scholarly journals Method Development, Validation and Stability Indicating Studies for Simultaneous Estimation of Anti-Hypertensive Drugs from Pharmaceutical Formulation by RP-HPLC

2020 ◽  
Vol 10 (6) ◽  
pp. 120-132
Author(s):  
V. M. Bhalme ◽  
P. P. Jumade ◽  
Ram D Bawankar ◽  
D. S. Wanjari ◽  
D. R. Mundhada
Keyword(s):  
Mobile Phase ◽  
Room Temperature ◽  
Method Development ◽  
Pharmaceutical Formulation ◽  
Simultaneous Estimation ◽  
Reverse Phase ◽  
Reverse Phase Chromatography ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Degradation Studies

Objective: Method development, validation & stability indicating studies for simultaneous estimation of Anti-Hypertensive drugs, Benidepine (BEN) and Metoprolol (MET) from pharmaceutical formulation by RP-HPLC. Methods: For present work, reverse phase chromatography was selected as its suggested use for ionic and moderate to non-polar compounds. Reverse phase chromatography is simple, suitable, better regarding efficiency, stability, and reproducibility. C18 packed column, a 100 X 2.1mm. ID column of 5.0 μm particle packing, was selected for separation of BEN and MET. Different solvent systems were tried and optimized in combinations as mobile phase. BEN (4 μg/ml) and MET (50 μg/ml) in 15mM ammonium formate-Methanol (15:85 v/v) was developed as it was showing good peak shapes and a significant amount of resolution. The mobile phase was flowed at 1.2 ml/min with detection of BEN analytes at 236 nm and MET analytes at 225 nm respectively. Result: Method development was done. Specificity, linearity, accuracy, precision, robustness, limit of detection and limit of quantitation were used to accomplish validation. The method was found linear from 32.5 – 500 µg.ml-1 for both BEN and MET individually. The percentage recovery of BEN when placed for period of 12 hours was found to 100% in 0.1N/M NaOH at 60˚C and Thermal (60˚C); 12 % degradation in 0.1N/M HCl at 60˚C; Oxidation (3-6% H2O2) at room temperature whereas for MET was 100 % in 0.1N/M NaOH, 0.1N/M HCl at 60˚C, at thermal (60˚C) as well as oxidation by 3-6% H2O2 at room temperature.  Conclusion: Developed analytical method for the simultaneous estimation of Benidipine (BED) and Metoprolol (MET) in both bulk and tablet formulation has obliged the ICH guidelines including, tailing factor (T), separation factors (α), theoretical plates (N), capacity factor (k’), resolution (R) and RSD (%). The validated stress degradation studies under thermal, oxidative, alkali and acid ascertained few degradation products for Benidipine whereas the Metoprolol was unaffected with forced degradation studies. Keywords: Benidipine, Metoprolol, Reverse-Phase High Performance Liquid Chromatography, Stability indicating method.

scholarly journals STABILITY INDICATING REVERSE-PHASE HIGH- PERFORMANCE LIQUID CHROMATOGRAPHY METHOD DEVELOPMENT AND VALIDATION FOR SIMULTANEOUS ESTIMATION OF TELMISARTAN AND BENIDIPINE HYDROCHLORIDE IN PHARMACEUTICAL DOSAGE FORM

2018 ◽  
Vol 11 (5) ◽  
pp. 342
Author(s):  
Majan Naim ◽  
Aejaz Ahmed ◽  
Khan Gj
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Dosage Form ◽  
Simultaneous Estimation ◽  
Reverse Phase ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Development And Validation

 Objective: Development and validation of stability indicating reverse-phase high- performance liquid chromatography (RP-HPLC) method for simultaneous estimation of telmisartan (TEL) and benidipine hydrochloride (BND) in pharmaceutical dosage form.Methods: Reverse phase chromatography was selected because of its suggested use for ionic and moderate to non-polar compounds. Reverse phase chromatography is simple, suitable, better regarding efficiency, stability, and reproducibility. C18 column, a 250×4.6 mm column of 5.0 μm particle packing, was selected for separation of TEL and BND. Different solvent systems were tried and optimized in combinations as mobile phase. TEL (40 μg/ml) and BND (4 μg/ml) in buffer, pH 4.0: Methanol (50:50) was developed as it was showing good peak shapes and a significant amount of resolution. The mobile phase was flowed at 1.0 ml/min with detection of both the analytes at 210 nm using photodiode array detector.Result: Development of method was done, and validation was accomplished using specificity, linearity, accuracy, precision, robustness, limit of detection, and limit of quantitation. The method was found linear from 20 to 60 μg/ml and 2–6 μg/ml for TEL and BND individually. The percentage recoveries of TEL 100.46% and BND100.08% were, respectively.Conclusion: This stability indicating RP-HPLC methods were developed by degradation of sample and compared with standard. The percentage relative standard deviation was also <2 % showing high degree of precision of the proposed method. The proposed method can be used for routine analysis of benidipine HCl and TEL in combined dosage form and quality control in bulk manufacturing.

Stability Indicating Assay Method Development and Validation of Simultaneous Estimation of Chlorzoxazone, Diclofenac Sodium and Paracetamol in Bulk Drug and Tablet by RP-HPLC

2021 ◽  
pp. 5024-5028
Author(s):  
Krutika Patel ◽  
Sudheer Kumar Verriboina ◽  
S.G. Vasantharaju
Keyword(s):  
Method Development ◽  
Diclofenac Sodium ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Assay Method ◽  
Simultaneous Estimation ◽  
Dihydrogen Phosphate ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Bulk Drug

A simple, accurate, specific and stability-indicating RP-HPLC method was developed for simultaneous determination of chlorzoxazone, diclofenac sodium and paracetamol, using C18 Vydac Monomeric 120A (250 × 4.6mm, 5μ) at 40ºC. The mobile phase contains a mixture of 20mM potassium dihydrogen phosphate buffer (pH 6.2 adjusted with potassium hydroxide) and acetonitrile (30:70 v/v). The flow rate was 1ml/min and detection was carried out at 275nm using PDA detector. The retention time of paracetamol, chlorzoxazone and diclofenac sodium were 3.28mins, 13.27mins and 15.61mins respectively. The analytical curve was linear over a concentration range of 0.65- 6.5μg/ml for paracetamol, 1-10μg/ml for chlorzoxazone and 0.1-1μg/ml for diclofenac sodium. The drugs in bulk and tablet were subjected to acid and alkali hydrolysis, oxidation, thermal and photolytic degradation. This method can be successfully employed for simultaneous quantitative analysis of Chlorzoxazone, Diclofenac sodium and Paracetamol in bulk drug and tablet formulation.

scholarly journals Validation of developed method by RP-HPLC for simultaneous estimation of famotidine and ibuprofen in human plasma and studying the stability of the drugs in plasma

2018 ◽  
Vol 12 (1) ◽  
pp. 34-48
Author(s):  
K. S Ashutosh ◽  
D. Manidipa ◽  
R. J. V. L. N. Seshagiri ◽  
S. D. Gowri
Keyword(s):  
Human Plasma ◽  
Mobile Phase ◽  
Simultaneous Estimation ◽  
Hplc Separation ◽  
Reverse Phase ◽  
Rp Hplc ◽  
The Stability ◽  
Sodium Dihydrogen ◽  
Isocratic Mode

The RP-HPLC separation was carried out by reverse phase chromatography on a Symmetry C18 (4.6 x 150 mm, 3.5 μm, make: XTerra) with a mobile phase composed of sodium dihydrogen ortho phosphate [pH 2.5] and acetonitrile in the ratio of 30:70 v/v in an isocratic mode at a flow rate of 1.2 mL/min. The run time was maintained for 8.0 min. The detection was monitored at 236 nm. The accuracy was calculated in human plasma and the % recovery was found 99.80 - 99.85 for famotidine and 99.56 -99.85.5 for ibuprofen and reproducibility was found to be satisfactory. The calibration curve for famotidine in human plasma was linear over 3.32 to 6.65 μg/mL and 100- 200 μg/mL for ibuprofen in human plasma respectively. The inter-day and intra-day precision in human plasma was found within limits. The proposed method has adequate sensitivity, reproducibility, and specificity for the determination of famotidine and ibuprofen in plasma. The LLOQ obtained by the proposed method in human plasma were 1.24 and 5.0 μg/mL for famotidine and ibuprofen respectively. The proposed method is simple, fast, accurate, and precise for the quantification of famotidine and ibuprofen in plasma as per the ICH guidelines.Kathmandu University Journal of Science, Engineering and TechnologyVol. 12, No. I, June, 2016, Page: 34-48

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.

DEVELOPMENT AND VALIDATION OF STABILITY INDICATING RP-HPLC METHOD FOR THE SIMULTANEOUS DETERMINATION OF BERBERINE AND CURCUMIN IN AN AYURVEDIC FORMULATION

INDIAN DRUGS ◽  
2016 ◽  
Vol 53 (08) ◽  
pp. 48-52
Author(s):  
K. P Parekh ◽  
◽  
A. P. Jadhav
Keyword(s):  
Mobile Phase ◽  
Herbal Medicines ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Quality And Safety ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Water Ph ◽  
Development And Validation

A simple, accurate, precise, robust stability indicating RP-HPLC method was developed and validated for simultaneous estimation of berberine and curcumin in an ayurvedic formulation. The two markers were resolved using a C-18 column using as the mobile phase methanol: water (pH 3 adjusted using acetic acid) in the ratio 75:25 V/V at a flow rate of 1mL/min. Retention times of berberine and curcumin were 2.58 ± 0.2 min and 8.5 ± 0.2 min, respectively at 358 nm. Linear response was observed in the concentration range of 2 – 8 ppm for berberine and 5 – 40 ppm for curcumin, with correlation coefficient (r2) of 0.994 and 0.998 for berberine and curcumin, respectively. The developed method was applied for quantitation of markers in marketed and in-house formulations of Gruhadhoomadi Churna. This method can also be used to evaluate formulations containing berberine and curcumin as markers, thus conforming to the need of ensuring quality and safety of herbal medicines.

scholarly journals AN INNOVATIVE METHOD DEVELOPMENT AND FORCED DEGRADATION STUDIES FOR SIMULTANEOUS ESTIMATION OF SOFOSBUVIR AND LEDIPASVIR BY RP HPLC

2018 ◽  
pp. 34-41
Author(s):  
B. Anjaneyulu Reddy ◽  
Md. Irshad Alam ◽  
Nazia Khanam ◽  
P. R. Adhakrishnanand
Keyword(s):  
High Performance ◽  
Method Development ◽  
Cost Effective ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Combination Tablet ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Effective Stability

Objective: To develop an innovative, rapid, simple, cost effective, stability indicating reverse phase-high performance liquid chromatography (RP-HPLC) method for simultaneous estimation of ledipasvir (LP) and sofosbuvir (SB) in combination pill dosage form. Methods: The method was developed using C8 column, 250 mm x 4.6 mm, 5mm using mobile section comprising of 0.1% (v/v) orthophosphoric acid buffer at pH 2.2 and acetonitrile in the ratio of 45:55 that was pumped through the column at a flow rate of 0.8 ml/min. Temperature was maintained at 30 °C, the effluents were monitored at 260 nm with the help of usage of PDA detector. Results: The retention time of LP and SB were found to be 2.246 min and 3.502 min. The approach was found to be linear with the variety of 9-36 µg/ml and 40-240 μg/ml for LP and SB respectively, the assay of estimated compounds were found to be 99.65% and 99.73% w/v for LP and SB respectively. Conclusion: The pressured samples changed into analyzed and this proposed a technique turned into determined to be particular and stability indicating as no interfering peaks of decay compound and excipients were observed. Hence, the approach was easy and economical that may be efficiently applied for simultaneous estimation of both LP and SB in bulk and combination tablet system.

scholarly journals 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

2019 ◽  
Vol 12 (1) ◽  
pp. 241 ◽  
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.

Sign in / Sign up

Export Citation Format

Share Document