Application of a Stability-Indicating Thin-Layer Chromatographic Method to the Determination of Tenatoprazole in Pharmaceutical Dosage Forms

Abstract A sensitive, selective, precise, and stability-indicating thin-layer chromatographic (TLC) method was developed and validated for the determination of tenatoprazole both as a bulk drug and in formulation. The method uses TLC aluminum plates precoated with Silica Gel 60F-254 as the stationary phase and the solvent system tolueneethyl acetatemethanol (6 4 1, v/v/v). This system gave compact spots for tenatoprazole (Rf value of 0.34 0.02). Tenatoprazole was subjected to acid and alkali hydrolysis, oxidation, and photodegradation. The peaks of the degradation products were well-resolved from that of the pure drug and had significantly different Rf values. Densitometric analysis of tenatoprazole was performed in the absorbance mode at 306 nm. The linear regression analysis data for the calibration plots showed a good linear relationship over the concentration range of 1001500 ng/spot. The mean values of the correlation coefficient, slope, and intercept were 0.9989 1.42, 10.27 0.965, and 4894.2 1.24, respectively. The method was validated for precision, robustness, and recovery. The limit of detection and limit of quantitation were 50 and 100 ng/spot, respectively. Statistical analysis showed that the method is repeatable and selective for estimation of tenatoprazole. Because the method can separate the drug from its degradation products, it can be used to monitor stability.

Download Full-text

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

Chromatography Research International ◽

10.4061/2011/278923 ◽

2011 ◽

Vol 2011 ◽

pp. 1-5 ◽

Cited By ~ 6

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.

Download Full-text

Validated Stability Indicating HPTLC Method for the Estimation of Amoxapine in Different Stress Conditions

Current Pharmaceutical Analysis ◽

10.2174/1573412914666171228163122 ◽

2019 ◽

Vol 15 (3) ◽

pp. 273-279

Author(s):

Shweta G. Rangari ◽

Nishikant A. Raut ◽

Pradip W. Dhore

Keyword(s):

High Performance ◽

Limit Of Detection ◽

Degradation Products ◽

Analysis Data ◽

Peak Height ◽

Good Resolution ◽

Stability Indicating ◽

Limit Of Quantitation ◽

Wide Range ◽

Hptlc Method

Background:The unstable and/or toxic degradation products may form due to degradation of drug which results into loss of therapeutic activity and lead to life threatening condition. Hence, it is important to establish the stability characteristics of drug in various conditions such as in temperature, light, oxidising agent and susceptibility across a wide range of pH values.Introduction:The aim of the proposed study was to develop simple, sensitive and economic stability indicating high performance thin layer chromatography (HPTLC) method for the quantification of Amoxapine in the presence of degradation products.Methods:Amoxapine and its degraded products were separated on precoated silica gel 60F254 TLC plates by using mobile phase comprising of methanol: toluene: ammonium acetate (6:3:1, v/v/v). The densitometric evaluation was carried out at 320 nm in reflectance/absorbance mode. The degradation products obtained as per ICH guidelines under acidic, basic and oxidative conditions have different Rf values 0.12, 0.26 and 0.6 indicating good resolution from each other and pure drug with Rf: 0.47. Amoxapine was found to be stable under neutral, thermal and photo conditions.Results:The method was validated as per ICH Q2 (R1) guidelines in terms of accuracy, precision, ruggedness, robustness and linearity. A good linear relationship between concentration and response (peak area and peak height) over the range of 80 ng/spot to 720 ng/spot was observed from regression analysis data showing correlation coefficient 0.991 and 0.994 for area and height, respectively. The limit of detection (LOD) and limit of quantitation (LOQ) for area were found to be 1.176 ng/mL and 3.565 ng/mL, whereas for height, 50.063 ng/mL and 151.707 ng/mL respectively.Conclusion:The statistical analysis confirmed the accuracy, precision and selectivity of the proposed method which can be effectively used for the analysis of amoxapine in the presence of degradation products.

Download Full-text

STABILITY INDICATING HPLC METHOD FOR DETERMINATION OF VILAZODONE HYDROCHLORIDE

International Journal of Current Pharmaceutical Research ◽

10.22159/ijcpr.2017v9i4.20975 ◽

2017 ◽

Vol 9 (4) ◽

pp. 123

Author(s):

Birva A. Athavia ◽

Zarna R. Dedania ◽

Ronak R. Dedania ◽

S. M. Vijayendra Swamy ◽

Chetana B. Prajapati

Keyword(s):

Limit Of Detection ◽

Degradation Products ◽

Hplc Method ◽

Alkaline Condition ◽

Forced Degradation ◽

Molecular Formula ◽

Stability Indicating ◽

Dry Heat ◽

Limit Of Quantitation

Objective: The aim and objective of this study was to develop and validate Stability Indicating HPLC method for determination of Vilazodone Hydrochloride.Methods: The method was carried out on a Phenomenex, C18 (250x4.6 mm, 5 µm) Column using a mixture of Acetonitrile: Water (50:50v/v), pH adjusted to 3.3 with Glacial Acetic Acid for separation. The flow rate was adjusted at 1 ml/min and Detection was carried out at 240 nm.Results: The retention time of vilazodone hydrochloride was found to be 2.3 min. The calibration curve was found to be linear in the range 25-75µg/ml with a correlation coefficient (R2=0.996). The limit of detection and limit of quantitation were found to be 4.78µg/ml and 14.48µg/ml respectively. The % recovery of vilazodone hydrochloride was found to be in the range of 98.21±0.08 % to 99.07±0.64%. The proposed method was successfully applied for the estimation of vilazodone hydrochloride in marketed tablet formulation.Vilazodone Hydrochloride was subjected to forced degradation under Acidic, Alkaline, Oxidation, Dry Heat and Photolytic degradation conditions. Vilazodone hydrochloride showed 3.12% degradation under acidic condition, 4.78% under alkaline condition, 7.8% under oxidation condition, 3.53% under dry heat condition and 4.9% under photolytic condition.Acid degradation impurity was identified and characterised by LC-MS/MS was found to be 1-(4-Penten-1-yl) piperazine having molecular weight 154.253 (m/z 155.08) and Molecular Formula C9H18N2.Conclusion: A simple, precise, rapid and accurate Stability Indicating HPLC method has been developed and validated for the determination of Vilazodone Hydrochloride in presence of its degradation products as per the ICH Guidelines.

Download Full-text

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

ISRN Chromatography ◽

10.5402/2012/278583 ◽

2012 ◽

Vol 2012 ◽

pp. 1-7 ◽

Cited By ~ 2

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.

Download Full-text

Stability-Indicating HPLC Determination of Trandolapril in Bulk Drug and Pharmaceutical Dosage Forms

International Journal of Analytical Chemistry ◽

10.1155/2015/820517 ◽

2015 ◽

Vol 2015 ◽

pp. 1-8 ◽

Cited By ~ 1

Author(s):

Leena A. Al-Hawash ◽

Ashok K. Shakya ◽

Maher L. Saleem

Keyword(s):

Limit Of Detection ◽

Uv Light ◽

Alkaline Condition ◽

Pharmaceutical Dosage Forms ◽

Stability Indicating ◽

Limit Of Quantitation ◽

Bulk Drug ◽

Oxidative Products ◽

Factorial Design Experiment

A rapid, simple, accurate, precise, economical, robust, and stability indicating reverse phase HPLC-PDA procedure has been developed and validated for the determination of trandolapril. The trandolapril was separated isocratically on Hypersil-Gold C18 column (250 mm × 4.6 mm, 5 μm) with a mobile phase consisting of 50% acetonitrile and 50% water (containing 0.025% triethylamine, pH3.0±0.1), at25±2°C. Retention time of the drug was ~4.6 min. The eluted compounds were monitored and identified at 210 nm. The linearity of the method was excellent(r2>0.9999)over the concentration range of 1–24 μg/mL; the limit of detection (LOD) and limit of quantitation (LOQ) were 0.0566 μg/mL and 0.1715 μg/mL, respectively. The overall precision was less than 2%. Mean recovery of trandolapril was more than 99%; no interference was found from the component present in the preparation. Stability studies indicate that the drug was stable to sunlight and UV light. The drug gives 6 different oxidative products on exposure to hydrogen peroxide. Slight degradation was observed in acidic condition. Degradation was higher in the alkaline condition compared to other conditions. The robustness of the method was studied using factorial design experiment.

Download Full-text

Development and Validation of a Stability-Indicating HPTLC Method for the Estimation of Eszopiclone in Pharmaceutical Dosage Forms

Asian Journal of Research in Pharmaceutical Science ◽

10.52711/2231-5659.2021.00035 ◽

2021 ◽

Vol 11 (3) ◽

pp. 219-223

Author(s):

Vidhya K. Bhusari ◽

Sunil R. Dhaneshwar

Keyword(s):

Mobile Phase ◽

High Performance ◽

Limit Of Detection ◽

Degradation Products ◽

Pharmaceutical Dosage Forms ◽

Stability Indicating ◽

Limit Of Quantitation ◽

Stress Degradation ◽

Bulk Drug ◽

Hptlc Method

Objective: A simple, sensitive, selective, precise repeatable and stability-indicating high-performance thin layer chromatographic method was developed and validated for Eszopiclone in bulk drug and in formulation. Method: Silica gel 60 F-254, TLC precoated aluminium plates was used as the stationary phase for analyzing Eszopiclone and its degradation products, using mobile phase consisting toluene: ethyl acetate: methanol (6: 4: 2 v/v/v). Result: This mobile phase gave compact spots for Eszopiclone with Rf value of 0.52 ± 0.02. Eszopiclone was exposed to hydrolysis, oxidation, neutral and photolytic conditions for conducting stress degradation study. The peak of Eszopiclone and the degradation product was well resolved from each other with a significantly different Rf value. Densitometric estimation of Eszopiclone was performed at 304nm. A good linear plot was obtained in the concentration range of 150-300ng/spot. The method was validated for precision, accuracy (recovery) and robustness study. The limit of detection (LOD) and limit of quantitation (LOQ) was found to be 130ng/spot and 150ng/spot, respectively. Conclusion: The developed HPTLC method can separate Eszopiclone from its degradation products, hence stability studies can be performed using this method.

Download Full-text

Determination of Cassiarin A Level of Cassia siamea Leaf Obtained from Various Regions in Indonesia Using the TLC-Densitometry Method

The Scientific World JOURNAL ◽

10.1155/2020/7367836 ◽

2020 ◽

Vol 2020 ◽

pp. 1-7

Author(s):

Wiwied Ekasari ◽

Yuli Widiyastuti ◽

Dyah Subositi ◽

Rini Hamsidi ◽

Aty Widyawaruyanti ◽

...

Keyword(s):

Limit Of Detection ◽

Antimalarial Activity ◽

Linear Regression Analysis ◽

Analysis Data ◽

Limit Of Quantification ◽

Cassia Siamea ◽

Limit Of Quantitation

Cassia siamea leaf has been proven in vitro and in vivo to have a strong antimalarial activity with Cassiarin A as its active compound. To obtain a source of C. siamea medicinal plant with high level of active antimalarial compound (Cassiarin A), a valid method for determining Cassiarin A level is needed. For this reason, this research conducts the validation of the Cassiarin A content with determination method using thin-layer chromatography (TLC) densitometry which includes the determination of selectivity (Rs), linearity (r), accuracy, precision, limit of detection (LOD), and limit of quantification (LOQ). Cassiarin A was chromatographed on silica gel 60 F254 TLC plate using chloroform : ethanol (85 : 15 v/v) as a mobile phase. Cassiarin A was quantified by densitometric analysis at 368 nm. The linear regression analysis data for the calibration plots showed good linear relationship with r = 0.9995. The method was validated for precision, recovery, repeatability. The minimum detectable amount was found to be 0.0027 μg/spot, whereas the limit of quantitation was found to be 0.008 μg/spot. The results of this validation are then used to determine the Cassiarin A level of C. siamea leaf from various regions in Indonesia. Based on the results of the study, it can be concluded that the TLC-densitometry method can be used to determine level of the Cassiarin A compound with the advantages of being fast, easy, accurate, and inexpensive. In addition, it showed that C. siamea leaves from Pacitan have the highest level of Cassiarin A compared to other areas studied.

Download Full-text

DEVELOPMENT AND VALIDATION OF A STABILITY INDICATING HPLC METHOD FOR THE DETERMINATION OF NILOTINIB HYDROCHLORIDE IN BULK AND PHARMACEUTICAL DOSAGE FORM

International Journal of Pharmacy and Pharmaceutical Sciences ◽

10.22159/ijpps.2016v8i9.11637 ◽

2016 ◽

Vol 8 (9) ◽

pp. 41

Author(s):

Ramu Ivaturi ◽

T. Manikya Sastry ◽

S. Satyaveni

Keyword(s):

Linear Regression Analysis ◽

Analysis Data ◽

Dosage Forms ◽

Hplc Method ◽

Pharmaceutical Dosage Form ◽

Pharmaceutical Dosage Forms ◽

Stability Indicating ◽

Rp Hplc ◽

Ich Guidelines

Objective: To develop a rapid, accurate, linear, sensitive and stability indicating RP-HPLC method for the determination of nilotinib in bulk and pharmaceutical dosage forms in the presence of its four related substances.Methods: The RP-HPLC method was developed for the chromatographic separation of nilotinib and its impurities by using waters Xterra RP-18 (150*4.6 mm, 3.5 µm) column with a mobile phase combination of 10 mM ammonium formate with pH-3.5 and acetonitrile in gradient mode. An injection volume of 20 µl. Flow rate was 1.0 ml/min and detection was carried a wavelength of 250 nm. The method was validated as per ICH guidelines.Results: The retention time for nilotinib and its four impurities were found to be 4.37, 7.40, 8.96, 10.21 and 10.87 min respectively. The linear regression analysis data for the calibration plots showed the good linear relationship in the concentration range of 0.04-3.0 ppm for the nilotinib impurities. The % recovery of nilotinib impurities was found to be 96.8-99.4% in the linearity range. The detection limit (LOD) values were about 0.014, 0.016, 0.005 and 0.03 ppm respectively and the quantification limit (LOQ) values were 0.042, 0.048, 0.014 and 0.09 ppm respectively. The % degradation at various stress conditions like acid, alkaline, oxidative, thermal and photolytic stress was found to be 8.92, 18.35,5.63, 0.88 and 3.89 respectively.Conclusion: The RP-HPLC method compatible with LC-MS was developed for the analysis of nilotinib and its four impurities. It was validated as per the ICH guidelines and found to be linear, robust, precise, accurate, sensitive, stability indicating and can be used for routine as well as stability analysis of capsule dosage forms as well as for drug substance.

Download Full-text

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

Journal of AOAC International ◽

10.1093/jaoac/93.3.787 ◽

2010 ◽

Vol 93 (3) ◽

pp. 787-791 ◽

Cited By ~ 12

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.

Download Full-text

STABILITY INDICATING UPLC METHOD FOR ESTIMATION OF METFORMIN HYDROCHLORIDE AND NATEGLINIDE SIMULTANEOUSLY IN THE PRESENCE OF STRESS DEGRADATION PRODUCTS

INDIAN DRUGS ◽

10.53879/id.57.05.11332 ◽

2020 ◽

Vol 57 (05) ◽

pp. 56-64

Author(s):

Rani A Prameela ◽

S. Madhavi ◽

Rao B. Tirumaleswara ◽

Sudheer Reddy CH.

Keyword(s):

Limit Of Detection ◽

Degradation Products ◽

Potassium Dihydrogen Phosphate ◽

Metformin Hydrochloride ◽

Forced Degradation ◽

Dihydrogen Phosphate ◽

Limit Of Quantification ◽

Pharmaceutical Dosage Forms ◽

Column Temperature

A novel Ultra Performance Liquid Chromatography (UPLC) method was developed and validated for the simultaneous determination of antidiabetic drugs metformin hydrochloride and nateglinide. The method was developed using a Waters ACQUITY UPLC SB C18 (100 × 2.1 mm, 1.8 μm) column. The mobile phase consisting of 0.01 % potassium dihydrogen phosphate buffer (pH 5.8): acetonitrile (50: 50 V/V) was used throughout the analysis. The flow rate was 0.3 mL/min, the injection volume was 1.0 μL, column temperature was 30 0C, run time 3 min and detection was carried at 238 nm using a TUV detector. The retention times of metformin hydrochloride and nateglinide were found to be 1.28 1.71 min, respectively. Metformin hydrochloride and nateglinide were found to be linear over the concentration range of 125-750 and 15-90 μg/mL. The limit of detection and the limit of quantification for metformin hydrochloride were found to be 0.22 and 0.68 μg/mL, respectively, and, for nateglinide, 0.02 and 0.6 μg/mL, respectively. Developed method was validated as per ICH guidelines. The specificity of the method was confirmed by forced degradation study. The suggested method is suitable for determination of metformin hydrochloride and nateglinide in bulk and pharmaceutical dosage forms.

Download Full-text