Solution Stability ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Stability Indicating Method

Objective: The present study aimed to develop a stability indicating ultra-performance liquid chromatography (UPLC) method for the estimation of panobinostat lactate in pharmaceutical dosage form and validate the method in accordance with ICH guidelines.Methods: The optimized conditions for the developed UPLC method are acquity UPLC hibar C18 (100 mm × 2.1 mm, 1.8µ) column maintained at 30°C with mobile phase consisting of 0.1% ortho phosphoric acid and acetonitrile in the ratio 50:50%v/v on isocratic mode at flow rate 0.3 ml/min. The sample was detected at 266 nm.Results: The retention time for panobinostat was found to be 1.6 min. The developed method was validated for accuracy, precision, specificity, ruggedness, robustness and solution stability. The method obeyed Beer’s law in the concentration range of 50µg/ml and 300µg/ml with correlation coefficient of 0.9998. Forced degradation studies were conducted by exposing the drug solution to various stress conditions such as acidic, basic, peroxide, neutral, photolytic and thermal conditions. The net degradation was found to be within the limits, indicating that drug is stable in stressed conditions.Conclusion: The developed method for the estimation ofpanobinostat can be utilized for the routine analysis of pharmaceutical dosage form.

scholarly journals Validated Stability-Indicating HPLC Method for Paricalcitol in Pharmaceutical Dosage Form According to ICH Guidelines: Application to Stability Studies

2011 ◽  
Vol 94 (2) ◽  
pp. 543-549
Author(s):  
Raquel Ortega ◽  
Natalia Navas ◽  
Antonio Salmerón ◽  
José Cabeza ◽  
Luís F Capitán-Vallvey
Keyword(s):  
Dosage Form ◽  
Uv Light ◽  
Storage Conditions ◽  
Hplc Method ◽  
Stability Study ◽  
Forced Degradation ◽  
Intermediate Precision ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Diluted Solution

Abstract A stability-indicating HPLC method with diode array detection for the determination of paricalcitol, a synthetic vitamin D2 analog, was developed. Analytical parameters were studied according to International Conference on Harmonization guidelines. A C18 column (250 4.6 mm, 5 m particle size) maintained at 25C was used as the stationary phase, and acetonitrilewater (70 30, v/v) as the mobile phase. Chromatograms were recorded at 250 nm. In forced degradation studies, the effects of acid, base, oxidation, temperature, and UV light were investigated and showed no interference with the drug peak. The method was found to be linear (r 0.9989) at concentrations ranging from 0.6 to 10.0 mg/L paricalcitol, precise (repeatability and intermediate precision estimated as RSD less than 3.5), accurate (recoveries higher than 95), specific, and robust. The LOD and LOQ were 0.6 and 0.2 mg/L, respectively. The validated method was used for paricalcitol determination in a formal stability study of its pharmaceutical dosage form in preloaded syringes. The stability of a diluted solution of its pharmaceutical form in Viaflo bags was also tested. The results showed that paricalcitol was stable in preloaded syringes during a period of 30 days from preparation in the different storage conditions tested (room temperature without protection from daylight and 4.4C with protection from daylight). On the contrary, paricalcitol was quickly lost when stored in Viaflo bags by adsorption onto the walls of the container.

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 A NEW STABILITY-INDICATING RP-HPLC-PDA METHOD FOR SIMULTANEOUS ESTIMATION OF TRIPLICATE MIXTURE OF RAMIPRIL, ATORVASTATIN AND CLOPIDOGREL IN TABLET DOSAGE FORM

2018 ◽  
Vol 10 (5) ◽  
pp. 90
Author(s):  
Subba Rao ◽  
B. Balaswami ◽  
P. Venkata Ramana ◽  
P. Sanjeeva ◽  
G. Srenivasulareddy
Keyword(s):  
Quality Control ◽  
Dosage Form ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Column Temperature ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Relative Standard ◽  
Quality Control Tool ◽  
Tablet Dosage

Objective: To develop a novel, accurate, precise and linear reverse phase high performance liquid chromatographic (RP-HPLC) method for simultaneous quantitative estimation of ramipril, atorvastatin and clopidogrel in Atamra-CV tablet and validate as per international conference on harmonization (ICH) guidelines and to perform the force degradation studies using the developed method.Methods: In the present work, the good chromatographic separation was achieved isocratically using a shim-pack HPLC Kromasil 150 mm x 4.6 mm, 5 m. m. And mobile phase consisting of 0.05 M potassium dihydrogen orthophosphate pH 3 adjusted with orthophosphoric acid and acetonitrile in the ratio (52:48), at flow rate 1 ml/min and column temperature (30 °C). The effluents obtained were monitored at 210 nm with the UV-visible detector.Results: The retention time of ramipril, atorvastatin and clopidogrel was found to be 2.893 min, 5.012 min and 6.102 min respectively. The linearity of ramipril, atorvastatin and clopidogrel was found in the range of 25-150 % and the correlation coefficient for ramipril, atorvastatin and clopidogrel were>0.999. The high recovery values (98%-101%) indicate a satisfactory accuracy. The low percent relative standard deviation (% RSD) values in the precision study reveals that the method is precise. The three-drug samples were subjected to stress conditions of acidic and alkaline hydrolysis, oxidation, photolysis and thermal degradation. The proposed method proved to be stability-indicating by resolution of the analytes from their forced-degradation products.Conclusion: The developed method is novel, simple, precise, rapid, accurate and reproducible for simultaneous estimation of ramipril, atorvastatin and clopidogrel tablet dosage form. Hence the proposed method may find practical applications as a quality-control tool in the simultaneous analysis of the three drugs in combined dosage forms in quality-control laboratories. The proposed method was made use of photodiode array (PDA) as a tool for peak identification and purity confirmation.

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