Deoxynivalenol in Winter Wheat: Thin Layer Chromatographic Method and Survey

1984 ◽  
Vol 67 (1) ◽  
pp. 43-45 ◽  
Author(s):  
Robert M Eppley ◽  
Mary W Trucksess Stanley Nesheim ◽  
Charles W Thorpe ◽  
Garnett E Wood ◽  
Albert E Pohland

Abstract A rapid method for the determination of deoxynivalenol (DON) in wheat was used to analyze 57 wheat samples collected from 4 midwestern states where the winter wheat crop was contaminated with Fusaria. The method involves sample extraction with acetonitrilewater (84 + 16), cleanup by charcoal-alumina column chromatography, and determination by thin layer chromatography (TLC), using an AlClj solution spray and heat to form a fluorescent derivative. Recoveries of DON added to wheat at levels as low as 0.2 μg/g averaged >80%. DON was detected at an average level of 3.6 μg/g; the levels ranged from 0.2 to 9.0 μg/g in 54 of 57 of the wheat samples. The quantity of DON was, in general, proportional to the percentage of total damaged kernels (grade). The chemical identity of DON was confirmed by mass spectrometry after isolation with preparative TLC.

1986 ◽  
Vol 69 (1) ◽  
pp. 37-40 ◽  
Author(s):  
Robert M Eppley ◽  
Mary W Trucksess ◽  
Stanley Nesheim ◽  
Charles W Thorpe ◽  
Albert E Pohland ◽  
...  

Abstract A collaborative study of a rapid method for the determination of deoxynivalenol (DON) in winter wheat was successfully completed. The method involves sample extraction with acetonitrile-water (84 + 16), cleanup using a disposable column of charcoal, Celite, and alumina, and detection by thin layer chromatography after spraying with an aluminum chloride solution. Each of the 15 collaborators analyzed 12 samples, 2 of which were naturally contaminated, and 10 to which DON was added, in duplicate, at levels of 0,50,100,300, and 1000 ng/ g. Average recoveries of DON ranged from 78 to 96% with repeatabilities of 30-64% and reproducibilities of 33-87%. The results of the study show that false positives were not a problem and that all of the analysts could detect DON at the 300 ng/g level or higher. The method has been adopted official first action.


1967 ◽  
Vol 50 (3) ◽  
pp. 680-682
Author(s):  
Laura A Roberts

Abstract Eight collaborators studied a fluoromelric and thin layer chromatographic method for aminacrine and its salts in powder and cream drug preparations. Recovery of aminacrine.HCI by fluorometer in both preparations averaged 100% for powder and 102% for cream. The mean concentration of aminacrine.HCI found in the powder was 0.108% with a standard deviation of ± 0.001%. The mean concentration of aminacrine found in the cream was 0.191% with a standard deviation of ± 0.003%. Seven of the 8 collaborators successfully used thin layer chromatography to identify the aminacrine in both sample forms supplied. The assay method for aminacrine and its salts in drug preparations is recommended for adoption as official, first action


Author(s):  
Nilcan Altınbaş ◽  
Mahir Aydın ◽  
İrem Özmen ◽  
Barış Çaldağ ◽  
Levent Şaylan

1974 ◽  
Vol 57 (3) ◽  
pp. 621-625 ◽  
Author(s):  
Peter M Scott

Abstract Collaborators in 20 laboratories studied a method for the determination of patulin in apple juice. The collaborators mixed patulin solutions with the apple juice to obtain 9 spiked samples (of which 2 were blanks) and 1 practice sample. After column chromatography of the apple juice extract, patulin was estimated visually by thin layer chromatography, using 3-methyl-2-benzothiazolinone hydrazone.HCl as the spray reagent. Mean recoveries of patulin ranged from 69.8 to 98.3% for 3 contamination levels. The method has been adopted as official first action for the determination of patulin in apple juice.


2000 ◽  
Vol 83 (6) ◽  
pp. 1484-1488
Author(s):  
Shaifali Srivastava ◽  
Madan M Gupta ◽  
Ram K Verma ◽  
Sushil Kumar

Abstract A new, simple, precise, and rapid high-performance thin-layer chromatographic method was developed for the determination of 6 benzodioxanes in Piper mullesua extract: 1′,3′-benzodioxole-5′-(2,4,8-triene-isobutyl nonanoate), 1′,3′-benzodioxole-5′-(2,4,12-triene-isobutyl tridecanoate), fargesin, sesamin, asarinin, 1′,3′-benzodioxole-5′-(2,4,8-triene-methyl nonanoate). The ingredients were separated on a precoated Silica Gel 60 F254 plate with a solvent system of toluene–acetone (92 + 8). The 6 benzodioxanes were well separated and easily identified in this chromatographic system. The separated benzodioxanes were visualized by color development with a spray reagent consisting of 1 g vanillin dissolved in 100 mL H2SO4–ethanol (5 + 95, v/v). Quantitation was performed by scanning the spots and comparing the integrated areas of compounds in samples with those of standards. Recoveries from samples spiked with known amounts of the benzodioxanes were excellent. The results were comparable with those estimated by liquid chromatography.


1968 ◽  
Vol 14 (7) ◽  
pp. 595-609 ◽  
Author(s):  
Irving Sunshine ◽  
Robert Maes ◽  
Rosalie Faracci

Abstract A gas chromatographic method for the quantitative determination of glutethimide was developed. This method was applied to samples obtained from patients who were comatose because of acute glutethimide intoxication. The results obtained from this procedure were compared with those obtained by using an ultraviolet method. The patients’ clinical conditions were assessed and correlated with the blood concentrations of glutethimide. The samples were processed to isolate glutethimide, as well as its metabolites. The metabolites were separated using thin-layer chromatography and were checked for purity by both thin-layer and gas chromatography.


2020 ◽  
Vol 6 (4) ◽  
pp. 198-204
Author(s):  
S. Veliyeva

Infield experiments on light chestnut soils of Mountain Shirvan, the effect of the dose and the ratio of organic and mineral fertilizers on nitrogen removal from aboveground biomass, grain quality, crop yield and economic efficiency in winter wheat crops were studied. The work was carried out in 2011–2014. During the work, standard methods for the determination of chemicals were used. As a result, the work is established. That high yield and net income were obtained in option N90P60K60.


1967 ◽  
Vol 45 (4) ◽  
pp. 531-539 ◽  
Author(s):  
R. S. Mathur ◽  
R. H. Common

Presumptive estriol and 16,17-epiestriol fractions were separated from laying hens' urine by subjecting the hydrophilic fraction of the urinary phenolic extract to successive thin-layer chromatography (t.l.c), alumina-column chromatography, further t.l.c, and finally, microsublimation. The presence of estriol in the presumptive estriol fraction was confirmed by comparison of the thin-layer chromatographic behaviors of the phenol and four derivatives thereof with the behaviors of reference estriol and four corresponding derivatives of this reference material each in three different solvent systems. The presence of 16,17-epiestriol in the presumptive 16,17-epiestriol fraction was confirmed by similar comparisons of the presumptive 16,17-epiestriol fraction and five derivatives thereof with reference 16,17-epiestriol and five corresponding derivatives each in three solvent systems; and chromatographic correspondences for two further derivatives were observed in one solvent system each.It is concluded that estriol and 16,17-epiestriol are normal constituents of hens' urine.


1980 ◽  
Vol 37 (6) ◽  
pp. 1038-1040 ◽  
Author(s):  
Doris V. Herbst

Residues of vancomycin in cooked lobster meat were detected by using a thin-layer chromatographic method with bioautography. Presumptive identification was provided by the Rf value coupled with the unique zone of inhibition, and residue levels of 5 μg/g could be detected. The procedure provides methodology needed for regulatory purposes.Key words: lobster meat, vancomycin, bioautography, thin-layer chromatography


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