Development and Validation of a Reversed-Phase Ultra-Performance Liquid Chromatographic Method for the Simultaneous Determination of Six Drugs Used for Combined Hypertension Therapy

2013 ◽  
Vol 96 (2) ◽  
pp. 295-300 ◽  
Author(s):  
Harshad O Kaila ◽  
Mrunal A Ambasana ◽  
Anamik K Shah
Keyword(s):  
Mobile Phase ◽  
Reversed Phase ◽  
Assay Method ◽  
Detector Response ◽  
Simultaneous Estimation ◽  
Good Resolution ◽  
Amlodipine Besylate ◽  
Hypertension Therapy ◽  
Liquid Chromatographic ◽  
Lercanidipine Hydrochloride

Abstract A simple, rapid, and reliable ultra-performance LC assay method has been developed for the simultaneous estimation of orally administered hypertension drugs (atenolol, hydrochlorothiazide, amlodipine besylate, indapamide, nifedipine, and lercanidipine hydrochloride), any of which may be administered with atenolol in combined hypertension therapy. Chromatography was carried out at 25°C on a 2.1 × 50 mm id, 1.7 μm particle size Acquity BEH C18 column with the isocratic mobile phase 0.01 M, 4.0 pH aqueous phosphate buffer–acetonitrile (50 + 50, v/v) at a flow rate of 0.35 mL/min. All drugs were separated in less than 4 min with good resolution and minimal tailing, without interference by excipients. The method was validated according to International Conference on Harmonization guidelines, and the acceptance criteria for accuracy, precision, linearity, specificity, and system suitability were met in all cases. The column effluent was monitored at 230 nm. The detector response was linear in the range of 1–20 μg/mL of these drugs. LOD obtained was 0.04 μg/mL for atenolol, 0.02 μg/mL for hydrochlorothiazide, 0.03 μg/mL for amlodipine besylate, 0.03 μg/mL for indapamide, 0.02 μg/mL for nifedipine, and 0.01 μg/mL for lercanidipine hydrochloride. The suggested method has the advantage that all the drugs can be quantified alone or in combination with atenolol using a single mobile phase.

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 RP-HPLC method development and validation for simultaneous estimation of efonidipine hydrochloride ethanolate and telmisartan in their synthetic mixture

2021 ◽  
pp. 190-195
Author(s):  
Grishma H Patel ◽  
Shreya D Adeshra ◽  
Dhananjay B Meshram
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Method Development ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Quality Control Laboratory ◽  
Efficient Option ◽  
Liquid Chromatographic

A Novel, selective, accurate and rapid Reversed Phase High Performance Liquid Chromatographic (RPHPLC) method for the analysis of Efonidipine Hydrochloride Ethanolate and Telmisartan in binary mixture has been developed and validated. The chromatographic system consisted of a Phenomenex Kinetex ® 5µ C18 Size: 150 * 4.6mm column and the separation was achieved by using ambient temperature with a mobile phase containing mobile Phase Acetonitrile:25mM Phosphate Buffer pH 4.9 (45:55). The samples were monitored at 253 nm for detection at a flow rate of 1.0 mL/min and the retention time was about 7.77 and 4.10 mins for Efonidipine Hydrochloride Ehanolate and Telmisartan respectively. The calibration curve was linear over the concentration range 5-30 and 10-60 ?g/mL for Efonidipine Hydrochloride Ehanolate and Telmisartan respectively. The proposed method is accurate in the range of 99.75% - 100.10% recovery and precise (%RSD of intraday variation and % RSD of inter day variation were found to be within the acceptance criteria). Therefore, this method can be used as a more convenient and efficient option for the analysis of Efonidipine Hydrochloride Ehanolate and Telmisartan in Quality control laboratory.

scholarly journals Development and Validation of Liquid Chromatographic Method for Estimation of Ibuprofen and Famotidine in Combined Dosage Form

2012 ◽  
Vol 2012 ◽  
pp. 1-5 ◽  
Author(s):  
Dimal A. Shah ◽  
Dixita J. Suthar ◽  
Sunil L. Baldania ◽  
Usman K. Chhalotiya ◽  
Kashyap K. Bhatt
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Chromatographic Method ◽  
Reversed Phase ◽  
Assay Method ◽  
Liquid Chromatographic Method ◽  
Phase Liquid ◽  
Development And Validation ◽  
Liquid Chromatographic

An isocratic, reversed phase-liquid-chromatographic assay method was developed for the quantitative determination of ibuprofen and famotidine in combined-dosage form. A Brownlee C18, 5 μm column with mobile phase containing water : methanol : acetonitrile (30 : 60 : 10, v/v/v) was used. The flow rate was 1.0 mL/min, and effluents were monitored at 264 nm. The retention times of ibuprofen and famotidine were 4.9 min and 6.8 min, respectively. The linearity for ibuprofen and famotidine was in the range of 2–20 μg/mL and 0.1–10 μg/mL, respectively. The proposed method was validated with respect to linearity, accuracy, precision, specificity, and robustness. The method was successfully applied to the estimation of ibuprofen and famotidine in combined dosage form.

scholarly journals SIMULTANEOUS ESTIMATION OF THIOCOLCHICOSIDE AND ACECLOFENAC BY HPTLC

2017 ◽  
Vol 9 (4) ◽  
pp. 55
Author(s):  
Pratima Syal ◽  
Ravinder Kumar ◽  
Govind Arora
Keyword(s):  
Silica Gel ◽  
Mobile Phase ◽  
Dosage Form ◽  
Operating Cost ◽  
Analytical Techniques ◽  
Assay Method ◽  
Detector Response ◽  
Simultaneous Estimation ◽  
Pharmaceutical Dosage Form ◽  
Hptlc Method

Objective: Therefore the aim of the present work was to develop simple, precise and accurate HPTLC method for simultaneous determination of THIO and ACE in pharmaceutical dosage form and application of the method for dissolution study with help of HPTLC method.Methods: The TLC procedure was optimized in view to develop a simultaneous assay method for THIO and ACE. HPTLC Pre-coated plates silica gel 60 F254 20×10 cm, layer thickness 0.2 mm (Merck, Germany). The samples were spotted in the form of bands (8 mm) with a Camag 100 microliter sample (Hamilton) syringe on silica gel precoated aluminium 60F254 plates. The mobile phase consisted of methanol: chloroform: water (9.6: 0.2: 0.2 v/v/v) and 10 ml of mobile phase were used per chromatography run. Plates were scanned over the range of 200-400 nm and the spectra were overlain.Results: The detector response was found to be linear in the concentration range of 0.03-0.180 µg/band and 0.75-4.5 µg/band for THIO and ACE and noting the peak areas. Accuracy of the assay method was evaluated with the recovery of the standards from excipients. The mean percentage recoveries obtained for THIO and ACE were 99.34% and 99.08%, respectively, reported. The peak purity of both drugs was assessed by comparing the respective spectra of standard drugs and samples at peak start, peak apex and peak end positions of the spot.Conclusion: HPTLC, with its advantage of low operating cost, high sample thought and minimum sample preparation need is now days preferred as routine analytical techniques for control and assurance. The validated HPTLC method employed here proved to be simple, fast, accurate, precise and sensitive, thus can be used for routine analysis of Thiocolchicoside and Aceclofenac in tablet dosage form.

DEVELOPMENT AND VALIDATION OF RP-UPLC METHOD USING EXPERIMENTAL DESIGN APPROACH FOR SIMULTANEOUS ESTIMATION OF CANDESARTAN CILEXETIL AND CHLORTHALIDONE

INDIAN DRUGS ◽  
2014 ◽  
Vol 51 (11) ◽  
pp. 36-46
Author(s):  
M Singhal ◽  
◽  
S Amin ◽  
A Kukrety ◽  
A Chauhan ◽  
...  
Keyword(s):  
Candesartan Cilexetil ◽  
Ultra Performance Liquid Chromatography ◽  
Reversed Phase ◽  
Detector Response ◽  
Simultaneous Estimation ◽  
Pharmaceutical Dosage Form ◽  
Ich Guidelines ◽  
Normal Probability ◽  
Development And Validation ◽  
Liquid Chromatographic

Candesartan Cilexetil is an antihypertensive agent currently available in combination with Hydrochlorothiazide. However, it has been proven by research that half dose of Chlorthalidone is equipotent to the dose of Hydrochlorothiazide in similar combination with Candesartan Cilexetil. At present there is no Liquid Chromatographic (LC) method available for the simultaneous estimation of Candesartan Cilexetil and Chlorthalidone in pharmaceutical dosage form. A simple, rapid, reliable and robust reversed phase ultra-performance liquid Chromatography (RP-UPLC) method was developed as per International Conference on Harmonization (ICH) guidelines. The best separation was achieved in less than 5 minutes on a 50 × 2.1 mm, 2.2 µm particle size Dionex C18 column with the gradient mobile phase 5 mM, 6.2 ± 0.5 pH ammonium acetate buffer - acetonitrile at a flow rate of 0.5 mL/min at 215nm. The detector response was linear in the range of 10-200 ppm of these drugs. LOD obtained was 3.04 ppm for Candesartan Cilexetil, 2.82 ppm for Chlorthalidone. Further evaluation of robustness of this method was carried out using Plackett-Burman verification with four factors two levels (high & low) within analytical QbD-principles using statistical software. The outcome of normal probability and overall desirability plots were found acceptable.

scholarly journals VALIDATED RP-HPLC METHOD AND UNIQUE MOBILE PHASE FOR THE SIMULTANEOUS ESTIMATION OF AMLODIPINE BESYLATE AND VALSARTAN FROM SOLID DOSAGE FORM AND ROSUVASTATIN AND VALSARTAN FROM BULK

2019 ◽  
pp. 156-162
Author(s):  
DYADE GK ◽  
SAWANT RL
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Dosage Form ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Amlodipine Besylate ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Liquid Chromatographic

Objective: A reverse-phase high-performance liquid chromatographic (RP-HPLC) method was developed and validated for the simultaneous estimation of amlodipine besylate (AD) and valsartan (VAL) in pharmaceutical dosage form, and rosuvastatin (RV) and VAL from the bulk mixture. Method: Chromatographic separation was performed on RP-C18 column. The optimized unique mobile phase (acetonitrile:water and pH adjusted to 4.8 with acetic acid) was pumped at a flow rate of 0.8 ml/min in the ratio of 75:25% v/v, and the eluents were monitored at 245 nm. Results: The assay was performed with tablet and percentage of assay was found to 101.39 for AD and 100.05 for VAL, respectively, and with bulk mixture, percentage of assay was found to 99.58 for RV and 100.32 for VAL, respectively. Linearity was obtained in the concentration range of 1–12 μg/ml for AD, 5–50 μg/mL for VAL, and 2–20 μg/ml for RV. The method was statistically validated and RSD was found to be <2%, indicating high degree of accuracy and precision of the proposed RP-HPLC method. Conclusions: The method suggests usefulness of unique mobile phase during the estimation of two or more multicomponent dosage forms. Due to its simplicity, rapidness, high precision, and accuracy, the proposed RP-HPLC method can be applied for simultaneous determination of AD and VAL in pharmaceutical dosage form, and RV and VAL in bulk mixture.

scholarly journals Stability-Indicating Reversed-Phase Liquid Chromatographic Method for Simultaneous Determination of Simvastatin and Ezetimibe from Their Combination Drug Products

2007 ◽  
Vol 90 (5) ◽  
pp. 1242-1249 ◽  
Author(s):  
Bharat G Chaudhari ◽  
Natvarlal M Patel ◽  
Paresh B Shah
Keyword(s):  
Mobile Phase ◽  
Degradation Products ◽  
Drug Product ◽  
Reversed Phase ◽  
Stress Conditions ◽  
Simultaneous Estimation ◽  
Combination Drug ◽  
Mobile Phase Flow Rate ◽  
Stability Indicating ◽  
Liquid Chromatographic

Abstract A simple, precise, and rapid stability-indicating reversed-phase column liquid chromatographic (RP-LC) method has been developed and subsequently validated for simultaneous estimation of simvastatin (SIM) and ezetimibe (EZE) from their combination drug product. The proposed RP-LC method utilizes a LiChrospher 100 C18, 5 m, 250 4.0 mm id column at ambient temperature; optimum mobile phase consisting of acetonitrilewatermethanol (60 + 25 + 15, v/v/v) with apparent pH adjusted to 4.0 0.1; mobile phase flow rate of 1.5 mL/min; and ultraviolet detection at 238 nm. SIM, EZE, and their combination drug product were exposed to thermal, photolytic, hydrolytic, and oxidative stress conditions, and the stressed samples were analyzed by the proposed method. There were no other coeluting, interfering peaks from excipients, impurities, or degradation products due to variable stress conditions, and the method is specific for the estimation of SIM and EZE in the presence of degradation products. The described method was linear over the range of 180 and 380 g/mL for SIM and EZE, respectively. The mean recoveries were 99.17 and 100.43 for SIM and EZE, respectively. The intermediate precision data were obtained under different experimental conditions, and the calculated value of the coefficient of variation was found to be less than the critical value. The proposed method can be useful in the quality control of bulk manufacturing and pharmaceutical dosage forms.

Stability indicating Analytical Method Development using Quality by Design (QbD) approach for simultaneous estimation of Ivabradine and Metoprolol

2021 ◽  
pp. 5937-5944
Author(s):  
Noopur K. Gandhi ◽  
Sindhu B. Ezhava
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Method Development ◽  
Quality By Design ◽  
Reversed Phase ◽  
Fractional Factorial ◽  
Simultaneous Estimation ◽  
Good Resolution ◽  
Mobile Phase Flow Rate ◽  
Stability Indicating

The applicability of a quality by design (QbD) approach for the development of a sensitive and selective stability indicating reversed-phase high performance liquid chromatography (RP-HPLC) method for the estimation of Ivabradine and Metoprolol was investigated. Design of experiments using a fractional factorial design approach was used for method development. Fifteen experimental runs were performed to optimize the chromatographic conditions like mobile phase, flow rate and column oven temperature. Mobile phase composition was optimized by changing Acetonitrile composition ranging between 13 and 17% v/v, Flow rate from 0.6 to 1.0 ml/min and temperature between 30 to 50 0C. The optimized method produced sharp peaks with good resolution (>2) for Metoprolol and Ivabradine with retention times of 3.3 and 9.2 min, respectively. The experimental data revealed that volume of Acetonitrile in mobile phase was prominently affecting the Retention time, Resolution & tailing factor of both the drugs. Normal probability plots revealed that the residual and predicted data fall approximately on a straight line, indicating that the experimental error for these studies was evenly distributed suggesting that the model could be used to navigate the design space. This approach is useful to expedite method development and optimization activities in analytical laboratories.

Reversed-Phase High Performance Liquid Chromatographic Analysis of Three First Line Anti-Tuberculosis Drugs

2019 ◽  
Vol 69 (12) ◽  
pp. 3590-3592
Author(s):  
Nela Bibire ◽  
Romeo Iulian Olariu ◽  
Luminita Agoroaei ◽  
Madalina Vieriu ◽  
Alina Diana Panainte ◽  
...  
Keyword(s):  
High Performance ◽  
Biological Fluids ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Assay Method ◽  
Active Pharmaceutical Ingredients ◽  
First Line ◽  
Pharmaceutical Ingredients ◽  
Liquid Chromatographic

Active pharmaceutical ingredients such as isoniazid, pyrazinamide and rifampicin are among the most important first-line anti-tuberculosis drugs. A simple, rapid and sensitive reversed phase-high performance liquid chromatographic assay method for the simultaneous determination of isoniazid, pyrazinamide and rifampicin has been developed. Separation of the interest compounds was achieved in a 10 min chromatographic run in gradient elution mode on a Zorbax SB-C18 stainless steel column (150 � 4 mm, 5 mm) using a guard column containing the same stationary phase. The gradient elution was carried out with a mobile phase of 10% CH3CN aqueous solution for channel A and 50% CH3CN in pH = 6.8 phosphate buffer (20 mM), to which 1.5 mL triethylamine were added for channel B. Quantification of the analyzed substances was carried out spectrophotometrically at 269 nm. Detection limits of 0.48 mg/L for isoniazid, 0.52 mg/L for pyrazinamide and 0.48 mg/L for rifampicin were established for the developed assay method. The present work showed that the proposed analysis method was advantageous for simple and rapid analysis of the active pharmaceutical ingredients in pharmaceuticals and biological fluids.

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