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

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.

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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.

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Development and Validation of a Stability-Indicating HPTLC Method for Analysis of Rasagiline Mesylate in the Bulk Drug and Tablet Dosage Form

Chromatography Research International ◽

10.1155/2012/273604 ◽

2012 ◽

Vol 2012 ◽

pp. 1-6 ◽

Cited By ~ 2

Author(s):

Singaram Kathirvel ◽

Suggala Venkata Satyanarayana ◽

Garikapati Devalarao

Keyword(s):

Dosage Form ◽

Degradation Products ◽

Linear Regression Analysis ◽

Pharmaceutical Dosage Form ◽

Stability Indicating ◽

Ich Guidelines ◽

Bulk Drug ◽

Rasagiline Mesylate ◽

Development And Validation ◽

Tablet Dosage

A simple and sensitive thin-layer chromatographic method has been established for analysis of rasagiline mesylate in pharmaceutical dosage form. Chromatography on silica gel 60 F254 plates with 6 : 1 : 2(v/v/v) butanol-methanol water as mobile phase furnished compact spots at Rf 0.76±0.01. Densitometric analysis was performed at 254 nm. To show the specificity of the method, rasagiline mesylate was subjected to acid, base, neutral hydrolysis, oxidation, photolysis, and thermal decomposition, and the peaks of degradation products were well resolved from that of the pure drug. Linear regression analysis revealed a good linear relationship between peak area and amount of rasagiline mesylate in the range of 100–350 ng/band. The minimum amount of rasagiline mesylate that could be authentically detected and quantified was 11.12 and 37.21 ng/band, respectively. The method was validated, in accordance with ICH guidelines for precision, accuracy, and robustness. Since the method could effectively separate the drug from its degradation products, it can be regarded as stability indicating.

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UPLC Method Development and Validation for the Determination of Chlophedianol Hydrochloride in Syrup Dosage Form

International Journal of Applied Pharmaceutical Sciences and Research ◽

10.21477/ijapsr.v2i2.7775 ◽

2017 ◽

Vol 2 (02) ◽

pp. 25-31

Author(s):

Anas Rasheed ◽

Osman Ahmed

Keyword(s):

Dosage Form ◽

Method Development ◽

Limit Of Detection ◽

Linear Regression Analysis ◽

Analysis Data ◽

Calibration Plot ◽

Limit Of Quantification ◽

Ich Guidelines ◽

Bulk Drug ◽

Development And Validation

A specific, precise, accurate ultra pressure liquid chromatography (UPLC) method is developed for estimation of chlophedianol hydrochloride in bulk drug and syrup dosage form. The method employed with Hypersil BDS C18 (100 mm x 2.1 mm, 1.7 μm) in a gradient mode, with mobile phase of methanol and acetonitrile in the ratio of 65:35 %v/v. The flow rate was 0.1 ml/min and effluent was monitored at 254 nm. Retention time was found to be 1.130±0.005 min. The method was validated in terms of linearity, accuracy, precision, limit of detection (LOD), limit of quantification (LOQ)in accordance with ICH guidelines. Linear regression analysis data for the calibration plot showed that there was good linear relationship between response and concentration in the range of 20-100 μg/ml respectively. The LOD and LOQ values were found to be 2.094(μg/ml)and 6.3466(μg/ml)respectively. No chromatographic interference from syrup excipients and degradants were found. The proposed method was successfully used for estimation of chlophedianol hydrochloride in syrup dosage form.

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

Journal of AOAC International ◽

10.1093/jaoac/93.3.798 ◽

2010 ◽

Vol 93 (3) ◽

pp. 798-803 ◽

Cited By ~ 4

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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Development and Validation of HPTLC Method for Estimation of Carbamazepine in Formulations and Its In Vitro Release Study

Chromatography Research International ◽

10.4061/2011/684369 ◽

2011 ◽

Vol 2011 ◽

pp. 1-8 ◽

Cited By ~ 5

Author(s):

Rashmin B. Patel ◽

Mrunali R. Patel ◽

Kashyap K. Bhatt ◽

Bharat G. Patel

Keyword(s):

High Performance ◽

Linear Regression Analysis ◽

In Vitro Release ◽

Analysis Data ◽

Limit Of Quantitation ◽

Bulk Drug ◽

Development And Validation ◽

Vitro Release

A new, simple, and rapid high-performance thin-layer chromatographic method was developed and validated for quantitative determination of Carbamazepine. Carbamazepine was chromatographed on silica gel 60 F254 TLC plate using ethyl acetate-toluene-methanol (5.0 + 4.0 + 1.0 v/v/v) as mobile phase. Carbamazepine was quantified by densitometric analysis at 285 nm. The method was found to give compact spots for the drug (Rf=0.47 ± 0.01). The linear regression analysis data for the calibration plots showed good linear relationship with r2=.9995 in the concentration range 100–600 ng/spot. The method was validated for precision, recovery, repeatability, and robustness as per the International Conference on Harmonization guidelines. The minimum detectable amount was found to be 16.7 ng/spot, whereas the limit of quantitation was found to be 50.44 ng/spot. Statistical analysis of the data showed that the method is precise, accurate, reproducible, and selective for the analysis of Carbamazepine. The method was successfully employed for the estimation of equilibrium solubility, quantification of Carbamazepine as a bulk drug, in commercially available preparation, and in-house developed mucoadhesive microemulsion formulations and solution.

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

Current Drug Discovery Technologies ◽

10.2174/1570163814666171027120238 ◽

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 &#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.

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Validated Stability Indicating HPTLC of Clopidogrel and its Pharmaceutical Formulations

International Journal of Scientific Research in Science Engineering and Technology ◽

10.32628/ijsrset207217 ◽

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 (Rfvalue 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 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 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.

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Development and validation of HPTLC method for the analysis of Olmutinib in Bulk drug

International Journal of PharmTech Research ◽

10.20902/ijptr.2019.130105 ◽

2020 ◽

Vol 13 (1) ◽

pp. 37-43

Author(s):

Balu S. Khandare

Keyword(s):

Regression Analysis ◽

Linear Regression ◽

High Performance ◽

Linear Regression Analysis ◽

Solvent System ◽

Average Recovery ◽

Bulk Drug ◽

Development And Validation ◽

Hptlc Method

This paper describes a simple, precise, rapid and accurate high- performance thin layer chromatographic (HPTLC) method for determination of Olmutinib in bulk drug. Chroma to graphic separation was per formed on aluminium plates precoated with silicagel60F254 as the stationary phase using solvent system consisted of chloro form: methanol: (9:1v/v). After the application of bands using CAMAG Automatic TLC Sampler 4, the plate was developed in the solvent system up to 70 mm in CAMAGT win Trough Chamber. This solvent system was found to give compact spot for Olmutinib with Rfvalue of 0.32±0.02. The spots were scanned at 267.68nm. The calibration curves were linear with co-relation coefficient of 0.995 for Olmutinib. Linear regression analysis showed good linearity in the concentration range of 100- 1100 ng per spot. The method was validated in terms of Precision, specificity, and Linearity. The average recovery of the standards in the samples was found to be 99.65% at the same time we have checked the C.V. values of Reproducibility, intra-day and inter-day tabulated further. The proposed method can be successfully applied to determine the drug content of bulk drug.

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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.

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Development and Validation of Stability-Indicating HPTLC Method for Determination of Solifenacin Succinate as bulk Drug and in Tablet Dosage Form

International Journal of Pharmaceutical Sciences and Drug Research ◽

10.25004/ijpsdr.2016.080405 ◽

2016 ◽

Vol 8 (04) ◽

Author(s):

M.C. Damle ◽

P. Rokade

Keyword(s):

High Performance ◽

Dosage Form ◽

Retention Factor ◽

Stability Indicating ◽

Solifenacin Succinate ◽

Ich Guidelines ◽

Bulk Drug ◽

Development And Validation ◽

Tablet Dosage ◽

Hptlc Method

A new simple, stability- indicating high performance thin layer chromatographic (HPTLC) method has been developed and validated for estimation of Solifenacin succinate in bulk and in tablet dosage form. The optimized mobile phase was Methanol: Water: Glacial acetic acid (9:1:0.1v/v/v) with UV detection at 216 nm. The retention factor for Solifenacin succinate was found to be 0.49 ± 0.03. The drug was subjected to stress conditions of hydrolysis under different pH conditions, oxidation, photolysis and thermal degradation as per ICH guidelines. Results were found to be linear in the concentration range of 2000-10000ng band-1.

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