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.

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.

Stability Indicating HPTLC Method for Sofosbuvir and Daclatasvir in Combination

2020 ◽  
Vol 13 (6) ◽  
pp. 5234-5242
Author(s):  
Mrinalini Damle ◽  
Nivedita Pawar
Keyword(s):  
Limit Of Detection ◽  
Fluorescent Light ◽  
Simultaneous Estimation ◽  
Major Advance ◽  
Good Resolution ◽  
Combination Tablet ◽  
Stability Indicating ◽  
Limit Of Quantitation ◽  
Wide Range ◽  
Hptlc Method

Direct acting antiviral agents represent the major advance in treatment of hepatitis C virus (HCV) infection. Daclatasvir with sofosbuvir that are co-administrated once per day oral dose has been reported to achieve a high rate of virological response in patients with HCV genotype 1, 2 or 3. So, the basic objective of a research involved development and validation of stability indicating HPTLC Method for simultaneous estimation of Sofosbuvir and Daclatasvir available in market in the form of combination tablet. Samples were applied on HPTLC aluminium plates precoated with silica gel 60 F254 (250μm thickness). Mobile phase consists of ethyl acetate: isopropanol in the ratio 9:1v/v. A good resolution was observed between peaks of both the drugs. The retention factor for Sofosbuvir is about 0.51 ±0.02. And for Daclatasvir is about 0.30 ± 0.02. Deuterium lamp as a source of radiation at the wavelength of 260 and 318 nm for analysis of Sofosbuvir and Daclatasvir, respectively. The proposed method was validated according to ICH guidelines and the results were acceptable for linearity and range, accuracy, precision, robustness, detection limit and quantitation limit. The calibration curves were linear over a wide range of 200-1000 ng/band (r2= 0.991) for Sofosbuvir and 45-225 ng/band (r2=0.990) for Daclatasvir. The limit of detection was found to be 21.17 ng/band and 4.38 ng/band for SOF and DAC and limit of quantitation was 64.18 ng/band and 13.28 ng/band for SOF and DAC respectively. During stress degradation study, it was observed that the Daclatasvir is degraded less in thermal and photolytic condition but more in basic hydrolysis condition. Sofosbuvir was found to be sensitive to all stress conditions except the fluorescent light. The suggested method was successfully applied for analysis of both drugs and excellent recovery results were obtained. Being simple, fast, robust, and economic, the method could be applied to the quality control and routine stability monitoring of Sofosbuvir and Daclatasvir.

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 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 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.

scholarly journals Estimation of Berberine in Ayurvedic Formulations Containing Berberis aristata

2008 ◽  
Vol 91 (5) ◽  
pp. 1149-1153 ◽  
Author(s):  
Kedar Kumar Rout ◽  
Subhalaxmi Pradhan ◽  
Sagar Kumar Mishra
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Linear Regression Analysis ◽  
Cost Effective ◽  
Analysis Data ◽  
Calibration Plot ◽  
Methanolic Extracts ◽  
Limit Of Quantitation ◽  
Tlc Plates ◽  
Hptlc Method

Abstract A sensitive, simple, rapid, and efficient high-performance thin-layer chromatographic (HPTLC) method has been developed and validated for the analysis of berberine in marketed Ayurvedic formulations containing Berberis aristata DC for regulatory purposes. Chromatography of methanolic extracts of these formulations was performed on silica gel 60 F254 aluminum-backed TLC plates of 0.2 mm layer thickness. The plate was developed up to 66 mm with the ternary-mobile phase butanolacetic acidwater (8 + 1 + 1, v/v/v) at 33 5C with 5 min of tank saturation. The marker, berberine, was quantified at its maximum absorbance of 350 nm. The limit of detection and limit of quantitation values were found to be 5 and 10 ng/spot. The linear regression analysis data for the calibration plot showed a good linear relationship with correlation coefficient 0.9994 in the concentration range of 10 to 50 ng/spot for berberine with respect to peak area. The instrumental precision was found to be 0.49 coefficient of variation (CV), and repeatability of the method was 0.73 CV. Recovery values from 98.27 to 99.11 indicate excellent accuracy of the method. The developed HPTLC method is very accurate, precise, and cost-effective, and it has been successfully applied to the assay of marketed formulations containing B. aristata for determination of berberine.

Optimization and Validation of HPTLC Method for Estimation of Ulipristal Acetate in Presence of Its Forced Degradation Products

2020 ◽  
Vol 58 (5) ◽  
pp. 427-432
Author(s):  
Gulzar Kamdar ◽  
Sonal Desai
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Uterine Fibroids ◽  
Forced Degradation ◽  
Ulipristal Acetate ◽  
Limit Of Quantitation ◽  
Emergency Contraceptive ◽  
Alkali Hydrolysis ◽  
Hptlc Method

Abstract Ulipristal acetate (UPA) is used as emergency contraceptive and for uterine fibroids. No validated method has been reported to estimate UPA in presence of its degradation products. Therefore it is mandatory to develop method which can accurately measure it in presence of impurity. A simple and sensitive high-performance thin-layer chromatography (HPTLC) method was developed for the estimation of UPA. Pre-coated silica gel 60F254 TLC plates were as stationary phase and ethyl acetate:toluene:glacial acetic acid (4:7:0.3, v/v/v) was used as mobile phase. Drug was subjected to acid and alkali hydrolysis, oxidation, photo degradation and thermal degradation to study its degradation behavior. UPA eluted with Rf value 0.38 ± 0.02. The method was found to be linear in the concentration range of 400–3,600 ng/band. Limit of detection and limit of quantitation were found to be 72.7786 ng/band and 220.5412 ng/band, respectively. The % recovery of the proposed method was found to be 100.05–100.65%. The proposed method was specific to measure UPA in presence of degradants. The method was found to be accurate, precise, robust and can be useful for routine analysis of formulations containing UPA in presence of its degradation products.

scholarly journals STABILITY INDICATING HPLC METHOD FOR DETERMINATION OF VILAZODONE HYDROCHLORIDE

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. 

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 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.

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