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

2011 ◽  
Vol 2011 ◽  
pp. 1-8 ◽  
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.

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

2010 ◽  
Vol 93 (3) ◽  
pp. 798-803 ◽  
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.

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

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.

scholarly journals HPTLC method development and validation of stigmasterol from different extracts of Tagetes erecta and Capsicum annuum

2019 ◽  
Vol 9 (6) ◽  
pp. 169-172
Author(s):  
Mohal Lal ◽  
Aboli Kadam ◽  
Aishwarya S. Padole
Keyword(s):  
Thin Layer ◽  
Capsicum Annuum ◽  
High Performance ◽  
Method Development ◽  
Linear Regression Analysis ◽  
Analysis Data ◽  
Tagetes Erecta ◽  
Development And Validation ◽  
Hptlc Method

A new, simple, sensitive, selective, precise and robust high-performance thin-layer chromatographic (HPTLC) method for analysis of stigmasterol was developed and validated for the determination of stigmasterol in different extracts. A new, simple, sensitive, selective, precise and robust high-performance thin-layer chromatographic (HPTLC) method for analysis of stigmasterol was developed and validated for the determination of stigmasterol in different extracts. Analysis of stigmasterol was performed on TLC aluminium plates pre-coated with silica gel 60F-254 as the stationary phase. Linear ascending development was carried out in twin trough glass chamber saturated with mobile phase consisting of Hexane : Acetone (8:2 v/v) at room temperature. (25 °C ± 2 °C) Camag TLC scanner III was used for spectrodensitometric scanning and analysis in absorbance mode at 490nm. The system was found to give compact spots for stigmasterol. (Rf value of 0.44 ± 0.02) The linear regression analysis data for the calibration plots showed good linear relationship with r2 =0.9997 ± 0.0002 in the concentration range 200-1200 ng spot−1 with respect to peak area. According to the International Conference on Harmonization (ICH) guidelines the method was validated for precision, recovery and robustness. Statistical analysis of the data showed that the method is reproducible and selective for the estimation of stigmasterol. Keywords: Tagetes erecta, Capsicum annuum, stigmasterol, HPTLC, method validation

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

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.

DEVELOPMENT AND VALIDATION OF A STABILITY-INDICATING HPLC METHOD FOR ANALYSIS OF ZIDOVUDINE (ZDV) IN BULK DRUG AND IN VITRO RELEASE STUDIES OF TABLETS

2011 ◽  
Vol 34 (8) ◽  
pp. 601-612 ◽  
Author(s):  
Dileep Mandloi ◽  
Priyanka Tripathi ◽  
Palanikar Mohanraj ◽  
Nagendra Singh Chauhan ◽  
Jay Ram Patel
Keyword(s):  
In Vitro Release ◽  
Hplc Method ◽  
Stability Indicating ◽  
Release Studies ◽  
Bulk Drug ◽  
Development And Validation ◽  
Vitro Release

scholarly journals Development and Validation of an HPTLC Method for Determination of Olanzapine in Formulations

2010 ◽  
Vol 93 (3) ◽  
pp. 811-819 ◽  
Author(s):  
Rashmin B Patel ◽  
Mrunali R Patel ◽  
Kashyap K Bhatt ◽  
Bharat G Patel
Keyword(s):  
Regression Analysis ◽  
Statistical Analysis ◽  
Mobile Phase ◽  
Linear Regression Analysis ◽  
Analysis Data ◽  
Equilibrium Solubility ◽  
Bulk Drug ◽  
Development And Validation ◽  
Hptlc Method

Abstract A new, simple, and rapid HPTLC method was developed and validated for quantitative determination of olanzapine on silica gel 60F254 layers using methanolethyl acetate (8.0 + 2.0, v/v) as the mobile phase. Olanzapine was quantified by densitometric analysis at 285 nm. The method was found to give compact bands for the drug (Rf = 0.35 0.02). The linear regression analysis data for the calibration plots showed a good linear relationship with r2 = 0.9997 in the concentration range of 100600 ng/band. The method was validated for precision, recovery, repeatability, and robustness as per the International Conference on Harmonization guidelines. The LOD was found to be 23.90 ng/band, and the LOQ was 91.04 ng/band. Statistical analysis of the data showed that the method is precise, accurate, reproducible, and selective for the analysis of olanzapine. The method was successfully used for the determination of equilibrium solubility and quantification of olanzapine as a bulk drug, in a commercially available preparation, and in in-house developed mucoadhesive microemulsion formulations and solution.

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

2011 ◽  
Vol 2011 ◽  
pp. 1-6 ◽  
Author(s):  
S. B. Bari ◽  
A. R. Bakhshi ◽  
P. S. Jain ◽  
S. J. Surana
Keyword(s):  
High Performance ◽  
Linear Regression Analysis ◽  
Analysis Data ◽  
Solvent System ◽  
Mean Value ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Ich Guidelines ◽  
Bulk Drug ◽  
Development And Validation

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.

scholarly journals Validation of an RP-HPLC Method for the Determination of Asenapine Maleate in Dissolution Media and Application to Study In Vitro Release from Co-Crystals

2021 ◽  
Vol 89 (1) ◽  
pp. 14
Author(s):  
Suhair S. Al-Nimry ◽  
Mai S. Khanfar
Keyword(s):  
In Vitro Release ◽  
Bipolar Disorders ◽  
Aqueous Solubility ◽  
Hplc Method ◽  
In Vitro Dissolution ◽  
Rp Hplc ◽  
Limit Of Quantitation ◽  
Vitro Release

Asenapine maleate is an antipsychotic drug that is indicated in the treatment of schizophrenia and bipolar disorders. It has low aqueous solubility and high permeability (Class II drug) and undergoes an extensive first pass effect. These problems result in low oral bioavailability (<2%). To enhance its solubility/dissolution rate and hence bioavailability, co-crystals using different co-formers in different ratios were prepared and evaluated. To study the in vitro dissolution of the drug from these co-crystals into phosphate buffer (pH 6.8), an RP-HPLC method was developed and validated according to the ICH Q2R1 guidelines. The method was linear in the range 0.1–14 µg/mL (R > 0.9998) and accurate and precise. An ANOVA test indicated that calibration curves run on different days did not differ significantly. It was sensitive (lower limit of quantitation (LLOQ) = 25.03 ng/mL), specific (the co-formers did not interfere with the determination of the drug), and robust to small changes in the mobile phase (pH, composition, and flow rate). The in vitro release of asenapine maleate from the co-crystals and the physical mixture was much enhanced when compared to the in vitro dissolution of the unprocessed drug. In conclusion, the developed and validated RP-HPLC method met the acceptance criteria and was applied successfully in evaluating the in vitro release of the drug.

Development and validation of an in vitro release method for topical particulate delivery systems

2015 ◽  
Vol 485 (1-2) ◽  
pp. 202-214 ◽  
Author(s):  
Maja Lusina Kregar ◽  
Marjana Dürrigl ◽  
Andrea Rožman ◽  
Želimir Jelčić ◽  
Biserka Cetina-Čižmek ◽  
...  
Keyword(s):  
In Vitro Release ◽  
Delivery Systems ◽  
Particulate Delivery ◽  
Development And Validation ◽  
Release Method ◽  
Vitro Release

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

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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