Determination of 3-Methoxy-4-Hydroxymandelic Acid (VMA) in Urine by Thin-Layer Chromatography

1965 ◽  
Vol 11 (10) ◽  
pp. 905-913 ◽  
Author(s):  
J S Annino ◽  
M Lipson ◽  
L A Williams

Abstract From studies of several variables, a method has been developed for the separation and quantitation of 3-methoxy-4-hydroxymandelic acid (VMA) in urine by thin-layer chromatography. The urine is pretreated with acid and Florisil, and then extracted with ethyl acetate. Thin-layer chromatography is performed on silica gel with a butanol: acetic acid:water solution. The VMA spot is located by spraying with fast red GG and potassium carbonate. After removal from the plate, maximum color is developed and quantitated by reading in a spectrophotometer at 510 mµ.

1973 ◽  
Vol 56 (4) ◽  
pp. 813-816 ◽  
Author(s):  
Peter M Scott ◽  
Barry P C Kennedy

Abstract Apple juice from a freshly opened container is extracted 3 times with ethyl acetate. The extract is dried, concentrated, diluted with benzene, and added to a silica gel column. Patulin is eluted by benzene-ethyl acetate (75+25) and detected by thin layer chromatography, using a 3-methyl-2-benzothiazolinone hydrazone hydrochloride solution as the spray reagent. Satisfactory recoveries were obtained for patulin added to apple juice at levels of 25–400 μg/L.


1982 ◽  
Vol 28 (2) ◽  
pp. 259-261 ◽  
Author(s):  
G. R. F. Davis ◽  
N. D. Westcott ◽  
J. D. Smith ◽  
G. A. Neish ◽  
H. B. Schiefer

An isolate of Fusarium sporotrichioides Sherbakoff obtained from hay from Kindersley, Saskatchewan, and producing metabolites toxic to insect larvae, rats, and mice was cultured on sterile rye grain and extracted with ethyl acetate. The most toxic fraction derived from column chromatography on silica gel was purified by thin-layer chromatography on silica gel and elution of the main band. This compound was identified as T-2 toxin by comparison with the pure chemical by thin-layer chromatography and, after crystallization, by determination of melting point, infrared spectrum, and nuclear magnetic resonance spectrum. This work demonstrates that strains of F. sporotrichioides capable of producing T-2 toxin may be present on hay in western Canada.


1981 ◽  
Vol 64 (4) ◽  
pp. 964-968
Author(s):  
Robert D Stubblefield ◽  
Odette L Shotwell

Abstract A method for the determination of aflatoxins in animal tissues has been developed, and applied successfully to beef, swine, chicken, and human livers, and to beef kidney, heart, spleen, muscle, and blood. Blended tissue is denatured with citric acid and extracted with dichloromethane on a wrist-action shaker. After filtration, the extract is partially purified on a silica gel column, and aflatoxins B1 and M1 are determined by 2-dimensional thin layer chromatography and densitometry. Recoveries of Bi and Mi added to meat tissues and blood were approximately 90 and 80%, respectively. The method gave results for a contaminated freeze-dried liver comparable to analyses by 3 other published meat tissue methods. The method is rapid and has a determination limit ≤0.1 ng/g. In addition, the method uses less toxic and smaller quantities of solvents and chemicals.


Author(s):  
Dewi Umniyatul ◽  
Dwi Kurniawati Sambodo

Background: Traditional herbs are ingredients or herbs in the form of plant material, animal ingredients, mineral ingredients, galenic preparations or mixtures of these ingredients, it has been used as medicine traditionally.Objective: This study is aimed to Identify of Sildenafil Citrate on “Jamu Kuat” (Herbal Medicine) products.Methods: This type of research was descriptive and the sample was determined by quota sampling. The method used Thin Layer Chromatography (TLC) which was a physicochemical method. There were seven samples were extracted by the soxhletation method until a thick extract was obtained to be spotted in the quite phase of TLC silica gel F254. The motion phase used to identify sildenafil citrate was chloroform: ethyl acetate (6: 4). Spots detection was done by observation under UV light 366 nm and the spots that appeared were calculated of Rf value and compared with the comparable Rf value of sildenafil citrate.Results: From this study, there were samples containing sildenafil citrate. Sample C with a sample Rf value of 0.75 and sample D with Rf value of sample 0.78 and a comparable Rf of sildenafil citrate 0.77.Conclusion: The seven samples of “Jamu Kuat” contained sildenafil citrate in Banguntapan and Pleret Districts, Bantul Regency. Keywords: Jamu Kuat (Herbal Medicine), Sildenafil citrate, TLC


1970 ◽  
Vol 27 (3) ◽  
pp. 596-601 ◽  
Author(s):  
U. H. M. Fagerlund

A method was developed for the simultaneous determination of nanogram quantities of cortisol and cortisone in 0.1-ml samples of salmonid plasma by competitive protein binding (CPB). The steroids were separated by thin-layer chromatography on silica gel and CPB analysis was performed with chicken serum in the presence of Florisil.


2018 ◽  
Vol 1 (T5) ◽  
pp. 137-142
Author(s):  
Linh Thi My Lam ◽  
Phu Hoang Dang ◽  
Hai Xuan Nguyen ◽  
Nhan Trung Nguyen ◽  
Mai Thi Thanh Nguyen

From the wood of n-hexane extract of Willughbeia cochinchinensis, perform column chromatography on a normal phase silica gel with n-hexane: ethyl acetate obtained in 8 fractions. From GD-D and GD-F fractions, multiple column chromatography on silica gel was performed in combination with normal and reverse phase thin-layer chromatography, four triterpene compounds as epifriedelanol (1), taraxeryl acetate (2), ambolic acid (3) and α- amyrin (4) were isolated. Their chemical structures were determined by spectrocopic methods as well as comparing with data in the literature. These compounds were isolated for the first time from Willughbeia cochinchinensis.


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.


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