Rapid Thin Layer Chromatographic Determination of Zearalenone in Corn, Sorghum, and Wheat

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

1984 ◽  
Vol 67 (1) ◽  
pp. 194-196
Author(s):  
Alberto Gimeno

Abstract A method is described for the determination of citrinin in corn and barley. The mycotoxin is extracted with a mixture of acetonitrile-10% glycolic acid in water, defatted with isooctane, and transferred to chloroform according to published methods. The mycotoxin is separated by thin layer chromatography (TLC) on plates previously impregnated with 10% glycolic acid solution in ethanol; identity is confirmed by chemical tests. Citrinin is then quantitated by the limit detection method. Recoveries of citrinin from corn and barley samples spiked at levels of 50, 80, 150, 300, 500, and 1000 μg/kg were in the range 91-98%. The minimum detectable concentration is 15-20 μg/ kg. Recoveries obtained with and without glycolic acid in the extraction solvent were compared. Sensitivities on TLC plates (limits of detection, μg/spot) impregnated with glycolic acid were compared with those on plates impregnated with oxalic acid.


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.


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.


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.


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.


1979 ◽  
Vol 62 (3) ◽  
pp. 573-578 ◽  
Author(s):  
Yuiko Takeda ◽  
Etsuko Isohata ◽  
Ryuji Amano ◽  
Mitsuru Uchiyama

Abstract A simple, systematic analytical method for multiple mycotoxins was developed for detecting 14 mycotoxins: aflatoxins Bl, B2, G1, and G2, sterigmatocystin, T-2 toxin, diacetoxyscirpenol, neosolaniol, fusarenon X, zearalenone, ochratoxin A, citrinin, luteoskyrin, and rugulosin. These mycotoxins were extracted with 20% H2SO4-4% KCl-acetonitrile (2+20+178), defatted with isooctane, and transferred to chloroform. The chloroform extract was cleaned up by silica gel column chromatography; the first 10 toxins were eluted with chloroform-methanol (97+3) and the remaining 4 toxins with benzene-acetone-acetic acid (75+20+5). Each fraction was analyzed by thin layer chromatography for the final determination. The method has been applied to polished rice, rough rice, corn, wheat, and peanuts as an analytical screening procedure. The detection limits in these commodities ranged from 10.0 to 800.0 μg/kg, depending on the mycotoxin, but all limits were superior to those obtained for the individual mycotoxins by using other methods.


1987 ◽  
Vol 70 (6) ◽  
pp. 1008-1011 ◽  
Author(s):  
Toshihiro Nagayama ◽  
Toshio Maki ◽  
Kimiko Kan ◽  
Mami Iida ◽  
Taichiro Nishima

Abstract A simple, rapid, highly sensitive liquid chromatographic method is described for the quantitative determination of paraquat and diquat residues in agricultural products. Paraquat and diquat are extracted with hot dilute hydrochloric acid and are cleaned up on an Amberlite CG-50 column, followed by reverse-phase liquid chromatography on an NH, column, with ultraviolet detection at 257 nm (paraquat) and 310 nm (diquat). The minimum detectable concentration of both paraquat and diquat was 0.5 ng per injection, which corresponds to a lower detection limit of approximately 0.02 fjg/g in the original samples. Recoveries of paraquat and diquat added to various samples were greater than 79%, and averaged 91 and 90%, respectively, at the 0.1 and 1.0 μg/g spiking levels.


1998 ◽  
Vol 81 (4) ◽  
pp. 844-847 ◽  
Author(s):  
Wynne W Landgraf ◽  
P Frank Ross

Abstract Monensin is extracted from feed with methanol and purified by solvent-partitioning solid-phase extraction. After solvent reduction, monensin is separated by thin-layer chromatography on silica gel and visualized by color development with vanillin. No false-positive results were obtained in validation studies by submitting or peer laboratories when blank samples were analyzed. Three of 20 samples spiked with 5 ppm monensin were reported as containing no monensin. All samples spiked with 10 ppm monensin were reported positive for monensin.


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.


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


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