scholarly journals Fast Stability Indicating UPLC Method for Quantitative Analysis of Dronedarone in Pharmaceutical Dosage Form: Force Degradation Study

2014 ◽  
Vol 2014 ◽  
pp. 1-7
Author(s):  
Batuk Dabhi ◽  
Hetal Jebaliya ◽  
Yashwantsinh Jadeja ◽  
Madhavi Patel ◽  
Anamik Shah ◽  
...  
Keyword(s):  
Dosage Form ◽  
Limit Of Detection ◽  
Chemical Oxidation ◽  
Pharmaceutical Dosage Form ◽  
Degradation Study ◽  
Stability Indicating ◽  
Time Value ◽  
Heat Degradation ◽  
Significant Difference ◽  
Alkali Hydrolysis

A simple, precise, rapid reproducible, selective, and stability indicating reverse phase UPLC method has been developed for the estimation of dronedarone in pharmaceutical dosage form. Estimation of dronedarone hydrochloride was achieved on Acquity BEH C18 (100 mm*2.1 mm) 1.7 μm column using buffer [20 mM KH2PO4 + 1 mL Triethylamine (pH=2.5 by orthophosphoric acid)] and methanol in ratio of 40 : 60 as mobile phase at 30°C. The flow rate was 0.4 mL/min and effluents were monitored at 290 nm. The method was validated with respect to linearity, accuracy, precision, LOD, LOQ, and robustness. The method was linear over the concentration range 0.38–90 μg/mL (r2=0.999), with a limit of detection and quantification of 0.1 and 0.38 μg/mL, respectively. Dronedarone was subjected to acid and alkali hydrolysis, chemical oxidation, dry heat degradation, and photo (sunlight) degradation. The degraded product peaks were well resolved from the drug peak with significant difference in their retention time value.

Stability Indicating TLC Method for Quantification of Brexpiprazole in Bulk and Its Pharmaceutical Dosage Form and Determination of Content Uniformity

2019 ◽  
Vol 57 (7) ◽  
pp. 644-652 ◽  
Author(s):  
Anjali M Thakkar ◽  
Usmangani K Chhalotiya ◽  
Nikunj Parekh ◽  
Jaineel V Desai ◽  
Dimal A Shah
Keyword(s):  
Dosage Form ◽  
Chemical Oxidation ◽  
Forced Degradation ◽  
Content Uniformity ◽  
Photo Degradation ◽  
Pharmaceutical Dosage Form ◽  
Dry Heat ◽  
Significant Difference ◽  
Alkali Hydrolysis

Abstract A sensitive, selective and precise high performance thin layer chromatographic method has been developed and validated for the quantification of Brexpiprazole in bulk drug and in pharmaceutical dosage form. The method employed HPTLC aluminum plates (pre-coated with silica gel 60 F254) as stationary phase while n-butanol was used as mobile phase. The Rf value of Brexpiprazole was observed to be 0.38. The densitometric analysis was carried out in absorbance mode at 215 nm. The linear regression analysis data for the calibration plots showed a good linear relationship for Brexpiprazole over a concentration range of 200–1,600 ng band−1. The limit of detection and limit of quantification for Brexpiprazole was found to be 66 and 200 ng band−1. To find out the possible degradation pathway, forced degradation studies were performed. The stock solutions of Brexpiprazole (1,000 μg mL−1) were subjected to acid and alkali hydrolysis, chemical oxidation, dry heat degradation and photo degradation. The drug was found to be susceptible to acid and alkali hydrolysis, chemical oxidation, photo degradation and dry heat. The degraded product peaks were well resolved from the pure drug peak with significant difference in their Rf values. Stressed samples were analyzed using developed HPTLC method. The proposed method was validated with respect to linearity, accuracy, precision and robustness. The method was successfully applied to the estimation of Brexpiprazole in marketed formulation and determination of content uniformity of tablet formulation. Statistical analysis showed that the method is repeatable, selective, and precise.

scholarly journals Stability-indicating liquid chromatographic method for quantification of new anti-epileptic drug lacosamide in bulk and pharmaceutical formulation

2012 ◽  
Vol 18 (1) ◽  
pp. 35-42 ◽  
Author(s):  
Usmangani Chhalotiya ◽  
Kashyap Bhatt ◽  
Dimal Shah ◽  
Sunil Baldania ◽  
Jigar Patel
Keyword(s):  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Chemical Oxidation ◽  
Reversed Phase ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Dry Heat ◽  
Alkali Hydrolysis ◽  
Liquid Chromatographic

An isocratic stability indicating reversed-phase liquid chromatographic determination was developed for the quantitative determination of lacosamide in the pharmaceutical dosage form. A Hypersil C-18, 4.5?m column with mobile phase containing acetonitrile-water (20:80, v/v) was used. The flow rate was 1.0 mL min-1 and effluents were monitored at 258 nm. The retention time of lacosamide was 8.9 min. The method was found to be linear in the concentration range of 5-100 ?g/ml and the recovery was found to be in the range of 99.15 - 100.09 %. The limit of detection and limit of quantification were found to be 2 ?g/ml and 5 ?g/ml, respectively. Lacosamide stock solutions were subjected to acid and alkali hydrolysis, chemical oxidation and dry heat degradation. The drug was found to be stable to the dry heat and acidic condition attempted. The proposed method was validated and successfully applied to the estimation of lacosamide in tablet dosage forms.

scholarly journals Development of Stability Indicating LC Method for the Estimation of Tolperisone in Bulk and Pharmaceutical Dosage Form

2013 ◽  
Vol 2013 ◽  
pp. 1-7
Author(s):  
U. K. Chhalotiya ◽  
K. K. Bhatt ◽  
D. A. Shah ◽  
S. L. Baldania ◽  
S. B. Patel
Keyword(s):  
Retention Time ◽  
High Performance ◽  
Dosage Form ◽  
High Performance Liquid Chromatographic ◽  
Chemical Oxidation ◽  
Reversed Phase ◽  
Hplc Method ◽  
Pharmaceutical Dosage Form ◽  
Significant Difference ◽  
Alkali Hydrolysis

A rapid, specific, and sensitive reverse phase high performance liquid chromatographic method has been developed and validated for analysis of tolperisone in both bulk and pharmaceutical dosage form. The HPLC method was performed with a reversed phase C18 SunFire column (250 mm × 4.6 mm i.d., 5 mm particle size), detection at 261 nm and a mixture of methanol, water and pH 7.5 adjusted by use of 1% solution of triethylamine (60 : 40) as mobile phase. The flow rate was 1.0 mL min−1 and effluents were monitored at 261 nm. The retention time of tolperisone was 4.8 min. Tolperisone was subjected to acid and alkali hydrolysis, chemical oxidation, wet hydrolysis, dry heat degradation, and sunlight degradation. The degraded product peaks were well resolved from the pure drug peak with significant difference in their retention time values. Stressed samples were assayed using developed LC method. The proposed method was validated with respect to linearity, accuracy, precision, and robustness. The method was successfully applied to the estimation of tolperisone in tablet dosage forms.

scholarly journals A VALIDATED GRADIENT STABILITY-INDICATING LC METHOD FOR THE ANALYSIS OF VALSARTAN IN PHARMACEUTICAL DOSAGE FORM

2016 ◽  
Vol 8 (9) ◽  
pp. 128
Author(s):  
Tripti Sharma ◽  
Sudan Chandra Si.
Keyword(s):  
Correlation Coefficient ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Research Work ◽  
Pharmaceutical Preparations ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Significant Difference ◽  
Bulk Drug

<p><strong>Objective: </strong>The objective of this research work was to develop a sensitive, precise, specific, linear and stability-indicating gradient HPLC method for the estimation of valsartan in bulk drug and in pharmaceutical preparations.</p><p><strong>Methods: </strong>Chromatographic separation was achieved on C-18 stationary phase with a gradient mobile phase consisting of orthophosphoric acid buffer (the pH of the solution was adjusted to 4.2±0.05 with triethylamine) and methanol. The eluent was monitored with PDA detector at 225 nm with a flow rate of 1.0 ml/min, run time of 65 min.</p><p><strong>Results: </strong>The method was linear over the range of 20-120μg/ml. The correlation coefficient was found to be 0.9994±0.02. In order to check the selectivity of the method for pharmaceutical preparations, forced degradation studies were carried out. Valsartan was found to be stable at light and oxidation experiments. The performance of the method was validated according to the present ICH guidelines for specificity, limit of detection, limit of quantification, linearity, accuracy, precision and robustness. .The LOQ was found to be 0.26µg/ml and the LOD was found to be 0.79µg/ml.<strong> </strong>Valsartan showed good correlation coefficient in the concentration range of 20-120μg/ml. The developed method was compared statistically by applying two-way anova and student's t-test to correlate with an isocratic method and was applied to bulk drug and tablet dosage form. There was no significant difference between the two methods.<strong></strong></p><p><strong>Conclusion: </strong>The proposed method was found to be accurate, precise, sensitive and robust. Hence, it can be used successfully for the routine analysis of valsartan in pharmaceutical formulation and for analysis of stability samples obtained during accelerated stability study.</p>

STABILITY INDICATING HPTLC METHOD FOR THE ESTIMATION OF TICAGRELOR IN BULK AND IN PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2016 ◽  
Vol 53 (10) ◽  
pp. 34-39
Author(s):  
◽  
Elakkiya L Shunmuganathan ◽  
F. A Mehta ◽  
U. K. Chhalotiya
Keyword(s):  
Thin Layer ◽  
High Performance ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Solvent System ◽  
Chemical Oxidation ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Significant Difference ◽  
Hptlc Method

A simple, sensitive, and precise high-performance thin-layer chromatographic method has been developed for the estimation of Ticagrelor in pharmaceutical dosage form. The method employed Thin-layer chromatography (TLC) aluminum plates precoated with silica gel 60 F254 as the stationary phase, while the solvent system was found to be toluene: ethyl acetate: acetic acid (5:4:1V/V/V). The Rf value was observed to be 0.33± 0.008. The spot was densitometrically analyzed in absorbance mode at 305 nm. The method was linear in the range of 50-250 ng/ band for ticagrelor. The limit of detection for ticagrelor was found to be 0.826 ng/ band. The limit of quantification for ticagrelor was found to be 2.64 ng/band. Ticagrelor stock solution was subjected to acid and alkali hydrolysis, chemical oxidation, dry heat degradation and photo degradation. The degraded product peaks were well resolved from the pure drug peak with significant difference in their Rf values. Stressed samples were assayed using developed HPTLC method. The proposed method was validated with respect to linearity, accuracy, precision and robustness. The method was successfully applied to the estimation of ticagrelor in its formulation.

Simultaneous Estimation of Ilaprazole and Domperidone in Pharmaceutical Dosage Form

2016 ◽  
Vol 9 (6) ◽  
pp. 3549-3555
Author(s):  
Gopi Patel ◽  
Kiral M Prajapati ◽  
Bhavesh Prajapati ◽  
Samir K Shah
Keyword(s):  
Dosage Form ◽  
Ammonia Solution ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Control Analysis ◽  
Linear Calibration ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Water Ph ◽  
Alkali Hydrolysis

A simple, accurate and precise stability-indicating RP-HPLC method was developed and subsequently validated for simultaneous determination of ilaprazole and domperidone in bulk and pharmaceutical dosage form. The proposed HPLC method utilizes  C18  (250 mm × 4.6 mm × 5 µm) column with mobile phase comprising of 0.5 % glacial acetic acid in water pH 5.5 adjusted with ammonia solution: methanol in the ratio 45:55 v/v at a flow rate of 1.0 ml/min. Quantitation was achieved with UV detection at 286 nm based on peak area with linear calibration curves at concentration  ranges 80-120µg/ml for ilaprazole and 240-360 µg/ml for domperidone  with correlation coefficient of 0.999.The retention times of ilaprazole and domperidone  were found to be 3.0 min, 5.4 min respectively. The mean recoveries obtained for ilaprazole and domperidone were found to be 99.76 ± 0.6463 % and 100.7 ± 0.2424 % respectively. Stress testing which covered acid, alkali hydrolysis, and peroxide, photolytic, thermal degradation was performed to prove the specificity of the proposed method and degradation was achieved. The proposed method was successfully applied for the stability indicating simultaneous estimation of ilaprazole and domperidone in routine quality control analysis in bulk and pharmaceutical formulation.

scholarly journals Stability-Indicating High-Performance Thin-Layer Chromatographic Method for Quantitative Estimation of Emtricitabine in Bulk Drug and Pharmaceutical Dosage Form

2012 ◽  
Vol 2012 ◽  
pp. 1-7 ◽  
Author(s):  
Atul S. Rathore ◽  
Lohidasan Sathiyanarayanan ◽  
Kakasaheb R. Mahadik
Keyword(s):  
Thin Layer ◽  
High Performance ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Linear Regression Analysis ◽  
Solvent System ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Limit Of Quantitation ◽  
Bulk Drug

A simple, sensitive, precise, specific and stability indicating high-performance thin-layer chromatographic (HPTLC) method for the determination of emtricitabine both in bulk drug and pharmaceutical dosage form was developed and validated. The method employed aluminium plates precoated with silica gel G60 F254 as the stationary phase. The solvent system consisted of toluene : ethyl acetate : methanol (2 : 8 : 1, v/v/v). This solvent system was found to give compact spots for emtricitabine with value . Densitometric analysis of emtricitabine was carried out in the absorbance mode at 284 nm. Linear regression analysis showed good linearity with respect to peak area in the concentration range of 30–110 ng spot−1. The method was validated for precision, limit of detection (LOD), limit of quantitation (LOQ), robustness, accuracy and specificity. Emtricitabine was subjected to acid and alkali hydrolysis, oxidation, neutral hydrolysis, photodegradation and dry heat treatment. Also the degraded products peaks were well resolved from the pure drug with significantly different values. Statistical analysis proved that the method is repeatable and specific for the estimation of the said drug. As the method could effectively separate the drugs from their degradation products, it can be employed as a stability indicating method.

scholarly journals Ultra Sensitive UPLC Method Development and Validation for the Simultaneous Estimation of Tamsulosin Hydrochloride and Tolterodine Tartrate in Bulk and Pharmaceutical Dosage Form

2018 ◽  
pp. 50-59
Author(s):  
Mahmoud M. Sebaiy ◽  
Sobhy M. El-Adl ◽  
Mohamed Baraka ◽  
Mostafa S. Mohram ◽  
Fatma Ibrahim
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Pharmaceutical Preparation ◽  
Potassium Phosphate ◽  
Reversed Phase ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Significant Difference

A rapid, sensitive and accurate ultra-performance reversed phase liquid chromatographic method was developed for the simultaneous determination of tamsulosin and tolterodine in pure form and pharmaceutical preparation. The developed UPLC method is superior to conventional HPLC with respect to speed, resolution, solvent consumption and cost. The separation was carried out on RP C18 nucleosil (1.7 µm, 5 cm x 2 mm) using an isocratic mode in eluting Tamsulosin and Tolterodine at 1.54 min and 2.43 min respectively with a mobile phase composed of acetonitrile and 0.025N potassium phosphate buffer pH 3.50 (60%:40%), respectively. Chromatographic run time was 5 min with a flow rate 0.5 ml/min and UV detection at 220 nm. The linearity for tamsulosin and tolterodine were in the range of 2-20 µg/mL for both drugs, showed excellent recoveries for bulk and tablet dosage form with a very low LOD of 4.29 and 0.59 ng/mL for tamsulosin and tolterodine, respectively. The method has been validated for linearity, accuracy, precision, specificity, and limit of detection, limit of Quantification, robustness, and ruggedness. The method which was developed was validated as per the ICH guidelines. Finally, the method was compared statistically with reference methods indicating that there is no significant difference between them in respect of precision and accuracy.

scholarly journals Stability indicating liquid chromatographic method for the estimation of desvenlafaxine in pharmaceutical dosage form

2011 ◽  
Vol 17 (3) ◽  
pp. 341-348 ◽  
Author(s):  
Dimal Shah ◽  
Riddhi Nakrani ◽  
Sunil Baldania ◽  
Usmangani Chhalotiya ◽  
Kashyap Bhatt
Keyword(s):  
Dosage Form ◽  
Chromatographic Method ◽  
Potassium Dihydrogen Phosphate ◽  
Chemical Oxidation ◽  
Base Hydrolysis ◽  
Dihydrogen Phosphate ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

A simple, sensitive, precise and stability indicating liquid chromatographic method has been developed for the estimation of desvenlafaxine succinate in pharmaceutical dosage form. A Hypersil C-18, 5 mm column with a mobile phase containing 0.05 M potassium dihydrogen phosphate: methanol (60:40 v/v) pH 7 was used. The flow rate was 1.0 mL/min and effluents were monitored at 226 nm. The retention time of desvenlafaxine was 7.4 min and the method was linear in the range of 0.1-20 ?g/mL. Desvenlafaxine stock solution was subjected to acid and alkali hydrolysis, chemical oxidation and dry heat degradation. The drug was found to be susceptible to base hydrolysis and developed method was found to give good separation between the pure drug and the degraded product. The method was successfully applied to the estimation of desvenlafaxine in tablet dosage forms.

scholarly journals METHOD DEVELOPMENT AND VALIDATION FOR SIMULTANEOUS QUANTIFICATION OF NETUPITANT AND PALONOSETRON IN BULK AND PHARMACEUTICAL DOSAGE FORM AND THEIR FORCED DEGRADATION STUDY BY RP-HPLC

2019 ◽  
pp. 119-123
Author(s):  
MANORANJANI M
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Degradation Study ◽  
Simultaneous Quantification ◽  
Relative Standard

Objective: The present paper describes a simple, accurate, and precise reversed-phase high-performance liquid chromatography (HPLC) method for rapid and simultaneous quantification of netupitant (NTP) and palonosetron (PLS) in bulk and pharmaceutical dosage form. Methods: The chromatographic separation was achieved on Luna C18 (250 mm × 4.6 mm, 5 μ). Mobile phase contained a mixture of 0.1% orthophosphoric acid and acetonitrile in the ratio of 60:40 v/v, flow rate 1.0 ml/min, and ultraviolet detection at 222 nm. Results: The proposed method shows a good linearity in the concentration range of 60–900 μg/ml for NTP and 0.1–1.5 μg/ml for PLS under optimized conditions. All the precision and recovery results are in between 98 and 102%. In the entire robustness conditions, percentage of relative standard deviation is <2.0%. Degradation has minimum effect in stress condition and solutions are stable up to 24 h. This method is validated different parameters such as precision, linearity, accuracy, limit of detection, limit of quantification, ruggedness, robustness, and forced degradation study were determined according to the International Conference of Harmonization (ICH) Q2B guidelines. Conclusion: All the parameters of validation were found to be within the acceptance range of ICH guidelines. Since there is no HPLC method reported in the literature for the estimation of NTP and PLS in pharmaceutical dosage forms, there is a need to develop quantitative methods under different conditions to achieve improvement in sensitivity, selectivity, etc. Hence, the author has attempted to develop a validation and forced degradation for simultaneous quantification of NTP and PLS.

Sign in / Sign up

Export Citation Format

Share Document