Thin Layer Chromatographic Determination of Aflatoxins, Ochratoxins, Sterigmatocystin, Zearalenone, Citrinin, T-2 Toxin, Diacetoxyscirpenol, Penicillic Acid, Patulin, and Penitrem A

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 (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.


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.


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.


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 (3) ◽  
pp. 743-748 ◽  
Author(s):  
Árpád Ambrus ◽  
Éva Hargitai ◽  
Gabriella Károly ◽  
András Fülöp Ambrus ◽  
János Lantos Ambrus

Abstract o-Tolidine plus KI, p-nitrobenzene-diazoniumfluoroborate, bioassay with fungi and enzyme sources, AgNO3 plus UV radiation, and p-dimethyl-aminobenzaldehyde modes of detection have been selected for TLC screening of pesticide residues in extracts of samples of unknown origin. Single solvents were used for the elution. Coefficients of variation of Rf values were studied as a function of Rf and eluants. Indicator compounds were used for controlling the proper conditions of detection. The detectability of 188 pesticide compounds was tested, and the minimum detectable amounts were determined.


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.


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.


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.


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