Thin Layer Chromatographic Determination of Aflatoxin in Corn Dust

1981 ◽  
Vol 64 (5) ◽  
pp. 1060-1063 ◽  
Author(s):  
Odette L Shotwell ◽  
William R Burg ◽  
Thomas Diller

Abstract Methods adopted by the AOAC and the American Association of Cereal Chemists for determining aflatoxin in corn were modified, and techniques were developed for application to samples of <1 to 10 g instead of the specified 50 g samples. Analysis included chloroform extraction of dust samples or dust collected from glass fiber filters, purification of extracts on a silica gel column of appropriate size, and measurement of aflatoxin by either 1- or 2-dimensional thin layer chromatography (TLC). The solvent for 1-dimensional TLC was chloroform-acetonewater (91 + 9 + 1). Solvents for 2-dimensional TLC were, first direction, ether-methanol-water (95 + 4 + 1, lined tank) and second direction, chloroformacetone- water (91 + 9 + 1, unlined tank), or first direction, chloroform-acetone-water (91 + 9 + 1, unlined tank) and second direction, toluene-ethyl acetate- formic acid (60 + 30 + 10, unlined tank). When samples weighed ≤0.1 g, the entire concentrated extract was applied to the TLC plate. About 0.5-1.0 ng aflatoxin B1 could be detected on the plate, making the limit of detection about 9 ng/g for 0.1 g samples.

1978 ◽  
Vol 61 (6) ◽  
pp. 1363-1365
Author(s):  
Per E Häggblom ◽  
Howard H Casper

Abstract A procedure is described for the purification and quantitation of aflatoxin B1 in corn silage. The toxin is extracted and partially purified using parts of the AOAC minicolumn detection method. The extract is further cleaned up on a 2-step minicolumn and is then analyzed by using thin layer chromatography. Essentially all interferences are removed when the procedure is applied to moldy and non-moldy corn silage. The estimated limit of detection is 5 μg aflatoxin B1/kg corn silage, and 73±8% of the added aflatoxin B1 (20 and 85 μg/kg) was recovered. No aflatoxin B1 was detected in 270 samples collected from 19 silage piles in late fall 1976 and early spring 1977. This procedure also removes interferences associated with moldy corn and mixed feeds.


1983 ◽  
Vol 66 (1) ◽  
pp. 85-91 ◽  
Author(s):  
Alberto Gimeno ◽  
Maria Ligia Martins

Abstract A method is described to determine the mycotoxins patulin, citrinin, and aflatoxins in apples and pears and their juices and jams. The mycotoxins are extracted with a mixture of acetonitrile and 4% aqueous KG (9 +1). The extract is cleaned up with water and then acidified, and the toxins are recovered with chloroform and separated by thin layer chromatography. Toxin identity is confirmed with various developing solvents, spray reagents, and chemical reactions, and then quantitated by the limit of detection method. The minimum detectable concentrations of the mycotoxins are patulin, 120-130 μg/kg; citrinin, 30-40 μg/kg; aflatoxin B1 or G1 , 2-2.8 μg/kg; af latoxin B2 or G2,2 μg/kg.


1985 ◽  
Vol 68 (5) ◽  
pp. 952-954
Author(s):  
Maria Luisa Serralheiro ◽  
Maria Lurdes Quinta

Abstract A method has been developed for the detection of aflatoxin Mi in milk. The toxin is extracted with chloroform, the extract is evaporated, and the residue is partitioned between carbon tetrachloride and an aqueous saline-methanol solution. The toxin is once again extracted with chloroform from the methanol solution and analyzed by thin layer chromatography. The limit of detection of Mi in powdered milk is 0.5 μg/ kg; recoveries of added Mj are about 83%. The limit of detection can be improved to 0.3 μg/kg if the plate is sprayed with an aqueous solution of H2S04 after development.


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.


1978 ◽  
Vol 61 (3) ◽  
pp. 581-583
Author(s):  
Thirugnana Subramanian ◽  
Kuppuswamy Mohan Namasivayam ◽  
Edayathimangalam R B Shanmugasundaram

Abstract Two methods have been developed for determining terreic acid, which is a mycotoxin produced by Aspergillus terreus, a common food contaminant. The organism was grown independently in synthetic minimal medium, bread, and rice. After 15 days of growth, the toxin was extracted with ethyl acetate, cleaned up by thin layer chromatography, and determined colorimetrically, using Folin's reagent or 2,4- dinitrophenylhydrazine. The production of terreic acid was greater on bread than on rice or minimal medium. Recoveries of 200–400 ≧g terreic acid/100 g bread and rice ranged from 62 to 98%. The lower limit of detection was 200 ≧g/100 g.


1984 ◽  
Vol 67 (3) ◽  
pp. 611-612
Author(s):  
Bernard Le Tutour ◽  
Abdelrhafour Tantaoui-Elaraki ◽  
Abdelhadi Aboussalim

Abstract A screening method has been developed for simultaneous determination of aflatoxin B1 and ochratoxin A in black olives. The technique includes extraction of both mycotoxins with aqueous methanol, cleanup using lead acetate, defatting with hexane, partitioning in chloroform, and thin layer chromatography. Detection limits are 5–7 μg aflatoxin B1 and 20 μg ochratoxin A/kg.


2021 ◽  
Vol 10 (4) ◽  
pp. 2804-2809

Thymus species belong to the Lamiaceae family, of which 18 species in the flora of Iran, 6 are endemic to Iran. In the current research, high-performance thin-layer chromatography (HPTLC) technique as an easy, fast, reproducible, and low-cost method was used for the determination of rosmarinic acid and caffeic acid in Thymus lancifolius (T. lancifolius) and two species of Thymus daenensis (T. daenensis) from Iran. Toluene-ethyl acetate-formic acid with a ratio of 67.72-22.90 and 9.38% was selected as the mobile phase of rosmarinic acid, and ethyl acetate-methanol-formic acid-water with a ratio of 85-8-2 and 5% was designated as the mobile phase of caffeic acid. The highest and lowest amount of rosmarinic acid was observed for T. daenensis 1 (10.54±0.12 mg/g) and T. lancifolius (0.46±0.01 mg/g), respectively. The amount of rosmarinic acid for T. daenensis 2 was obtained as 7.85±0.02 mg/g for each of the dried plants. In the following, HPTLC analysis of caffeic acid for T. daenensis 1, T. daenensis 2, and T. lancifolius was acquired amounts of 0.78±0.007, 0.13±0.007, and 0.26±0.007 mg/g for each of dried plants, respectively. Therefore, regarding the special effects of phenolic acids and properties of the Thymus genus, the acquired results are suitable for application in pathogenic research, infections, immunology diseases, and evaluation of the antioxidant activity.


1980 ◽  
Vol 63 (1) ◽  
pp. 1-4 ◽  
Author(s):  
Miroslav Dadic ◽  
Joris E A Van Gheluwe ◽  
Robert L Weaver

Abstract Free gallic acid and total gallotannins are determined in wine and cider by thin layer densitometry. The beverage is extracted with ethyl acetate and the extract is subjected to thin layer chromatography on silica gel. After elution with chloroform-ethyl formate-formic acid (50+40+ 10), the dry plate is sprayed uniformly with a freshly prepared solution of 0.3% aqueous FeCl3 and 0.3% aqueous K3FeCN6. If the gallic acid spot appears (Rf 0.28), densitometry readings are taken at 600 nm, and free gallic acid (GAF) is calculated from the formula GAF = GA (μg, from calibration curve) × 1.25. The calibration curve was obtained by plotting thin layer densitometric readings at 600 nm (prussian blue) vs. μg gallic acid. In a second method, the beverage is hydrolyzed, and extraction and densitometry are performed as before to give “total gallic acid after hydrolysis:” GAH (mg/L) = GA (μg, from calibration curve) × 25. Total gallotannins (GALLT) are calculated from the formula: GALLT (mg/L) = GAH – GAF. Results for 10 wines and 5 ciders are presented and briefly discussed.


Author(s):  
Kamran Ashraf ◽  
Syed Adnan Ali Shah ◽  
Mohd Mujeeb

<p><strong>Objective: </strong>A simple, sensitive, precise, and accurate stability indicating HPTLC (high-performance thin-layer chromatography) method for analysis of 10-gingerol in ginger has been developed and validated as perICH guidelines.</p><p><strong>Methods: </strong>The separation was achieved on TLC (thin layer chromatography) aluminum plates pre-coated with silica gel 60F<sub>254</sub> using n-hexane: ethyl acetate 55:45 (%, v/v) as a mobile phase. Densitometric analysis was performed at 569 nm.</p><p><strong>Results: </strong>This system was found to have a compact spot of 10-gingerol at <em>R</em><sub>F</sub> value of 0.57±0.03. For the proposed procedure, linearity (<em>r</em><sup>2</sup> = 0.998±0.02), limit of detection (18ng/spot), limit of quantification (42 ng/spot), recovery (ranging from 98.35%–100.68%), were found to be satisfactory.</p><p><strong>Conclusion: </strong>Statistical analysis reveals that the content of 10-gingerol in different geographical region varied significantly. The highest and lowest concentration of 10-gingerol in ginger was found to be present in a sample of Patna, Lucknow and Surat respectively which inferred that the variety of ginger found in Patna, Lucknow are much superior to other regions of India.</p>


1964 ◽  
Vol 47 (5) ◽  
pp. 801-803 ◽  
Author(s):  
Peter John Andrellos ◽  
George R Reid

Abstract Three confirmatory tests have been devised to identify aflatoxin B±. Portions of the isolated toxin are treated with formic acid-thionyl chloride, acetic acid-thionyl chloride, and trifluoroacetic acid, respectively, and aliquots of the three fluorescent reaction products are spotted on thin-layer chromatography plates. Standards treated with each of the three reagents, plus an untreated standard, are spotted on the same plate, and after development the spots are compared under ultraviolet light.


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