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 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.

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.

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 DEVELOPMENT AND VALIDATION OF STABILITY INDICATING HPTLC METHOD FOR DETERMINATION OF APIXABAN AS BULK DRUG

2019 ◽  
pp. 37-42
Author(s):  
Mrinalini C. Damle ◽  
Swapnil S Waghmare ◽  
PURUSHOTAM SINHA
Keyword(s):  
Thin Layer ◽  
High Performance ◽  
Limit Of Detection ◽  
Chromatography Method ◽  
Stability Indicating ◽  
Chromatographic Condition ◽  
Bulk Drug ◽  
Development And Validation ◽  
Hptlc Method

Objective: To develop and validate simple, sensitive stability indicating HPTLC (High performance thin layer chromatography) method for apixaban. Methods: The chromatographic separation was performed on aluminium plates precoated with silica gel 60 F254 using toluene: ethyl acetate: methanol (3:6:1 v/v/v) as mobile phase followed by densitometric scanning at 279 nm. Results: The chromatographic condition shows sharp peak of apixaban at Rf value of 0.38±0.03. Stress testing was carried out according to international conference on harmonization (ICH)Q1A (R2) guidelines and the method was validated as per ICH Q2(R1) guidelines. The calibration curve was found to be linear in the concentration range of 100-500 ng/band for apixaban. The limit of detection and quantification was found to be 11.66ng/bandand35.33ng/band, respectively. Conclusion: A new simple, sensitive, stability indicating high performance thin layer chromatographic (HPTLC) method has been developed and validated for the determination of apixaban.

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 STABILITY INDICATING HPTLC METHOD FOR ESTIMATION OF SWERTIAMARIN IN BULK AND DOSAGE FORM

2017 ◽  
Vol 9 (6) ◽  
pp. 80
Author(s):  
H. Padh ◽  
S. Parmar ◽  
B. Patel
Keyword(s):  
High Performance ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Bulk Drug ◽  
Development And Validation ◽  
Layer Chromatography ◽  
Herbal Formulations ◽  
Hptlc Method ◽  
Ich Guideline

Objective: In the present study a novel stability-indicating high-performance thin-layer chromatography (HPTLC) method for quantitative determination of Swertiamarin (SW) in bulk drug and formulation has been developed and validated as per ICH guideline Q2 (R1) for global acceptance of standardized herbal formulations.Methods: HPTLC method is developed and validated using solvent ethyl acetate: ethanol: chloroform (3:2.5:4.5 v/v/v) (Rf of SW 0.65±0.04) in the absorbance mode at 243 nm. Various forced degradation conditions were used to check degradation of drug.Results: The method showed a good linear relationship (r2 = 0.9990) in the concentration range 200-700 ng per spot. It was found to be linear, accurate, precise and specific.Conclusion: It can be applied for quality control as well as for stability testing of different dosage forms containing swertiamarin. The developed method is validated as per ICH guideline Q2(R1) for global acceptance of standardized herbal formulations.

scholarly journals Development and Validation of a Stability-Indicating Assay Method for Simultaneous Determination of Perindopril and Indapamide in Combined Dosage Form by Reversed-Phase High-Performance Liquid Chromatography

2010 ◽  
Vol 93 (1) ◽  
pp. 108-115 ◽  
Author(s):  
Hitesh Jogia ◽  
Umesh Khandelwal ◽  
Tripti Gandhi ◽  
Sukhdev Singh ◽  
Darshana Modi
Keyword(s):  
Simultaneous Determination ◽  
Stress Testing ◽  
Degradation Products ◽  
Stress Conditions ◽  
Base Hydrolysis ◽  
Assay Method ◽  
Forced Degradation ◽  
Solution Stability ◽  
Stability Indicating

Abstract An approach of forced degradation study was successfully applied for the development of a stability-indicating assay method for simultaneous determination of perindopril and indapamide in a formulation in the presence of its degradation products. The method showed adequate separation of perindopril and indapamide from their associated main impurities and degradation products. Separation was achieved on an XTerra&lt;sup/&gt; RP18, 5 µm, 150 4.6 mm id column at 55°C by using the mobile phase NaH2PO4 buffer (pH 2.0; 0.005 M)acetonitrile (75 + 25, v/v ) at a flow rate of 1 mL/min and UV detection at 215 nm. Comprehensive stress testing of perindopril and indapamide was carried out according to the International Conference on Harmonization (ICH) guideline Q1A (R2). The specificity of the method was determined by assessing interference from the placebo and by stress testing of the drug (forced degradation). The drug was subjected to acid hydrolysis, base hydrolysis, oxidation, dry heat, and photolysis to apply stress conditions. There were no other coeluting, interfering peaks from excipients, impurities, or degradation products due to variable stress conditions, and the method was specific for determination of perindopril and indapamide in the presence of degradation products. The method was validated in terms of linearity, precision, accuracy, specificity, robustness, and solution stability. The linearity of the proposed method was investigated in the range of 2456 µg/mL (r2 = 0.9993) for perindopril and 7.517.5 µg/mL (r2 = 0.9992) for indapamide. Degradation products produced as a result of stress studies did not interfere with the detection of perindopril and indapamide, and the assay can thus be considered stability indicating.

Sign in / Sign up

Export Citation Format

Share Document