Thin Layer Chromatographic Determination of Ctrinin

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.

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.


1978 ◽  
Vol 61 (1) ◽  
pp. 92-95
Author(s):  
Ugo R Cieri

Abstract A method is presented for determining the nitrofurans furazolidone and nitrofurazone in animal feeds. The sample is extracted with acetone, and aliquots of the concentrated extract are spotted on thin layer chromatographic fluorescent plates. After development in CHCl3-methanol (90+10), the bands containing the nitrofurans are detected under shortwave ultraviolet light, scraped from the plate, and extracted with ethanol. The centrifuged extracts are scanned from 500 to 300 nm on a recording spectrophotometer with a tungsten lamp, and the absorbance maxima near 360 nm are used for quantitation. To compensate for extraction and chromatographic losses and for other interferences, the nitrofuran not present in the sample is added as an internal standard. The method is generally not applicable at a level below 0.005% since detection of the bands becomes difficult.


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.


1986 ◽  
Vol 69 (4) ◽  
pp. 699-703 ◽  
Author(s):  
Thomas R Romer

Abstract Small charcoal/alumina cleanup columns have been effectively used to remove interfering materials from grain, feed, and food extracts prior to chromatographic determination of trichothecene mycotoxins. A thin layer chromatographic method has been developed that can simultaneously detect part per billion concentrations of deoxynivalenol, fusarenon X, nivalenol, T-2 toxin, HT-2 toxin, neosolaniol, and diacetoxyscirpenol in food and feed samples. Recoveries of 90-99% can be obtained. The use of charcoal/alumina cleanup columns in conjunction with liquid chromatography and gas chromatography of trichothecenes is also discussed.


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.


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.


1967 ◽  
Vol 50 (2) ◽  
pp. 264-268
Author(s):  
H Borfitz ◽  
J Para ◽  
J V Stickles ◽  
G B Ginther ◽  
B C Southworth

Abstract A procedure has been developed for determining buquinolate (ethyl 4-hydroxy- 6,7- diisobutoxy - 3 - quinolinecarboxylate) in finished chicken feeds. In the procedure, a chloroform extract of the feed is concentrated to a small known volume, separated from background substances by thin layer chromatography on silica gel (two solvent systems), eluted from the plate, and compared fluorometrically with reference standard buquinolate. No background interference was found from 157 feed samples investigated or from 11 common feed additives. Recovery experiments on 31 samples at levels ranging from 0.0044 to 0.0143% buquinolate averaged 99.7% with a standard deviation of 3.3. The method is equally applicable to both fresh and aged feeds. This method was studied collaboratively, results were good, and the method is recommended for adoption as official, first action


1984 ◽  
Vol 67 (1) ◽  
pp. 40-43 ◽  
Author(s):  
Mary W Trucksess ◽  
Stanley Nesheim ◽  
Robert M Eppley

Abstract A thin layer chromatographic (TLC) method for determining deoxynivalenol (DON) in corn and wheat was developed. DON is extracted from the grain with acetonitrile–water (84 + 16) and filtered through a column of mixed alumina–charcoal–Celite (0.5 g + 0.7 g + 0.3 g). The solvent is evaporated on a steam bath. Ethyl acetate is added to the residue and heated to dissolve DON. After cooling, the residue is transferred to a vial with additional ethyl acetate and is dissolved in CHCl3–acetonitrile (4 + 1) for TLC on an AlCl3-impregnated silica gel plate with CHCI3–acetone–isopropanol (8 + 1 + 1). The plate is heated in a 120°C oven for 7 min; a blue fluorescent spot is produced under longwave ultraviolet light. DON is quantitated visually and/or fluorodensitometrically by comparison with reference standards. The minimum detectable amount of DON is ca 20 ng/spot. The limit of DON determination is ca 40 ng/g for wheat and 100 ng/g for corn. Recoveries of DON added to wheat and corn at 100, 500, and 1000 ng/ g levels were 85, 93, and 88% and 77, 80, and 80%, respectively.


Sign in / Sign up

Export Citation Format

Share Document