scholarly journals Simultaneous Densitometric Determination of Indomethacin and Its Degradation Products, 4-Chlorobenzoic Acid and 5-Methoxy-2-Methyl-3-Indoleacetic Acid, in Pharmaceutical Preparations

2001 ◽  
Vol 84 (6) ◽  
pp. 1703-1707 ◽  
Author(s):  
Jan Krzek ◽  
Magorzata Starek
Keyword(s):  
Detection Limit ◽  
Thin Layer ◽  
Mobile Phase ◽  
Indoleacetic Acid ◽  
Degradation Products ◽  
Pharmaceutical Preparations ◽  
Chlorobenzoic Acid ◽  
Rf Values ◽  
Layer Chromatography

Abstract A densitometric method was developed for the identification and determination of indomethacin and its degradation products, 4-chlorobenzoic acid and 5-methoxy-2-methyl-3-indoleacetic acid, in pharmaceuticals. To separate these compounds, silica gel-coated thin-layer chromatography plates and the following mobile phase were used: 2-propanol–25% ammonia–water (8 + 1 + 1, v/v). UV densitometric measurements were made by comparing the absorption spectra and Rf values of appropriate standards with the pharmaceutical preparations examined. The conditions for separation were established and a low detection limit was obtained. Average recoveries were 100.69, 90.09, and 91.17% for indomethacin, 4-chlorobeznzoic acid, and 5-methoxy-2-methyl-3-indoleacetic acid, respectively.

scholarly journals Application of Thin-Layer Chromatography in Combination with Densitometry for the Determination of Diclofenac in Enteric Coated Tablets

2019 ◽  
Vol 12 (4) ◽  
pp. 183 ◽  
Author(s):  
Wioletta Parys ◽  
Alina Pyka-Pająk ◽  
Małgorzata Dołowy
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Degradation Products ◽  
Low Cost ◽  
Diclofenac Sodium ◽  
Pharmaceutical Preparations ◽  
Pharmaceutical Products ◽  
Enteric Coated ◽  
Layer Chromatography

Diclofenac belongs to the drug class non-steroidal anti-inflammatory drugs widely used in Europe as well as all over the world. Thus, it is important to conduct research on its quality control of available pharmaceutical preparations like for example enteric coated tablets. Among various analytical techniques, thin-layer chromatography (TLC) is ideal for this task due to their short time analysis, ease of operation and low cost. Hence, the aim of this study was to develop the optimal conditions of analysis and quantitative determination of diclofenac sodium in enteric tablets by using TLC in combination with densitometry. Of all chromatographic systems tested, the best is the one which consists of silica gel 60F254 and cyclohexane: chloroform:methanol:glacial acetic acid (6:3:0.5:0.5 v/v) as the mobile phase, which allows the successful separation of examined diclofenac sodium as active component and the largest number (twelve) of its degradation products as potential impurities of its pharmaceutical products. This indicates that the newly developed method is more effective than previously reported assays by Starek and Krzek. Linearity range was found to be 4.00–18.00 μg/spot for diclofenac sodium. The results of the assay of enteric tablet formulations equals 98.8% of diclofenac sodium in relation to label claim is in a good agreement with pharmaceutical requirements.

scholarly journals Column and Thin-Layer Chromatographic Methods for the Simultaneous Determination of Acediasulfone in the Presence of Cinchocaine, and Cefuroxime in the Presence of Its Hydrolytic Degradation Products

2007 ◽  
Vol 90 (2) ◽  
pp. 405-413 ◽  
Author(s):  
Mohammad Abdul-Azim Mohammad ◽  
Nagwan H Zawilla ◽  
Fawzy M El-Anwar ◽  
Samir M El-Moghazy Aly
Keyword(s):  
Thin Layer ◽  
Simultaneous Determination ◽  
Mobile Phase ◽  
Degradation Products ◽  
Hydrolytic Degradation ◽  
Ammonium Hydroxide ◽  
Dosage Forms ◽  
Ultraviolet Detection ◽  
Layer Chromatography

Abstract Column liquid chromatography (LC) and thin-layer chromatography (TLC)densitometry methods are described for simultaneous determination of acediasulfone (Ace) and cinchocaine (Cinco). In the LC method, the separation and quantitation of the 2 drugs was achieved on a Zorbax C8 column (5 μm, 150 × 4.6 mm id) using a mobile phase composed of methanol-phosphate buffer, pH 2.5 (66 + 34, v/v), at a flow rate of 1 mL/min and ultraviolet detection at 300 and 327 nm for Ace and Cinco, respectively. The method showed linearity over concentration ranges of 20-200 and 45685 μg/mL, respectively. In the TLCdensitometry method, a mobile phase composed of methanol-tetrahydrofuran-acetic acid (45 + 5 + 0.5, v/v/v) was used for the separation of the 2 drugs. The linearity range was 0.5-4 and 2-9 μg/spot, respectively. In addition, stability indicating TLCdensitometry method has been developed for determination of cefuroxime sodium in the presence of 570% of its known hydrolytic degradation products. The mobile phase butanol-methanol-tetrahydrofuran-concentrated ammonium hydroxide (50 + 50 + 50 + 5, v/v/v/v) was used. The concentration range was 210 g/spot. The optimized methods proved to be specific and accurate for the analysis of the cited drugs in laboratory-prepared mixtures and dosage forms. The obtained results agreed statistically with those obtained by the reference methods.

Recent Applications of High Performance Thin Layer Chromatography and Derivative Spectrophotometry in Pharmaceutical Analysis

2020 ◽  
Vol 16 (6) ◽  
pp. 671-689
Author(s):  
Marcin Gackowski ◽  
Marcin Koba ◽  
Katarzyna Mądra-Gackowska ◽  
Piotr Kośliński ◽  
Stefan Kruszewski
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Pharmaceutical Analysis ◽  
High Performance ◽  
Degradation Products ◽  
Derivative Spectrophotometry ◽  
Accuracy And Precision ◽  
Post Marketing ◽  
Layer Chromatography

At present, no one can imagine drug development, marketing and post-marketing without rigorous quality control at each stage. Only modern, selective, accurate and precise analytical methods for determination of active compounds, their degradation products and stability studies are able to assure the appropriate amount and purity of drugs administered every day to millions of patients all over the world. For routine control of drugs simple, economic, rapid and reliable methods are desirable. The major focus of current scrutiny is placed on high-performance thin layer chromatography and derivative spectrophotometry methods, which fulfill routine drug estimation’s expectations [1-4]. The present paper reveals state-of-the-art and possible applications of those methods in pharmaceutical analysis between 2010 and 2018. The review shows advantages of high-performance thin layer chromatography and derivative spectrophotometry, including accuracy and precision comparable to more expensive and time-consuming methods as well as additional fields of possible applications, which contribute to resolving many analytical problems in everyday laboratory practice.

IDENTIFIKASI DAN PENETAPAN KADAR RHODAMIN B DALAM KERUPUK BERWARNA MERAH YANG BEREDAR DI PASAR ANTASARI KOTA BANJARMASIN

2017 ◽  
Vol 1 (1) ◽  
pp. 85
Author(s):  
Eka Kumalasari
Keyword(s):  
Thin Layer ◽  
Rhodamine B ◽  
Textile Industry ◽  
Mobile Phase ◽  
Uv Lamp ◽  
Tapioca Flour ◽  
Red Dye ◽  
Layer Chromatography ◽  
Rhodamin B

Crackers are made from tapioca flour batter mixed with flavorings and colorings, still many outstanding crackers that contain ingredients banned dye Rhodamine B. Rhodamine B is a chemical used for red dye in the textile industry and plastic. Rhodamine B can cause cancer, poisoning, lung irritation, sore eyes, and sore throat. This study aims to identify and determination the levels of Rhodamine B in circulating red crackers Antasari market Banjarmasin.The population is that sold in the red crackers that sold in Antasari market Banjarmasin.. The sampling is technique incidental sampling , that is based on chance, so any population by chance met with researchers can be used as a sample. Identification of Rhodamine B was done by Thin Layer Chromatography (TLC) by using the stationary phase silica GF 254 and mobile phase is elution solvent is n-butanol, ethyl acetate, ammonia (10:4:5). Then detected with a UV lamp 254 nm and 366 nm. While for the determination of levels using Vis spectrophotometry at a wavelength of 544 nm.The results showed that the samples of 6 found one sample containing Rhodamine B, namely samples 5 (cassava crackers matches) and obtained values of 7,25 ± 3,8640 levels mg / kg. Based on these results, Rhodamine B still found in crackers that sold in the market Antasari Banjarmasin.

Additional Cleanup of Samples on GLC Column for TLC Determination of Pesticide Residues

1967 ◽  
Vol 50 (3) ◽  
pp. 615-623
Author(s):  
Kenneth T Hartman
Keyword(s):  
Liquid Chromatography ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Pesticide Residues ◽  
Gas Liquid Chromatography ◽  
Rf Values ◽  
Layer Chromatography

Abstract Gas-liquid chromatography (GLC) following conventional isolation procedures has been used to clean up pesticide residues for confirmation by thin layer chromatography (TLC). This procedure is more rapid and efficient than present cleanup procedures and permits the determination of pesticide residues that do not survive these rigorous acid or alkali treatments. The method also permits TLC confirmation of pesticide residues that have similar Rf values but different GLC retention times. Recoveries ranged from 85 to 105% for 25 of 28 pesticides tested

Comparison of Postcolumn Derivatization-Liquid Chromatography with Thin-Layer Chromatography for Determination of Aflatoxins in Naturally Contaminated Corn

1990 ◽  
Vol 73 (4) ◽  
pp. 579-581 ◽  
Author(s):  
Rodney W Beaver ◽  
David M Wilson ◽  
Mary W Trucksess
Keyword(s):  
Liquid Chromatography ◽  
Detection Limit ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Correlation Coefficient ◽  
Low Levels ◽  
Aflatoxin B2 ◽  
Layer Chromatography ◽  
Postcolumn Derivatization

Abstract Quantitation of aflatoxins by liquid chromatography with postcolumn iodine derlvatization (LC-PCD) and fluorescence detection was compared with quantitation by the AOAC CB method, 968.22. Thirty-seven naturally contaminated corn samples were ground and then divided. One portion was extracted, and the extract was cleaned up and analyzed by thin-layer chromatography according to the CB method. The second portion was extracted and cleaned up In a similar fashion, but quantitation was by the LC-PCD method. For aflatoxin B1, concentrations ranging from 0 to 150 ng/g, results obtained by the 2 methods were fitted to a linear equation with the LC-PCD results as the dependent variable. The correlation coefficient was 0.99, the Intercept was near 0, and the slope was near 1. For aflatoxin B2, the correlation coefficient was 0.97, and the Intercept was near 0. However, the slope of the equation relating LC-PCD concentration to TLC concentration was only 0.5. We believe that this lack of equivalence between the methods for determination of aflatoxin B2 is due to overestlmatlon by the TLC method because the low levels present are near the TLC detection limit for B2.

scholarly journals Determination of New Antidepressants in Pharmaceuticals by Thin-Layer Chromatography with Densitometry

2010 ◽  
Vol 93 (3) ◽  
pp. 778-782 ◽  
Author(s):  
Tatána Gondová ◽  
Iveta Petríková
Keyword(s):  
Thin Layer ◽  
Stationary Phase ◽  
Thin Layer Chromatography ◽  
Mobile Phase ◽  
Pharmaceutical Formulations ◽  
Simultaneous Separation ◽  
Tlc Plates ◽  
Precision And Accuracy ◽  
Layer Chromatography

Abstract A new and simple TLC-densitometry method has been developed for the simultaneous separation of the two noradrenergic and specific serotonergic antidepressants mirtazapine and mianserine and validated for their determination in commercially available tablets. The method used TLC plates precoated with silica gel 60F254 as the stationary phase, and the mobile phase consisted of hexaneisopropanol25 ammonia (70 + 25 + 5, v/v/v). Densitometric analysis was carried out in the absorbance mode at 280 nm. The method was validated in accordance with International Conference on Harmonization guidelines in terms of linearity, LOD, LOQ, precision, and accuracy. Calibration curves were linear (R2 > 0.9970) with respect to peak area in the concentration range of 5002500 and 5005000 ng/spot for mirtazapine and mianserine, respectively. The LODs were 20 and 35 ng/spot for mirtazapine and mianserine, respectively. The described method was successfully applied to the determination of mirtazapine and mianserine in their pharmaceutical formulations with recovery ranging from 99.83 to 101.20 of the labeled amount of the compounds. The proposed method can be used in routine QC of these drugs in pharmaceutical formulations.

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