Stability-indicating RP-HPLC method development and validation for simultaneous estimation of telmisartan and rosuvastatin calcium in bulk and in tablet dosage form

Abstract Background The stability-indicating chromatographic method was developed and validated for simultaneous estimation of telmisartan and rosuvastatin calcium in bulk and in tablet dosage form. The RP-HPLC elution was carried out at 242.0 nm using column Oyster ODS3 (150 × 4.6 mm, 5 µm) isocratically, and a mobile phase containing 10 mM phosphate buffer with 1.1 g octane-1-sulfonic acid sodium salt having pH 2.5 (adjusted with 5% OPA) and acetonitrile, with a proportion of 500:500, v/v was pumped through the column maintained at ambient (about 25 °C) temperature with 1.0 mL/min flow rate. The proposed method was validated according to ICH Q2 (R1) guideline. Results Telmisartan and rosuvastatin were eluted at 2.553 min and 4.505 min, respectively. The method is linear from 99.9073 to 299.7218 µg/mL for telmisartan (R2 = 1.000) and 23.6841 – 71.0522 µg/mL for rosuvastatin (R2 = 0.999). The average recovery percentage was found 100.51, 99.76, and 99.14% for telmisartan and 99.68, 99.72, and 98.56% for rosuvastatin at three different levels. Results of method repeatability and intermediate precision were found within acceptable limits. Results of solution stability showed that mobile phase was stable for 2 days; standard and sample preparations are stable for 1 day at room temperature as well as in the refrigerator (2–8 °C). Also, forced degradation study results show that method is stability indicating as capable of distinguishing the active analytes peak from the degraded product. Conclusion The developed stability-indicating method is linear in studied concentration range as well as precise, accurate, specific, and robust. Hence, successfully this method can be used for routine analysis and stability study. Graphical abstract

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

INDIAN DRUGS ◽

10.53879/id.53.06.10500 ◽

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.

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

International Journal of Applied Pharmaceutics ◽

10.22159/ijap.2018v10i5.26945 ◽

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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A stability indicating RP-HPLC- PDA method for simultaneous estimation of segesterone acetate and ethinyl estradiol in tablet dosage form

Research Journal of Chemistry and Environment ◽

10.25303/259rjce113117 ◽

2021 ◽

Vol 25 (9) ◽

pp. 113-117

Author(s):

Narendra Reddy Yeragodala ◽

Sreeramulu Jadi

Keyword(s):

Flow Rate ◽

Mobile Phase ◽

Dosage Form ◽

Ethinyl Estradiol ◽

Simultaneous Estimation ◽

Precise Method ◽

Stability Indicating ◽

Rp Hplc ◽

Tablet Dosage

A simple, accurate, precise method was developed for the simultaneous estimation of the Segesterone acetate and Ethinyl estradiol in a tablet dosage form. The chromatogram was run through Discovery C18 150 x 4.6mm, 5mm column and mobile phase containing buffer 0.01N KH2PO4: Acetonitrile taken in the ratio 50:50 was pumped through the column at a flow rate of 1 ml/min. The temperature was maintained at 30°C. The optimized wavelength selected was 240.0 nm. Ethinyl estradiol and Segesterone acetate were eluted at 2.348 min and 3.855 min respectively.

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

Oriental Journal Of Chemistry ◽

10.13005/ojc/370324 ◽

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.

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DEVELOPMENT OF STABILITY INDICATING RP-HPLC-PDA METHOD FOR THE SIMULTANEOUS ANALYSIS OF NAPROXEN SODIUM AND DIPHENHYDRAMINE HYDROCHLORIDE IN BULK AND TABLET DOSAGE FORMS

INDIAN DRUGS ◽

10.53879/id.52.09.10259 ◽

2015 ◽

Vol 52 (09) ◽

pp. 40-47

Author(s):

B. N Nalluri ◽

◽

B. Mrudula ◽

K Chitralatha ◽

S. A Sultana ◽

...

Keyword(s):

Naproxen Sodium ◽

Simultaneous Estimation ◽

Forced Degradation ◽

Pharmaceutical Dosage Form ◽

Stability Indicating ◽

Diphenhydramine Hydrochloride ◽

Rp Hplc ◽

The Stability ◽

Tablet Dosage ◽

Liquid Chromatographic

The present paper describes a sensitive and simple RP-HPLC-PDA method for the simultaneous estimation of Naproxen Sodium (NPX) and Diphenhydramine Hydrochloride (DPH) in the presence of their degradants. The drugs were subjected to stress conditions (forced degradation) to show the stability-indicating power of the method. The separation was achieved on Inertsil ODS C18 column (250×4.6mm, 5μ). The optimized liquid chromatographic conditions were found to be a mobile phase of 15mM ammonium acetate buffer: acetonitrile (60:40V/V) combination at a flow rate of 1.0 mL/min in isocratic mode with an injection volume of 10µL. The proposed method provided retention times of 4.6 and 10.8min, with linear responses over a range of 60-140μg/mL and 10-30μg/mL and regression coefficient (R2) of 0.999 and 0.996 respectively for NPX and DPH. No interference from other components of pharmaceutical dosage form and degradants was observed. The method was validated as per ICH guidelines and was successfully applied for the simultaneous estimation of both the drugs in bulk and tablet preparations.

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Stability Indicating RP-HPLC Method for Determination of Valsartan in Pure and Pharmaceutical Formulation

E-Journal of Chemistry ◽

10.1155/2010/487197 ◽

2010 ◽

Vol 7 (1) ◽

pp. 246-252 ◽

Cited By ~ 7

Author(s):

S. K. Patro ◽

S. K. Kanungo ◽

V. J. Patro ◽

N. S. K. Choudhury

Keyword(s):

Linear Response ◽

Mobile Phase ◽

Hplc Method ◽

Forced Degradation ◽

Control Analysis ◽

Solution Stability ◽

Stability Indicating ◽

Quality Control Analysis ◽

Rp Hplc

A simple, rapid and accurate and stability indicating RP-HPLC method was developed for the determination of valsartan in pure and tablet forms. The method showed a linear response for concentrations in the range of 50-175 µg/mL using 0.01 M NH4H2PO4(pH 3.5) buffer: methanol [50:50] as the mobile phase with detection at 210 nm and a flow rate of 1 mL/min and retention time 11.041 min. The method was statistically validated for accuracy, precision, linearity, ruggedness, robustness, forced degradation, solution stability and selectivity. Quantitative and recovery studies of the dosage form were also carried out and analyzed; the % RSD from recovery studies was found to be less than 1. Due to simplicity, rapidity and accuracy of the method, we believe that the method will be useful for routine quality control analysis.

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

Journal of AOAC International ◽

10.1093/jaoac/93.2.523 ◽

2010 ◽

Vol 93 (2) ◽

pp. 523-530 ◽

Cited By ~ 5

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.

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ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF NEW STABILITY-INDICATING REVERSE-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR SIMULTANEOUS ESTIMATION OF METFORMIN HYDROCHLORIDE AND EMPAGLIFLOZIN IN TABLET DOSAGE FORM

Asian Journal of Pharmaceutical and Clinical Research ◽

10.22159/ajpcr.2019.v12i1.26537 ◽

2019 ◽

Vol 12 (1) ◽

pp. 241 ◽

Cited By ~ 1

Author(s):

Geetha Susmita A ◽

Rajitha G ◽

Ramya Yadav Y ◽

Uma P

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

High Performance ◽

Dosage Form ◽

Simultaneous Estimation ◽

Reverse Phase ◽

Stability Indicating ◽

Rp Hplc ◽

Relative Standard ◽

Tablet Dosage

Objective: The objective of this study was to develop and validate a stability-indicating reverse-phase high-performance liquid chromatography (RP-HPLC) method for the simultaneous estimation of the metformin and empagliflozin in tablet dosage forms.Methods: The chromatographic conditions were optimized and it was run through Std. BDS (250 mm × 4.6 mm, 5 m) column with mobile phase consisting of 0.1% orthophosphoric acid buffer: acetonitrile in the ratio of 50:50. The flow rate was 1 ml/min and optimized wavelength was 210 nm. Temperature was maintained at 30°C.Results: The retention times of metformin and empagliflozin were found to be 2.588 min and 3.679 min and percentage relative standard deviation (RSD) of the metformin and empagliflozin was found to be 0.59 and 1.2, respectively. Percentage recovery was in the range of 100.01–100.65% for metformin and empagliflozin, respectively.Conclusion: A sensitive, rapid, and specific method has been developed for the simultaneous estimation of metformin and empagliflozin using RP-HPLC in tablet dosage form.

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