Thin Layer Chromatographic Determination of Aflatoxin B1 in Corn Silage

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.


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.


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.


1981 ◽  
Vol 64 (6) ◽  
pp. 1356-1363 ◽  
Author(s):  
Mary V Howell ◽  
Philip W Taylor

Abstract A sensitive, reliable, and economical method for the determination of 6 mycotoxins in mixed feeds is described. The feed is extracted with chloroform-water and the extract is cleaned up by using a disposable Sep-Pak silica cartridge. The procedure requires less time (15 min from sample extraction to extract preparation) and less solvent (approximately one-tenth) compared with conventional methods and is suitable for a fast, economical screen. Additional cleanup procedures, involving dialysis or extraction into base, are described for samples containing high levels of interfering compounds. Thin layer chromatography (TLC) and high performance liquid chromatography (HPLC) with fluorescence detection are described for identification and estimation of mycotoxins. The method has been applied to a wide range of mixed feeds, including laboratory animal diets, and raw materials. The limit of detection is 1 μg/kg for all mycotoxins measured by HPLC.


1979 ◽  
Vol 62 (3) ◽  
pp. 579-585 ◽  
Author(s):  
Alberto Gimeno

Abstract A general method is described for determining 16 mycotoxins in mixed feeds and other food products used in the manufacture of these feedstuffs. The mycotoxins are extracted and cleaned up by extracting with solvents of different pH. Thin layer chromatography is used to separate the toxins; toxins are then quantitated by the limit detection method. The minimum detectable concentration of mycotoxins in various products is: aflatoxin B1 or G1, 4–5 μg/kg; cchratoxin A or ethyl ester A 140–145 μg/kg; citrinin 600–750 μg/kg; zearalenone, 410–500 μg/kg; sterigmatocystin, 140–145 μg/kg; diacetoxyscirpenol, 2400–2600 μg/kg; T-2 toxin, 800-950 μg/kg; patulin, 750-800 μg/kg; penitrem A 14,000–14,500 μg/kg; penicillic acid 3400-3650 μg/kg.


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.


1983 ◽  
Vol 66 (3) ◽  
pp. 565-569
Author(s):  
Alberto Gimeno

Abstract Arapid method is described for determining zearalenone in corn, sorghum, and wheat. The myco-toxin is extracted with a mixture of acetonitrile and 4% KC1 in HC1. The extract is cleaned up with iso- octane, evaporated, and redissolved in chloroform. Zearalenone is separated by thin layer chromatography; identity is confirmed with various developing solvents and spray reagents. Zearalenone is then quantitated by the limit detection method. The minimum detectable concentration is 140-160 μg/kg when aluminum chloride solution is used as spray reagent, and 85-110 μg/kg when Fast Violet B salt is used as spray reagent


1980 ◽  
Vol 63 (5) ◽  
pp. 1052-1054 ◽  
Author(s):  
Mary W Trucksess ◽  
Leonard Stoloff

Abstract A method for determining aflatoxins in dry ginger root and ginger oleoresin, using 1-dimensional thin layer chromatography (TLC) for the determinative step, has been developed. The key cleanup steps that permit this change from the 2-dimensional TLC previously required are partitioning of the extract with carbon tetrachloride and use of an improved eluting system for the silica gel adsorption column. Recoveries of aflatoxins B1, B2, G1, and G2 added to samples of ground ginger were 82, 101, 106, and 110%, respectively; recoveries of these aflatoxins added to ginger oleoresin were 75, 100, 93, and 125%, respectively. The method is applicable to fish meal and a number of mixed feeds.


1979 ◽  
Vol 62 (3) ◽  
pp. 570-572
Author(s):  
Ramaswamy V Chalam ◽  
Henry M Stahr

Abstract A thin layer chromatographic (TLC) method is described for the determination of citrinin in feeds. Citrinin is extracted from feed with methanol and water, the mixture is made alkaline with 10% sodium carbonate, and the aqueous solution is filtered and extracted with chloroform to remove most of the interfering materials. The aqueous layer is acidified with 2N HCl and extracted with chloroform. The chloroform extract is concentrated and spotted on a thin layer chromatographic (TLC) plate which is developed in chloroform-acetoneethanol- water (60+40+10+1). The citrinin is viewed under ultraviolet light after TLC. Either visual or fiuorodensitometric quantitation is used. Recoveries of citrinin from various feed samples spiked at levels of 2.0–5 μg/g were 75–92%. The proposed method can detect 0.5 μg/g feed, including corn, silage, ready mixed feeds, and feed pellets.


1983 ◽  
Vol 66 (3) ◽  
pp. 582-586
Author(s):  
Gail M Shannon ◽  
Odette L Shotwell ◽  
William F Kwolek

Abstract A method was developed for the determination of aflatoxin B1 in commercially prepared feeds. The method incorporates methylene chloride and citric acid solution extraction, cleanup on a small silica gel column, and thin layer chromatography for quantitation. Commercial turkey starter, catfish chow, medicated pig starter, broiler finisher, rabbit chow, horse feed, rat chow, and dog chow were investigated. The feeds were spiked with naturally contaminated corn at 4 different levels of aflatoxin B1 (16-130 μg/kg). Three assays were run on each of the 32 combinations of feed and levels of aflatoxin. Mean recoveries were 85.9-92.8% at levels of 16.5,32.9,65.8, and 131.6 μg/kg. The relative standard deviation per assay was 18.6%. This method is more rapid and less involved than most previously published methods for mixed feeds.


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