scholarly journals Validated Stability Indicating HPTLC of Clopidogrel and its Pharmaceutical Formulations

2019 ◽  
pp. 557-567
Author(s):  
D. S. Ghotekar ◽  
Vishal N. Kushare
Keyword(s):  
High Performance ◽  
Linear Regression Analysis ◽  
Pharmaceutical Formulations ◽  
Analysis Data ◽  
Solvent System ◽  
Assay Method ◽  
Related Substance ◽  
Stability Indicating ◽  
Regular Production

The present paper describes stability indicating high-performance thin-layer chromatography (HPTLC) assay method for clopidogrel in bulk drugs. The method employed TLC aluminium plates precoated with silica gel 60F-254 as the stationary phase. The solvent system consisted of toluene: methanol: triethylamine (6.5: 4.0: 0.1 v/v/v). The system was found to give compact spot for Clopidogrel (<em>R</em><sub>f</sub>value of 0.40 ± 0.010). Densitometric analysis of Clopidogrel was carried out in the absorbance mode at 254 nm. The linear regression analysis data for the calibration plots showed good linear relationship with <em>r</em>2 = 0.999 with respect to peak area in the concentration range 30 - 120 ng/spot. The developed HPTLC method was validated with respect to accuracy, precision, recovery and robustness. Also to determine related substance and assay determination of Clopidogrel that can be used to evaluate the quality of regular production samples. The developed method can also be conveniently used for the assay determination of Clopidogrel .The limits of detection and quantitation were 4.062and 12.322ng/spot, respectively by height.

Development of Validated Stability Indicating HPTLC Method for Assay of Ozagrel and its Pharmaceutical Formulations

2018 ◽  
pp. 36-48 ◽  
Author(s):  
Vishal N Kushare ◽  
Sachin S Kushare
Keyword(s):  
High Performance ◽  
Linear Regression Analysis ◽  
Pharmaceutical Formulations ◽  
Base Hydrolysis ◽  
Assay Method ◽  
Related Substance ◽  
Stability Indicating ◽  
Regular Production ◽  
Hptlc Method

The present paper describes stability indicating high-performance thin-layer chromatography (HPTLC) assay method for Ozagrel in bulk drugs. The method employed TLC aluminium plates precoated with silica gel 60F-254 as the stationary phase. The solvent system consisted of toluene: methanol: triethylamine (6.5: 4.0: 0.1 v/v/v). The system was found to give compact spot for Ozagrel (Rf value of 0.40 ± 0.010). Densitometric analysis of Ozagrel was carried out in the absorbance mode at 280 nm. The linear regression analysis data for the calibration plots showed good linear relationship with r2 = 0.999 with respect to peak area in the concentration range 30 - 120 ng/spot. The developed HPTLC method was validated with respect to accuracy, precision, recovery and robustness. Also to determine related substance and assay determination of Ozagrel that can be used to evaluate the quality of regular production samples. The developed method can also be conveniently used for the assay determination of Ozagrel in pharmaceutical formulations. The limits of detection and quantitation were 4.069 and 12.332 ng/spot, respectively by height. Ozagrel was subjected to acid and alkali hydrolysis, oxidation, photochemical and thermal degradation. The drug undergoes degradation under acidic, basic, oxidation and heat conditions. This indicates that the drug is susceptible to acid, base hydrolysis, oxidation and heat. Statistical analysis proves that the method is repeatable, selective and accurate for the estimation of said drug. The proposed developed HPTLC method can be applied for identification and quantitative determination of Ozagrel in bulk drug and tablet formulation.

scholarly journals Validated Stability-indicating HPTLC Determination of Baclofen in Bulk Drug, Pharmaceutical Formulations and Real Human Urine and Plasma.

2016 ◽  
Vol 8 (1) ◽  
pp. 1545-1554 ◽  
Author(s):  
Safaa F. Saleh ◽  
Mahmoud A. Omar ◽  
Sayed M. Derayea
Keyword(s):  
Human Urine ◽  
High Performance ◽  
Linear Regression Analysis ◽  
Reference Method ◽  
High Sensitivity ◽  
Pharmaceutical Formulations ◽  
Analysis Data ◽  
Calibration Plot ◽  
Stability Indicating

A simple, highly selective and stability-indicating high-performance thin-layer chromatographic method was developed and validated for the analysis of baclofen in bulk powder, pharmaceutical formulations and human urine and in and real human plasma. The method employed TLC aluminum plates precoated with silica gel 60 F254 as the stationary phase. The solvent system consisted of butanol–acetic acid–water (3.0: 0.5: 0.5, v/v/v). This system was found to give compact spots for baclofen (Rf value of 0.54). Densitometric analysis was carried out in the absorbance mode at 238 nm. The linear regression analysis data for the calibration plot showed good linear relationship (r2 = 0.9983) in the concentration range 1.5-7.5 µg per spot. The analytical performance of the method was fully validated, and the results were satisfactory. The limits of detection and quantitation were 0.31 and 1.03 µg per spot, respectively. Baclofen was subjected to acid and alkali hydrolysis, oxidation and photodegradation. The degraded product was well separated from the pure drug. Results indicate that the drug is stable against light and basic conditions. However, additional peaks were observed at Rf value of 0.65 and at Rf value of 0.14 with hydrogen peroxide and hydrochloric acid respectively, indicating that the drug is susceptible to oxidation and acid degradation. The method was applied for the analysis of baclofen in commercial tablets and the results were similar to those obtained using the reference method. As the method could effectively separate the drug from its degradation product, it can be employed as a stability-indicating one. The high sensitivity of the proposed method allowed determination of baclofen in real human urine and plasma.

Quantification of Newly Discovered Anti-Cancer Drug Enzalutamide in Bulk and Synthetic Mixture by Stability Indicating TLC Method

2019 ◽  
Vol 16 (1) ◽  
pp. 104-112
Author(s):  
Dharmendra Jayantibhai Prajapati ◽  
Usmangani Khalilurraheman Chhalotiya ◽  
Minesh Dahyabhai Prajapati ◽  
Jalpa Upendrabhai Patel ◽  
Jaineel Vinodrai Desai
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Linear Regression Analysis ◽  
Analysis Data ◽  
Solvent System ◽  
Chemical Oxidation ◽  
Synthetic Mixture ◽  
Cancer Drug ◽  
Limit Of Quantification ◽  
Stability Indicating

Objective: An impressionable, discriminatory and precise stability indicating high performance thin layer chromatographic method has been developed and validated for the estimation of Enzalutamide in bulk and synthetic mixture. Method: The method engaged HPTLC aluminium plates pre-coated with silica gel 60F-254 as the stationary phase while the solvent system was ethyl acetate: toluene (4.5:5.5, v/v). The Rf value of enzalutamide was detected to be 0. 39 &amp;#177; 0. 005 and the densitometric analysis was carried out in absorbance mode at 246 nm. The linear regression analysis data for the calibration plots presented a virtuous linear relationship for enzalutamide over a concentration range of 20 - 1000ng/band. Results: The limit of detection and limit of quantification for enzalutamide was found to be 9.05 and 27.43 ng/band. Enzalutamide was imperilled to acid and alkali hydrolysis, chemical oxidation, dry heat degradation and photolytic degradation. The degraded product peaks were well resolved from the pure drug peak with substantial difference in their Rf values. Conclusion: Stressed samples were assayed using developed TLC technique. Suggested method was validated with respect to linearity, accuracy, precision and robustness. The method was successfully applied to the estimation of enzalutamide in synthetic mixture.<P&gt;

scholarly journals Assay of Clopidogrel by Using HPLTC Method

2018 ◽  
pp. 557-561
Author(s):  
D. S. Ghotekar ◽  
Vishal N. Kushare
Keyword(s):  
Regression Analysis ◽  
Linear Regression ◽  
Thin Layer ◽  
Stationary Phase ◽  
High Performance ◽  
Linear Regression Analysis ◽  
Analysis Data ◽  
Solvent System ◽  
Assay Method ◽  
Layer Chromatography

The present paper describes stability indicating high-performance thin-layer chromatography (HPTLC) assay method for clopidogrel in bulk drugs. The method employed TLC aluminium plates precoated with silica gel 60F-254 as the stationary phase. The solvent system consisted of toluene: methanol: triethylamine (6.5: 4.0: 0.1 v/v/v). The system was found to give compact spot for clopidogrel (<em>R</em><sub>f</sub>value of 0.40 ± 0.010). Densitometric analysis of Clopidogrel was carried out in the absorbance mode at 254 nm. The linear regression analysis data for the calibration plots showed good linear relationship with <em>r</em>2 = 0.888 with respect to peak area in the concentration range 30 - 120 ng/spot.

scholarly journals Development and Validation of Stability-Indicating HPTLC Determination of Tamsulosin in Bulk and Pharmaceutical Dosage Form

2011 ◽  
Vol 2011 ◽  
pp. 1-6 ◽  
Author(s):  
S. B. Bari ◽  
A. R. Bakhshi ◽  
P. S. Jain ◽  
S. J. Surana
Keyword(s):  
High Performance ◽  
Linear Regression Analysis ◽  
Analysis Data ◽  
Solvent System ◽  
Mean Value ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Ich Guidelines ◽  
Bulk Drug ◽  
Development And Validation

A simple, economic, selective, precise, and stability-indicating high-performance thin-layer chromatographic method for analysis of tamsulosin hydrochloride, both as a bulk drug and in formulations, was developed and validated according to ICH guidelines. The method employed HPTLC aluminium plates precoated with silica gel 60F-254 as the stationary phase while the solvent system consisted of toluene  :  methanol  :  triethylamine (3.5  :  1.2  :  0.2 v/v). The system was found to give compact spot for drug ( value of ). Densitometric analysis of tamsulosin was carried out in the absorbance mode at 280 nm. The linear regression analysis data for the calibration plots showed good linear relationship, with respect to peak area in the concentration range 400–2400 ng per spot. The mean value ± SD of slope and intercept were and with respect to peak area. The method was validated for precision, recovery, and robustness. The limits of detection and quantitation were 20.49 and 62.10 ng per spot, respectively. Tamsulosin was subjected to hydrolysis, oxidation, and thermal degradation which indicate the drug is susceptible to hydrolysis, oxidation, and heat. Statistical analysis proves that the method is repeatable, selective, and accurate for the estimation of tamsulosin.

scholarly journals Stability-Indicating High-Performance Thin-Layer Chromatographic Method for Quantitative Determination of Omeprazole in Capsule Dosage Form

2010 ◽  
Vol 93 (3) ◽  
pp. 787-791 ◽  
Author(s):  
Preeta Jha ◽  
Rabea Parveen ◽  
Suroor A Khan ◽  
Ozair Alam ◽  
Sayeed Ahmad
Keyword(s):  
Quantitative Determination ◽  
Mobile Phase ◽  
High Performance ◽  
Dosage Form ◽  
Linear Regression Analysis ◽  
Analysis Data ◽  
Stability Testing ◽  
Mean Values ◽  
Stability Indicating

Abstract A novel HPTLC method has been developed and validated for quantitative determination of omeprazole (OPZ) in capsule dosage form. The method was validated according to the International Conference on Harmonization guidelines for accuracy, precision, linearity, specificity, and robustness. HPTLC aluminum sheets precoated with silica gel 60F254 were used as the stationary phase and chloroformmethanol (9 + 1) as the mobile phase. The mobile phase was found to give compact bands for OPZ (Rf value of 0.39 0.12) in densitometric analysis in the absorbance mode at 302 nm. The linear regression analysis data for the calibration plots showed good linearity (r2 = 0.997) with respect to peak area in the concentration range 503000 ng/band. The mean values of the slope and intercept were 9.896 0.0753 and 1870.761 16.866, respectively. The method was also applied for stability testing of OPZ in different stress conditions and found to be accurate, linear, precise, robust, specific, and stability indicating. The method proposed can be used for QC and stability testing of different dosage forms such as tablets and capsules, as well as for bulk drug analysis of OPZ.

Stability Indicating Liquid Chromatographic Method for the Determination of Fenofibrate and its Application to Kinetic Studies

2013 ◽  
Vol 5 (4) ◽  
pp. 1866-1874
Author(s):  
K. Srinivasa Rao ◽  
Keshar N K ◽  
N Jena ◽  
M.E.B Rao ◽  
A K Patnaik
Keyword(s):  
Degradation Products ◽  
Kinetic Studies ◽  
Pharmaceutical Formulations ◽  
Assay Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Zero Order Kinetics ◽  
Relative Standard ◽  
Liquid Chromatographic

A stability-indicating LC assay method was developed for the quantitative determination of fenofibrate (FFB) in pharmaceutical dosage form in the presence of its degradation products and kinetic determinations were evaluated in acidic, alkaline and peroxide degradation conditions. Chromatographic separation was achieved by use of Zorbax C18 column (250 × 4.0 mm, 5 μm). The mobile phase was established by mixing phosphate buffer (pH adjusted 3 with phosphoric acid) and acetonitrile (30:70 v/v). FFB degraded in acidic, alkaline and hydrogen peroxide conditions, while it was more stable in thermal and photolytic conditions. The described method was linear over a range of 1.0-500 μg/ml for determination of FFB (r= 0.9999). The precision was demonstrated by relative standard deviation (RSD) of intra-day (RSD= 0.56– 0.91) and inter-day studies (RSD= 1.47). The mean recovery was found to be 100.01%. The acid and alkaline degradations of FFB in 1M HCl and 1M NaOH solutions showed an apparent zero-order kinetics with rate constants 0.0736 and 0.0698  min−1 respectively and the peroxide degradation with 5% H2O2 demonstrated an apparent first-order kinetics with rate constant k = 0.0202 per min. The t1/2, t90   values are also determined for all the kinetic studies. The developed method was found to be simple, specific, robust, linear, precise, and accurate for the determination of FFB in pharmaceutical formulations.  

scholarly journals Validated Stability Indicating HPTLC Method for the Determination of Dutasteride in Pharmaceutical Dosage Forms

2011 ◽  
Vol 2011 ◽  
pp. 1-5 ◽  
Author(s):  
Dipti B. Patel ◽  
Natubhai J. Patel ◽  
Sejal K. Patel ◽  
Paresh U. Patel
Keyword(s):  
Thin Layer ◽  
Chromatographic Method ◽  
Degradation Products ◽  
Linear Regression Analysis ◽  
Solvent System ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Wet Heat ◽  
Pure Drug

This paper describes simple, sensitive, precise, specific, and stability-indicating high-performance thin-layer chromatographic method for the determination of dutasteride (DUTA) in bulk and tablet formulation. Validation was carried out in compliance with International Conference on Harmonization guidelines. The thin-layer chromatographic method employed aluminium plates precoated with silica gel G60F254 as stationary phase. The solvent system consisted of toluene/methanol/triethylamine (9 : 2 : 1, v/v/v). This solvent system was found to give compact spots for dutasteride with value 0.71 ± 0.01. Densitometric analysis of DUTA was carried out in the absorbance mode at 274 nm. Linear regression analysis showed good linearity () with respect to peak area in the concentration range of 200–3000 ng per spot. The method was validated for precision, accuracy, specificity, and robustness. Pure drug was subjected to acid and alkali hydrolysis, oxidation, photo degradation, dry heat and wet heat treatment. The drug underwent degradation under acidic, basic, oxidative, and wet heat conditions. The degraded products were well separated from the pure drug. Statistical analysis proved that the method is reproducible and selective for estimation of DUTA in bulk and tablets. As the method could effectively separate the drugs from their degradation products, it can be employed as a stability indicating method.

scholarly journals Development and Validation of a Stability-Indicating Column High-Performance Liquid Chromatographic Assay Method for Determination of Nebivolol in Tablet Formulation

2008 ◽  
Vol 91 (3) ◽  
pp. 557-561 ◽  
Author(s):  
Pankaj K Kachhadia ◽  
Ashish S Doshi ◽  
Hitendra S Joshi
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Assay Method ◽  
Array Detector ◽  
Solution Stability ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Relative Standard ◽  
Liquid Chromatographic

Abstract A simple, precise, and accurate isocratic reversed-phase (RP) stability-indicating column high-performance liquid chromatographic (HPLC) assay method was developed and validated for determination of nebivolol in solid pharmaceutical dosage forms. Isocratic RP-HPLC separation was achieved on a Phenomenex Luna C8 (2) column (250 mm 4.6 mm id, 5 m particle size) using mobile phase composed of acetonitrilepH 3.5 phosphate buffer (35 + 65, v/v) at a flow rate of 1.0 mL/min, and detection was performed at 280 nm using a photodiode array detector. The drug was subjected to oxidation, hydrolysis, photolysis, and heat to apply stress conditions. The method was validated for specificity, linearity, precision, accuracy, robustness, and solution stability. The method was linear in the drug concentration range of 40160 g/mL with a correlation coefficient of 0.9999. The repeatability relative standard deviation (RSD) for 6 samples was 0.69, and the intermediate precision (RSD) for 6 samples was 1.39. The accuracy (recovery) was between 98.57 and 99.55. Degradation products produced as a result of stress studies did not interfere with detection of nebivolol, and the assay can thus be considered stability-indicating.

scholarly journals Development and Validation of a Reversed-Phase High-Performance Thin-Layer ChromatographyDensitometric Method for Determination of Atorvastatin Calcium in Bulk Drug and Tablets

2010 ◽  
Vol 93 (3) ◽  
pp. 798-803 ◽  
Author(s):  
Atul A Shirkhedkar ◽  
Sanjay J Surana
Keyword(s):  
High Performance ◽  
Linear Regression Analysis ◽  
Analysis Data ◽  
Reversed Phase ◽  
Atorvastatin Calcium ◽  
Aluminum Sheets ◽  
Compact Band ◽  
Bulk Drug ◽  
Development And Validation

Abstract Atorvastatin calcium is a synthetic HMGCoA reductase inhibitor that is used as a cholesterol-lowering agent. A simple, sensitive, selective, and precise RP-HPTLCdensitometric determination of atorvastatin calcium both as bulk drug and from pharmaceutical formulation was developed and validated according to International Conference on Harmonization guidelines. The method used aluminum sheets precoated with silica gel 60 RP18F254s as the stationary phase, and the mobile phase consisted of methanolwater (3.5 + 1.5, v/v). The system gave a compact band for atorvastatin calcium with an Rf value of 0.62 0.02. Densitometric quantification was carried out at 246 nm. The linear regression analysis data for the calibration plots showed a good linear relationship with r = 0.9992 in the working concentration range of 100-800 ng/band. The method was validated for precision, accuracy, ruggedness, robustness, specificity, recovery, LOD, and LOQ. The LOD and LOQ were 6 and 18 ng, respectively. The drug underwent hydrolysis when subjected to acidic conditions and was found to be stable under alkali, oxidation, dry heat, and photodegradation conditions. Statistical analysis proved that the developed RP-HPTLCdensitometry method is reproducible and selective and that it can be applied for identification and quantitative determination of atorvastatin calcium in bulk drug and tablet formulation.

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