scholarly journals Assay of Clopidogrel by Using HPLTC Method

Author(s):  
D. S. Ghotekar ◽  
Vishal N. Kushare

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 (<em>R</em><sub>f</sub>value 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 <em>r</em>2 = 0.888 with respect to peak area in the concentration range 30 - 120 ng/spot.

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (12) ◽  
pp. 42-48
Author(s):  
P. J. Patel ◽  
◽  
D. A Shah ◽  
F. A. Mehta ◽  
U. K. Chhalotiya

A simple, sensitive and precise high performance thin layer chromatographic (HPTLC)method has been developed for the estimation of ondansetron (OND) and ranitidine (RAN) in combination. The method was employed on thin layer chromatography (TLC) and aluminium plates were precoated with silica gel 60 F254 as the stationary phase, while the solvent system was methanol. The Rf values were observed to be 0.5 ± 0.02, and 0.3 ± 0.02 for OND and RAN, respectively. The separated spots were densitometrically analyzed in absorbance mode at 299 nm. This method was linear in the range of 25-300 ng/band for OND and 50-600 ng/band for RAN. The limits of detection for OND and RAN were found to be 3.47 and 1.83 ng/band, respectively. The limits of quantification for OND and RAN were found to be 10.53 and 5.55 ng/band, respectively. The proposed method was validated with respect to linearity, accuracy, precision and robustness. The method was successfully applied to the estimation of OND and RAN in combined dosage form.


Author(s):  
D. S. Ghotekar ◽  
Vishal N. Kushare

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 (<em>R</em><sub>f</sub>value 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 <em>r</em>2 = 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.


2020 ◽  
Vol 13 (1) ◽  
pp. 37-43
Author(s):  
Balu S. Khandare

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.


2020 ◽  
Vol 13 (1) ◽  
pp. 054-061
Author(s):  
Iman Tagelsir Abdalla Mohamed ◽  
Wasim Khan ◽  
Karishma Chester ◽  
Abdelwahab Hassan Mohamed ◽  
Sayeed Ahmad ◽  
...  

Background: Solanum dubium is a plant believed to have several therapeutic effects including anti-asthmatic properties. The objective of this study was to investigate the quantitative estimation of Gallic acid and Ellagic acid from the seed extract of Sudanese Solanum dubium. Methods: A simple and rapid high-performance thin-layer chromatographic method was developed and validated for quantitative estimation of Gallic acid and Ellagic acid from the seed extract of Sudanese Solanum dubium. Results: Ellagic acid and Gallic acid were quantified by using HPTLC. The seeds were found to contain 1.1% w/w of Ellagic acid and 2.1% w/w of Gallic acid in extract. Gallic acid and Ellagic acid were chromatographed on silica gel 60 F254 TLC plate using Toluene: Ethyl acetate – Methanol – Formic acid (3:3:1:0.4 v/v/v/v) as mobile phase and quantified by densitometric scanning at 280 nm. The method was found to give compact spots for Gallic acid (Rf 0.35) and Ellagic acid (Rf 0.21). The linear regression analysis data for standard Gallic and Ellagic acids spots showed good linear relationship with r2 = 0.988 and 0.994 respectively, in the concentration range 100-3000 ng/spot, accurate (99.23-102.7%), (98.7-100.2%); precise (% RSD ≤ 2); robust (% RSD ≤ 2) and specific. The LOD and LOQ of the method were found as 653 and 396.8ng/spot and 215.5and 130 ng/spot, of Gallic acid and Ellagic acid respectively. Conclusion: The method was validated for precision, recovery and repeatability as per the International Conference on Harmonization Guidelines for Gallic acid and Ellagic acid. Statistical analysis of the data showed that the method is precise, accurate, reproducible and selective for the analysis of Gallic acid and Ellagic acid.


1999 ◽  
Vol 82 (4) ◽  
pp. 825-829 ◽  
Author(s):  
Danica Agbaba ◽  
Tatjana Miljkovic ◽  
Valentina Marinkovic ◽  
Dobrila Zivanov-Stakic ◽  
Sote Vladimirov

Abstract A simple and reliable thin-layer chromatographic method for determining sulpiride and impurities of 2-aminomethyl-1-ethylpyrrolidine and methyl-5-sulphamoyl-2-methoxybenzoate was developed and validated. A methylene chloride–methanol–ammonia solution (25%; 18 + 2.8 + 0.4, v/v) solvent system is used for separation and quantitative evaluation of chromatograms. The chromatographic plate is first scanned at 240 nm to locate chromatographic zones corresponding to sulpiride and methyl-5-sulphamoyl-2-methoxybenzoate. Then 2-aminomethyl-1-ethylpyrrolidine is derivatized in situ with ninhydrin, and resulting colored spots are measured at 500 nm. The method is reproducible and convenient for quantitative analysis and purity control of sulpiride in its raw material and in its dosage forms.


Pteridines ◽  
1994 ◽  
Vol 5 (2) ◽  
pp. 49-54 ◽  
Author(s):  
Peter Mayersbach ◽  
Roman Augustin ◽  
Harald Schennach ◽  
Dietmar Fuchs ◽  
Ernst R. Werner ◽  
...  

Summary We have evaluated a new commercially available enzyme-linked immunorsorbant assay for neopterin :or its suitability in the context of screening of voluntary blood donors. The assay was performed on 1040 consecutive blood donors, and compared with radioimmunoassay and. in a fraction of 142 donors . . : Iso with high performance liquid chromatography. On repetitive assays of all donations showing a concentration exceeding 8.0 nmol/L in the initial assay. three of the radioimmunoassay results were identified as gross outliers. No such gross outliers were detected for the enzyme-linked immunosorbant assay. RegarJing the reproducibility of results exceeding a cut-off limit of \0 nmol/L neopterin. the enzyme-linked ;mmunosorbant assay was better than the radioimmunoassay. Moreover. the enzyme-linked immunosorbant assay was slightly superior to radioimmunoassay when both tests were compared with high performance liquid chromatography (based on linear regression analysis. evaluation of frequencies of concentrations bant assay was slightly superior to radioimmunoassay when both tests were compared with high performance liquid chromatography (based on linear regression analysis. evaluation of frequencies of concentrations rations. Its slight superiority compared to the conventional radioimmunoassay likely results from the higher degree of automatization employed.


Author(s):  
Pratheema Philomindoss

Objective: The present study is designed to develop a new simple, precise, rapid and selective high‐performance thin‐layer chromatographic (HPTLC) method for the determination of stigmasterol in methanolic rhizomes extract of Alpinia calcarata.Methods: As per International Conference on Harmonization (ICH) guidelines we have applied different concentrations of stigmasterol as standard on HPTLC plates for the quantification of stigmasterol from the Alpinia calcarata rhizomes. The concentration of standard stigmasterol is 1 mg/ml.Results: The retention factor of stigmasterol was 0.58. Linearity was obtained in the range of 50 ng‐250 ng for stigmasterol. The developed and validated HPTLC method was employed for stigmasterol in methanolic rhizomes extract of Alpinia calcarata for standardization of the content of the marker. The linear regression data for the calibration plots showed a good linear relationship with r=0.99977 for stigmasterol, respectively Satisfactory recoveries of 99.77 % were obtained for stigmasterol.Conclusion: The results obtained in validation assays indicate the accuracy and reliability of the developed HPTLC method for the quantification of stigmasterol in methanolic rhizomes extract of Alpinia calcarata


2012 ◽  
Vol 2012 ◽  
pp. 1-7 ◽  
Author(s):  
Atul S. Rathore ◽  
Lohidasan Sathiyanarayanan ◽  
Kakasaheb R. Mahadik

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.


Sign in / Sign up

Export Citation Format

Share Document