scholarly journals A Validated Stability Indicating RP-HPLC Method for Quantification of Cilnidipine in Bulk and in Tablet Dosage Form

2021 ◽  
Vol 37 (5) ◽  
pp. 1167-1177
Author(s):  
Rameshwar Gholve ◽  
Sanjay Pekamwar
Keyword(s):  
Detection Limit ◽  
Dosage Form ◽  
Hplc Method ◽  
Drug Substance ◽  
Solution Stability ◽  
Stability Indicating ◽  
Quantitation Limit ◽  
Rp Hplc ◽  
The Mean ◽  
Tablet Dosage

A stability indicating RP-HPLC method has been developed for quantification of Cilnidipine in bulk and in tablet dosage form. The chromatographic analysis was accomplished at ambient temperature on Xttera RP18 (100 x 4.6 mm, 3.5 µm) column and 1 mL/min flow rate by using Eluent composed of 10 mM phosphate buffer pH 2.6 with Acetonitrile (300:700, v/v). The UV detection at the wavelength of 240 nm was carried out using 20 µL injection volume. The Cilnidipine retention time was found to be 3.029 min. The method in the range of 40.0573 – 120.1719 µg/mL was found to be linear (R2 = 0.999) with a detection limit and quantitation limit of 1.2038 and 3.6478 μg/mL, respectively. The mean recovery % over the three tested levels of 50, 100, and 150% were found to be 98.74, 99.60, and 98.23%, respectively. The mean % assay of 99.29 for method repeatability and 98.82 for intermediate precision were found with % RSD of 0.68 and 0.31, respectively. Cilnidipine drug substance and their product exposed to acid, alkali, oxidative, thermal, photolytic, and humidity stress conditions. The acid, alkali, and photolytic induced stress studies signifying the formation of a variety of degradants and their peaks were well resolved from that of active analyte peak. Hence, it is recommended that the Cilnidipine drug substance, as well as drug product, should be store in a tightly closed container protected from light. The method as per ICH guidelines was validated for specificity, linearity, detection limit, quantitation limit, precision, accuracy, robustness, solution stability, and can be effectively used for routine analysis.

scholarly journals Stability Indicating RP-HPLC Method Development and Validation for Simultaneous Estimation of Metoprolol Succinate and Chlorthalidone in Bulk and in Tablet Dosage Form

2021 ◽  
Vol 37 (3) ◽  
pp. 683-694
Author(s):  
Rameshwar Gholve ◽  
Sanjay Pekamwar ◽  
Tukaram Kalyankar
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Solution Stability ◽  
Combination Drug ◽  
Metoprolol Succinate ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Tablet Dosage

RP-HPLC method has been developed along with stability indicating attribute for simultaneous estimation of Metoprolol Succinate and Chlorthalidone in bulk and in tablet dosage form with minimized drug extraction steps. The chromatographic analysis was performed isocratically by using Oyster ODS3, 150 - 4.6 mm column having particle size of 5 µm (Merck) as stationary phase maintained at ambient temperature (about 25 °C) with 1.0 mL/minute of flow rate and 20 mM phosphate buffer having pH 2.3 (adjusted with10% orthophosphoric acid) and Acetonitrile (650:350, v/v) as Eluent at wavelength 225 nm. Individual drug substances as well as combination drug product was subjected to acid, alkali, oxidative, photolytic, thermal and humidity degradation, the peaks due to degraded product were significantly separated out from active analytes peak. The method was validated for the specificity, linearity, detection limit, quantitation limit, precision, accuracy, robustness and solution stability as per ICH guidelines and successfully used for regular analysis.

STABILITY-INDICATING RP-HPLC METHOD FOR THE SIMULTANEOUS DETERMINATION OF AMLODIPINE BESYLATE AND AZILSARTAN MEDOXOMIL IN TABLET DOSAGE FORM

INDIAN DRUGS ◽  
2016 ◽  
Vol 53 (06) ◽  
pp. 51-61
Author(s):  
J. G Modi ◽  
◽  
J. K. Patel
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Good Resolution ◽  
Amlodipine Besylate ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Tablet Dosage ◽  
Azilsartan Medoxomil

A novel, simple, rapid, and highly selective stability indicating RP-HPLC method was developed and validated for simultaneous estimation of azilsartan medoxomil (AZL) and amlodipine besylate HCl (AMLO) in tablet dosage form having strength of 20 mg and 2.5 mg, respectively. The effective chromatographic separation was achieved on a Phenomenex luna ODS C18 (15 cm X 4.6 mm internal diameter, 3.5 μm Particle size) with a mobile phase composed of phosphate buffer (pH-2.5) adjusted with ortho phosphoric acid : acetonitrile in the ratio of 60:40 v/v. The mobile phase was pumped using an isocratic HPLC system at a flow rate of 0.7 mL/min with injection volume 20μl and quantification of the analytes was done at detection wavelength 254 nm. The retention times were found to be 5.918 min and 14.901 min for AMLO and AZL, respectively. The proposed HPLC method was validated with respect to linearity, ranges, precision, accuracy, specificity, robustness, LOD, and LOQ as per ICH Q2 (R1) guideline. Calibration plots were linear over the concentration range of 75-125 µg/mL and 600-1000 µg/mL with correlation coefficients 0.9966 and 0.9948 for AMLO and AZL, respectively. Forced degradation studies were performed using hydrolysis, oxidation, photolytic, and thermal degradation conditions with good resolution between the degradants and analytes. Degradation products resulting from the stress studies did not interfere with the detection of AMLO and AZL, thus the proposed method is sensitive and stability-indicating. The validated HPLC method was successfully applied to the analysis of AMLO and AZL in tablet dosage form.

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.

A Validated Stability Indicating RP-HPLC Method for the Estimation of an Anti-Cancer Drug Regorafenib in Pure and Pharmaceutical Dosage Form

2017 ◽  
Vol 4 (1) ◽  
pp. 5-10 ◽  
Author(s):  
Ramesh Jayaprakash ◽  
Senthil Kumar Natesan
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Cancer Drug ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A simple, economic, accurate, sensitive, specific and precise stability indicating reverse phase high performance liquid chromatographic [RP-HPLC] method for the determination of Regorafenib in pure and tablet dosage from was developed and validated. The chromatographic separation was carried out using Phenomenex Luna-C18 column (4.5x250 mm; 5 µm particle size) as a stationary phase and methanol: acetonitrile: water (55:25:20 v/v/v) as a mobile phase. The flow rate of 1 mL/min was used with PDA detection at 275 nm. The retention time of Regorafenib was 2.480 min. RP-HPLC method was developed with linearity range of 40-240 µg/mL of Regorafenib. The correlation coefficient [r2] was found to be 0.9999. The assay results obtained was in good agreement with the corresponding labeled amount by developed method within range of 98.83 ± 0.6937. Accuracy of the method was confirmed by recovery studies and the recoveries were found to be between 99.61 % and 100.22 %, the corresponding %RSD was found to be 0.2029. Precision, LOD, LOQ, specificity, robustness and ruggedness were performed as per ICH Q2(R1) guidelines and were within the acceptance criteria. This method can be conveniently used to detect the possible degradation product in the dosage form of Regorafenib during stability studies (acidic, alkaline, oxidative, thermal and photolytic). The method proved to be effective on the analysis of stressed marketed tablet formulation.

Method Development and Validation for Estimation of Istradefylline in Tablet Dosage form by RP-HPLC

2021 ◽  
pp. 4767-4772
Author(s):  
Krishna Kishore Adireddy ◽  
Srinivasa Rao Baratam ◽  
Nagarjuna Hari Pratap S
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Hplc Method ◽  
Solution Stability ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Tablet Dosage

A simple, rapid, accurate and precise RP-HPLC method was developed and validated for the determination of Istradefylline in table dosage form. Chromatographic analysis of the drug was achieved on Shimadzu HPLC comprising of LC- 20 AD binary gradient pump, a variable wavelength programmable SPD-20A detector and SCL system controller. C18G column (250 mm x 4.6 mm, 5 μ) as stationary phase with mobile phase consisting of 0.1 % orthophosphoric acid and acetonitrile in the ratio of 30: 70 v/v. The method showed a good linear response in the concentration range of 10-90 μg/ml with correlation coefficient of 0.9993. The flow rate was maintained at 1.0 ml/min and detection was carried out at 246 nm. The retention time was 3.125 min. The method was statistically validated for accuracy, precision, linearity, ruggedness, robustness, solution stability, selectivity and sensitivity. The results obtained in the study were within the limits of ICH guidelines and hence this method can be used for the determination of istradefylline in tablet formulation.

Development and validation of stability indicating RP-HPLC method for estimation of roflumilast in tablet dosage form

2021 ◽  
Vol 14 (2) ◽  
pp. 863-868
Author(s):  
Pooja Avula ◽  
Rajitha Galla ◽  
Geetha Susmita Adepu ◽  
Hari Babu Vemanaboina ◽  
Sivaranjani Tyagarajan
Keyword(s):  
Dosage Form ◽  
Hplc Method ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Development And Validation ◽  
Tablet Dosage
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