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

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.

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

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.

Stability Indicating HPTLC Method for Simultaneous Determination of Amlodipine Besylate and Lisinopril in Combined Dose Tablet Formulation

2021 ◽  
pp. 6250-6256
Author(s):  
Sagar B. Wankhede ◽  
Deepak S. Khobragade ◽  
Sukeshini B. Lote ◽  
S. Patil
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Cost Effective ◽  
Tablet Formulation ◽  
Simultaneous Estimation ◽  
Amlodipine Besylate ◽  
Stability Indicating ◽  
Limit Of Quantitation ◽  
Dose Tablet

A combined dose tablet formulation containing Amlodipine besylate and Lisinopril is used for the treatment of essential hypertension. The present study reports development and validation of stability indicating high performance thin layer chromatographic method for simultaneous estimation of these drugs in combined dose tablet formulation. The two drugs were satisfactorily resolved on aluminum plates precoated with silica gel 60F254 using n-butanol : methanol: ammonia (4:4:1 v/v/v) as mobile phase. The Rf value for lisinopril and amlodipine besylate were 0.27±0.02 and 0.62±0.02, respectively. Densitometric evaluation of the separated bands was performed at 215nm. The calibration curves for lisinopril and amlodipine besylate were found to be linear in the concentration range of 1000-6000ng/band. The method was validated as per ICH guidelines for accuracy, precision, robustness, specificity, limit of detection and limit of quantitation. Statistical analysis proves that the method is suitable for simultaneous analysis of Lisinopril and Amlodipine besylate in pharmaceutical formulation without any interference from the excipients/degradant. The developed method offers several advantages such as sensitive, rapid, cost effective and less time consuming as compared to the reported methods. As the method could effectively separate the drugs from its degradation products, it can be employed as a stability indicating method.

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 Stability-Indicating High-Performance Liquid Chromatographic Assay of Atorvastatin with Fluorescence Detection

2007 ◽  
Vol 90 (6) ◽  
pp. 1547-1553 ◽  
Author(s):  
Alaa Khedr
Keyword(s):  
High Performance ◽  
Uv Light ◽  
Degradation Products ◽  
High Performance Liquid Chromatographic ◽  
Base Hydrolysis ◽  
Good Resolution ◽  
Stability Indicating ◽  
Limit Of Quantitation ◽  
Bulk Drug ◽  
Liquid Chromatographic

Abstract The purpose of this work was to develop a sensitive, selective, and validated stability-indicating high-performance liquid chromatographic (LC) assay of atorvastatin (ATV) in bulk drug and tablet form. ATV was subjected to different stress conditions, including UV light, oxidation, acid-base hydrolysis, and temperature. ATV and its degradation products were analyzed on an Agilent Zorbax XDB C18 column using isocratic elution with acetonitrile0.02 M sodium acetate, pH 4.2 (45 + 55, v/v) for 25 min. The samples were monitored with fluorescence (FL) detection at 282 nm (excitation)/400 nm (emission). The response ratio of FL to UV detection (at 247 nm) for ATV was 1.66. The method showed good resolution of ATV from its decomposition products. The photodegradation products were separated by silica gel thin-layer chromatography using double development with ethyl acetaten-hexaneglacial acetic acidmethanol (40 + 55 + 0.5 + 4.5, v/v/v/v) followed by (39 + 55 + 0.5 + 5.5, v/v/v/v), and confirmed by LC-FL analysis. The FL response was linear over the investigated range for ATV. The linear range was 101200 ng/injection, and the limit of quantitation was 2.0 ng/injection.

scholarly journals Validated HPTLC Method for Quantification of Luteolin and Apigenin inPremna mucronataRoxb., Verbenaceae

2015 ◽  
Vol 2015 ◽  
pp. 1-7 ◽  
Author(s):  
Nayan G. Patel ◽  
Kalpana G. Patel ◽  
Kirti V. Patel ◽  
Tejal R. Gandhi
Keyword(s):  
Thin Layer ◽  
Mobile Phase ◽  
High Performance ◽  
Chromatographic Method ◽  
Methanolic Extract ◽  
Limit Of Detection ◽  
Quantitative Estimation ◽  
Reflection Mode ◽  
Limit Of Quantitation ◽  
Hptlc Method

A simple, rapid, and precise high-performance thin-layer chromatographic method was developed for quantitative estimation of luteolin and apigenin inPremna mucronataRoxb., family Verbenaceae. Separation was performed on silica gel 60 F254HPTLC plates using toluene : ethyl acetate : formic acid (6 : 4 : 0.3) as mobile phase for elution of markers from extract. The determination was carried out in fluorescence mode using densitometric absorbance-reflection mode at 366 nm for both luteolin and apigenin. The methanolic extract ofPremna mucronatawas found to contain 10.2 mg/g % luteolin and 0.165 mg/g % of apigenin. The method was validated in terms of linearity, LOD and LOQ, accuracy, precision, and specificity. The calibration curve was found to be linear between 200 and 1000 ng/band for luteolin and 50 and 250 ng/band for apigenin. For luteolin and apigenin, the limit of detection was found to be 42.6 ng/band and 7.97 ng/band while the limit of quantitation was found to be 129.08 ng/band and 24.155 ng/band, respectively. This developed validated method is capable of quantifying and resolving luteolin and apigenin and can be applicable for routine analysis of extract and plant as a whole.

scholarly journals Stability Indicating HPLC Determination of Risperidone in Bulk Drug and Pharmaceutical Formulations

2011 ◽  
Vol 2011 ◽  
pp. 1-6 ◽  
Author(s):  
Zarna R. Dedania ◽  
Ronak R. Dedania ◽  
Navin R. Sheth ◽  
Jigar B. Patel ◽  
Bhavna Patel
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Assay Method ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Stress Studies ◽  
Liquid Chromatographic Separation ◽  
Bulk Drug ◽  
Liquid Chromatographic

The objective of the current study was to develop a validated stability-indicating assay method (SIAM) for risperidone after subjecting it to forced decomposition under hydrolysis, oxidation, photolysis, and thermal stress conditions. The liquid chromatographic separation was achieved isocratically on a symmetry C18 column (5 μm size, 250 mm × 4.6 mm i.d.) using a mobile phase containing methanol: acetonitrile (80 : 20, v/v) at a flow rate of 1 mL/min and UV detection at 280 nm. Retention time of risperidone was found to be . The method was linear over the concentration range of 10–60 μg/mL with a limit of detection and quantitation of 1.79 and 5.44 μg/mL, respectively. The method has the requisite accuracy, specificity, sensitivity, and precision to assay risperidone in bulk form and pharmaceutical dosage forms. Degradation products resulting from the stress studies did not interfere with the detection of Risperidone, and the assay is thus stability indicating.

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 performance liquid chromatographic method for simultaneous quantitation of degradation products of telmisartan and hydrochlorothiazide in combination dosage form

2020 ◽  
Vol 11 (2) ◽  
pp. 2070-2082
Author(s):  
Narasimha Reddy G P ◽  
Sreenivasulu Reddy T ◽  
Sidda Reddy K ◽  
Shashi Kumar K N
Keyword(s):  
Mobile Phase ◽  
Method Development ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Drug Product ◽  
Wave Length ◽  
Stability Study ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating

This work is intended to thrive a stability indicating Ultra performance liquid method for the estimation of (TLM) and (HCTZ) and degradation products pharmaceutical dosage forms. Separation was carried out on Zorbax Eclipse XDB C-18(50 x 2.1 mm, 1.7 ) column using a gradient method. Mobile phase A is 10mM KH2PO4 having 1% (v/v) of and mobile phase B is used in this work. 0.5 / minute is the flow of rate and at 271nm noticed wave length is monitored. Method development trails were carried out on six different columns. For specificity, limit of quantification, limit of detection, linearity, accuracy, method precision, robustness and stability this method is validated. Correlation coefficient of the impurities is more than 0.99. Stability indicating method confirmed that there were no interference of all impurities of TLM and HCTZ. Hence, developed LC method was stability indicating and well applied for drug product stability study as well as to quality monitoring.

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

2015 ◽  
Vol 2015 ◽  
pp. 1-8 ◽  
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.

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

2009 ◽  
Vol 92 (2) ◽  
pp. 387-393 ◽  
Author(s):  
Sunil R Dhaneshwar ◽  
Vidhya K Bhusari ◽  
Mahadeo V Mahadik ◽  
B Santakumari
Keyword(s):  
Thin Layer ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Linear Regression Analysis ◽  
Analysis Data ◽  
Pharmaceutical Dosage Forms ◽  
Mean Values ◽  
Stability Indicating ◽  
Limit Of Quantitation

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.

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