The determination of vitamin D in pharmaceutical preparations by thin-layer chromatography

The Analyst ◽  
1964 ◽  
Vol 89 (1061) ◽  
pp. 529 ◽  
Author(s):  
L. T. Heaysman ◽  
E. R. Sawyer
2019 ◽  
Vol 12 (4) ◽  
pp. 183 ◽  
Author(s):  
Wioletta Parys ◽  
Alina Pyka-Pająk ◽  
Małgorzata Dołowy

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.


2005 ◽  
Vol 88 (5) ◽  
pp. 1537-1543 ◽  
Author(s):  
Caitlin Sullivan ◽  
Joseph Sherma

Abstract A new quantitative method using silica gel high-performance thin-layer chromatography plates with channels and a concentration zone, manual application of standards and samples, development with methanol–ethyl acetate (15 + 85) mobile phase, and ultraviolet absorption densitometry is reported for the determination of caffeine in diuretic pharmaceutical preparations. Tablet and capsule products containing potassium salicylate, acetaminophen, and salicylamide as active ingredients were analyzed to test the applicability of the new method, and precision, accuracy, linearity, limits of detection and quantitation, and selectivity were validated. The milligrams of caffeine in each tablet ranged from 48.0 to 51.0, and the milligrams in each capsule from 37.9 to 40.3. Within-day precision was 1.48 and 1.78% (n = 6), and interday precision 0.723 and 1.26% (n = 5) for analysis of 2 tablets and 2 capsules, respectively. Accuracy validation of the tablet and capsule results produced errors of 1.0 and 1.9% for spiked blank analyses and 2.6 and 3.5% for standard addition analyses, respectively. A comparative study using a caffeine standard solution and a multicomponent analgesic tablet solution containing caffeine, acetaminophen, and acetylsalicylic acid showed that manual application on the concentration zone, instrumental application on the concentration zone, and instrumental application on the silica gel gave quite similar results in terms of number of theoretical plates, resolution, limit of detection, and linearity.


Author(s):  
Tiara Fitrizal ◽  
Sestry Misfadhila ◽  
Harrizul Rivai

Chlortalidone is a compound that is often used in the pharmaceutical world as an oral drug to treat hypertension. This review article discusses the summary of methods for determining the concentration of chlorthalidone in pharmaceutical preparations and biological matrices. We took the data collected in this review article was taken through trusted sites such as Google Scholar with the search keywords "chlorthalidone determination," "pharmaceutical preparations," and "biological matrices," with a period of the last twenty years (2001-2021). This review article aims to provide an overview of the assay used to determine the concentration of chlorthalidone either in the form of a single substance or pharmaceutical dosage forms. Overall, the determination of chlorthalidone levels has been carried out using various analytical methods. Including spectrophotometry, high-performance liquid chromatography (HPLC), chemometrics and thin-layer chromatography (TLC) - densitometric, capillary zone electrophoresis (CZE) methods, spectrofluorimetric methods, liquid chromatography-mass spectrometry-mass spectrometry (LC-MS-MS) methods, ultrafast liquid chromatography (UFLC), supercritical fluid chromatography method and high-performance thin-layer chromatography (HPTLC)-densitometric method. Analysis with the HPLC technique is widely used in research because it can detect samples with the lowest concentrations up to the nanogram level.


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