scholarly journals STABILITY INDICATING REVERSE PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD FOR SIMULTANEOUS ESTIMATION OF LABETALOL AND ITS DEGRADATION PRODUCTS IN TABLET DOSAGE FORMS

2016 ◽  
pp. 242 ◽  
Author(s):  
V. Ashok Chakravarthy ◽  
Sailaja Bbv ◽  
Praveen Kumar A
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Dosage Forms ◽  
Forced Degradation ◽  
Reverse Phase ◽  
Stability Indicating ◽  
Liquid Chromatographic Method ◽  
Forced Degradation Studies ◽  
Tablet Dosage ◽  
Liquid Chromatographic

<p>ABSTRACT<br />Objective: The objective of the present work is to develop a simple, efficient, and reproducible stability indicating reverse phase high-performance<br />liquid chromatographic method for simultaneous determination labetalol and its degradation products in tablet dosage forms.<br />Methods: The chromatographic separation of labetalol and its degradation products in tablets was carried out on Zorbax Eclipse Plus C-18<br />(100 × 4.6 mm, 3.5 µm) column using 0.1% trifluoroacetic acid (TFA) (v/v) in 1000 ml of water and 0.1% TFA (v/v) in 1000 ml of acetonitrile:<br />Methanol (1:1) by linear gradient program. Flow rate was 1.0 mL min<br /> with a column temperature of 35°C, and detection wavelength was carried out<br />at 230 nm. Known impurity is well resolved from the main active drug within 14 minutes run time.<br />−1<br />Results: The forced degradation studies were performed on labetalol tablets under acidic, basic, oxidation, thermal, humidity, and photolytic<br />conditions. No degradation products were observed from the forced degradation studies, and the known impurity is well resolved from the main<br />active drug. The method was validated in terms of specificity, linearity, limit of detection (LOD), limit of quantitation (LOQ), accuracy, precision, and<br />robustness as per the ICH guidelines. The method was found to be linear in the range of LOQ to 120% for all the known and unknown impurities.<br />The LOD and LOQ values of known impurity were found between 0.3593 and 0.7187 µg mL<br />, and the percentage recovery values were in the range<br />of 95.5-105.2% at different concentration levels. Relative standard deviation for precision and intermediate precision results were found to be &lt;5%.<br />The correlation coefficient found for all compounds was not &lt;0.99. The results obtained from the validation experiments prove that the developed<br />method is a stability indicating method.<br />−1<br />Conclusion: The developed method can be successfully applied for routine analysis, quality control analysis and also suitable for stability analysis of<br />the simultaneous determination of labetalol and its degradation products in tablet dosage forms as per the regulatory requirements.<br />Keywords: Labetalol, Development, Validation, Reverse phase high-performance liquid chromatography.</p>

scholarly journals Simultaneous Determination of Simvastatin and Ezetimibe in Tablets by HPLC

2009 ◽  
Vol 6 (2) ◽  
pp. 541-544 ◽  
Author(s):  
D. Anantha Kumar ◽  
D. P. Sujan ◽  
V. Vijayasree ◽  
J. V. L. N. Seshagiri Rao
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Ammonium Acetate ◽  
High Performance Liquid Chromatographic ◽  
Dosage Forms ◽  
Reverse Phase ◽  
Liquid Chromatographic Method ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A reverse phase high performance liquid chromatographic method was developed for the simultaneous determination of simvastatin and ezetimibe in tablet dosage forms. The separation was effected on a C18 Supelcosil column (250 mm x 4.6 mm; 5µ) using a mobile phase consisting of 0.01 M ammonium acetate buffer and acetonitrile (35:65v/v) at a flow rate of 1 mL/min. The detection was made at 240 nm. The retention times for ezetimibe and simvastatin were 5.9 and 8.5 min respectively. Calibration curves were linear over the ranges of 0.5-40 µg/mL for simvastatin and 2.5-50 µg/mL for ezetimibe. The proposed method was validated as per the ICH and USP guidelines. The method is accurate and precise and found to be suitable for the quantitative analysis of both the drugs individually and in combination in tablet dosage forms.

scholarly journals Development of a Stability-Indicating High-Performance Liquid Chromatographic Method for the Simultaneous Determination of Alprazolam and Sertraline in Combined Dosage Forms

2008 ◽  
Vol 91 (6) ◽  
pp. 1344-1353 ◽  
Author(s):  
Ashutosh Pathak ◽  
Sadhana J Rajput
Keyword(s):  
High Performance ◽  
Chromatographic Method ◽  
Degradation Products ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Dosage Forms ◽  
Dihydrogen Phosphate ◽  
Stability Indicating ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Abstract The objective of the current study was to develop a validated stability-indicating high-performance liquid chromatographic method for alprazolam and sertraline in combined dosage forms. The method was validated by subjecting the drugs to forced decomposition under hydrolysis, oxidation, photolysis, and thermal stress conditions prescribed by the International Conference on Harmonization. The drugs were successfully separated from major and minor degradation products on a reversed-phase C18 column by using 75 mM potassium dihydrogen phosphate buffer (pH 4.3)acetonitrilemethanol (50 45 5, v/v/v) as the mobile phase with determination at 227 nm. The flow rate was 0.9 mL/min. The method was validated with respect to linearity, precision, accuracy, system suitability, and robustness. The responses were linear over the ranges of 180 and 5200 g/mL for alprazolam and sertraline, respectively. The recoveries of both drugs from a mixture of degradation products were in the range of 97101. The utility of the procedure was verified by its application to marketed formulations that were subjected to accelerated stability studies. The method distinctly separated the drugs and degradation products, even in actual samples. The products formed in marketed tablets were similar to those formed during stress studies.

scholarly journals Stability-Indicating RP-HPLC Method for Simultaneous Estimation of Enrofloxacin and Its Degradation Products in Tablet Dosage Forms

2015 ◽  
Vol 2015 ◽  
pp. 1-11 ◽  
Author(s):  
V. Ashok Chakravarthy ◽  
B. B. V. Sailaja ◽  
Avvaru Praveen Kumar
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Dosage Forms ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Column Temperature ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Tablet Dosage

The present work was the development of a simple, efficient, and reproducible stability-indicating reverse-phase high performance liquid chromatographic (RP-HPLC) method for simultaneous determination enrofloxacin (EFX) and its degradation products including ethylenediamine impurity, desfluoro impurity, ciprofloxacin impurity, chloro impurity, fluoroquinolonic acid impurity, and decarboxylated impurity in tablet dosage forms. The separation of EFX and its degradation products in tablets was carried out on Kromasil C-18(250×4.6 mm, 5 μm) column using 0.1% (v/v) TEA in 10 mM KH2PO4(pH 2.5) buffer and methanol by linear gradient program. Flow rate was 1.0 mL min−1with a column temperature of 35°C and detection wavelength was carried out at 278 nm and 254 nm. The forced degradation studies were performed on EFX tablets under acidic, basic, oxidation, thermal, humidity, and photolytic conditions. The degraded products were well resolved from the main active drug and also from known impurities within 65 minutes. The method was validated in terms of specificity, linearity, LOD, LOQ, accuracy, precision, and robustness as per ICH guidelines. The results obtained from the validation experiments prove that the developed method is a stability-indicating method and suitable for routine analysis.

ENANTIOSELECTIVE ANALYSIS OF GUAIFENESIN IN BULK AND PHARMACEUTICAL DOSAGE FORMS BY CHIRAL REVERSE PHASE HPLC-PDA METHOD

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (02) ◽  
pp. 36-43
Author(s):  
B. Tharunkumar ◽  
◽  
P. Kalyani ◽  
M. Lakshmiprasanna ◽  
B. N. Nalluri
Keyword(s):  
Dosage Forms ◽  
Racemic Mixture ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
High Pressure Liquid Chromatographic ◽  
Pharmaceutical Dosage Forms ◽  
Enantioselective Analysis ◽  
Liquid Chromatographic Method ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A novel, accurate and precise chiral reverse-phase high pressure liquid chromatographic method was developed for enantioselective analysis of guaifenesin (GFN) in bulk and tablet dosage forms. Chiral separation was achieved on phenomenex Lux Cellulose-4 column (250×4.6mm, 5μ) using 0.02% formic acid: acetonitrile (90:10 V/V) as the mobile phase at a flow rate of 1mL/min at 230nm. The retention times of GFN enantiomers A and B was 15 and 16 minutes, respectively, with good peak resolutions and showing good linearity in the concentration range of 10-50 μg/mL (R2 > 0.999). The developed method was validated as per the International Conference on Harmonization guidelines and the results were well within the acceptable limits. The percentage assay in tablet dosage form was found to be 98.8 and 98.2 respectively, for enantiomers A and B and was with in the compendial specifications, demonstrating the suitability of developed method for enantioselective analysis of guaifenesin racemic mixture.

scholarly journals ESTIMATION OF AMLODIPINE BESYLATE AND IRBESARTAN IN PHARMACEUTICAL FORMULATION BY RP-HPLC WITH FORCED DEGRADATION STUDIES

2019 ◽  
pp. 159-167 ◽  
Author(s):  
T Hemant Kumar ◽  
CH. ASHA ◽  
D. GOWRI SANKAR
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
Forced Degradation ◽  
Amlodipine Besylate ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Forced Degradation Studies ◽  
Liquid Chromatographic

Objective: To develop and validate a simple, specific, accurate, precise and sensitive reverse phase high performance liquid chromatographic (RP-HPLC) method with forced degradation studies for the simultaneous estimation of amlodipine besylate and irbesartan in the pharmaceutical formulation. Methods: The chromatographic separation of the two drugs were achieved using Enable C 18G column (250 ×4.6 mm; 5 µm) in isocratic mode with mobile phase consisting of sodium acetate buffer (pH 4.0) and acetonitrile (30:70, % v/v) with a flow rate of 0.6 ml/min. Ultraviolet(UV) detection was carried out at 238 nm. The proposed method was validated for linearity, range, accuracy, precision, robustness, limit of detection (LOD) and limit of quantification (LOQ). The tablet formulation was subjected to stress conditions of degradation including acidic, alkaline, oxidative, thermal and photolysis. Results: The retention time for amlodipine besylate and irbesartan were found to be 5.512 and 6.321 min respectively. Linearity was observed over a concentration range 4-32 µg/ml for amlodipine besylate (r2 =0.9999) and 10-70 µg/ml for Irbesartan (r2 =0.9998). The % relative standard deviation (RSD) for Intraday and Interday precision was found to be 0.436 and 0.699 for amlodipine besylate and 0.435 and 0.30 for irbesartan. Amlodipine besylate shown stability towards acidic and thermal whereas in basic, oxidative and photolytic it shown less stability in which it degraded to more extent. Irbesartan shown stability towards thermal conditions whereas in remaining conditions it degrades to more extent especially in oxidative conditions. Conclusion: The developed reverse phase high performance liquid chromatographic (RP-HPLC) method was also found to be simple, precise and sensitive for the simultaneous determination of amlodipine besylate and irbesartan in the tablet dosage form.

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