Mycotoxins in Animal Feedstuffs: Sensitive Thin Layer Chromatographic Detection of Aflatoxin, Ochratoxin A, Sterigmatocystin, Zearalenone, and T-2 Toxin

1979 ◽  
Vol 62 (6) ◽  
pp. 1265-1267
Author(s):  
Deryck S P Patterson ◽  
Basil A Roberts

Abstract Improvements have been made to a previously described multi-mycotoxin method that involved a membrane cleanup step. Using 2-dimensional thin layer chromatography and appropriate solvent systems, aflatoxin B1 can be detected in mixed feedstuffs and various ingredients at levels ranging from 0.1 to 0.3 μg/kg. Corresponding detection limits for ochratoxin A and sterigmatocystin are 5 to 20 μg/kg and for T-2 toxin and zearalenone 20 to 200 μg/kg.

2014 ◽  
Vol 21 (1) ◽  
pp. 11-15
Author(s):  
Daiva Kazlauskienė ◽  
Guoda Kiliuvienė ◽  
Palma Nenortienė ◽  
Giedrė Kasparavičienė ◽  
Ieva Matukaitytė

By conducting the toxicological analysis it is meaningful to determine the analytical system that could identify simultaneously several medicinal preparations quickly and precisely. The purpose of this work was to create and validate the method of thin-layer chromatography that would be suitable to separate the components of antidepressant mixture (amitriptyline hydrochloride, paroxetine hydrochloride, sertraline hydrochloride, fluvoxamine maleate and buspirone hydrochloride) and to identify them. The system was validated with regard to the sensitivity, repetition of data, resistance and particularity. The solvent systems with potential of high separation of components in their mixture were created: acetonitrile, methanol, ammonia solution 25 percent (85:10:5); acetonitrile, methanol, ammonia solution 25 percent (75:20:5); dichlormethane, 1,4-dioxane, ammonia solution 25 percent (50:45:5); dichlormethane, 1,4-dioxane, ammonia solution 25 percent (42:55:3); trichlormethane, 1,4-dioxane, ammonia solution 25 percent (25:70:5); trichlormethane, 1,4-dioxane, ammonia solution 25 percent (60:36:4). One of the most suitable solvent systems for separation of the analyzed mixture (sertraline, amitriptyline, paroxetine, buspirone, fluvoxamine) was determined – acetonitrile, methanol, ammonia solution 25 percent (85:10:5). When this solvent system was used, the average Rf values of the analyzed compounds differed the most. Validation was conducted – the relative standard deviation (RSD, percent) of the average Rf value of the analyzed compounds varied from 0,6 to 1,8 percent and did not exceed the permissible error of 5 percent. The sensitivity of methodology was determined by assessing the intensity of the mixture’s spots on the chromatographic plate. The detection limit of buspirone was 0,0012 µg; sertraline – 0,0008 µg; amitriptyline – 0,0004 µg; fluvoxamine – 0,0004 µg; paroxetine – 0,0008 µg. The resistance of results to the changed conditions – it was determined that when the amounts of the solvents acetonitrile and methanol were increased or decreased to two milliliters, the average Rf values of the analyzed compounds did not change statistically significantly


1968 ◽  
Vol 51 (6) ◽  
pp. 1247-1260
Author(s):  
M B Abou-Donia ◽  
D B Menzel

Abstract Infrared spectroscopy, in combination with TLC and GLC, offers an effective technique for isolation, separation, and identification of DDT-type compounds. Rf values for DDT and 13 other compounds, most of which have been reported as DDT breakdown products, have been determined in 27 solvent systems, using TLC techniques. Three columns, in combination with the electron capture detector, have been experimentally studied to analyze the 13 DDT-like compounds. The positions and intensities of the infrared bands of the 14 compounds have been measured in KBr. The variations of these measurements have been discussed in relation to the structural changes of DDT-type compounds.


1977 ◽  
Vol 60 (6) ◽  
pp. 1369-1371 ◽  
Author(s):  
B G Egon Josefsson ◽  
Tord E Möller

Abstract A screening method has been developed for the detection of aflatoxins, ochratoxin A, patulin, sterigmatocystin, and zearalenone in cereals. After extraction, the sample is cleaned up by gel filtration. The mycotoxins are separated by thin layer chromatography. The limits of detection are about 5 μg aflatoxins, 10 ochratoxin A, 50 μg patulin, 10 μg sterigmatocystin, and 35 μg zearalenone/kg.


1983 ◽  
Vol 66 (4) ◽  
pp. 1009-1012
Author(s):  
Radhakrishnan Sundararajan ◽  
Ram Parkash Chawla

Abstract Thin layer chromatography employing silver nitrate-impregnated alumina G plates has been extended for the routine detection and confirmation of the identity of halogenated synthetic pyrethroid insecticides. Of the solvent systems tried, maximum resolution was achieved by using n-hexane-benzene (45+ 55) and n-hexane-chloroform (60 + 40), which gave distinct separations of the cis- and trans-isomers of permethrin and cypermethrin from fenvalerate and decamethrin. Possible interference of HCH isomers and DDT and its analogs can also be checked by a concurrent run of the sample mixture in these 2 systems. A minimum of 50 ng each of cis- and trans-permethrin and cypermethrin isomers and fenvalerate and decamethrin can be positively detected. Using this technique, the minimum detectable limit of permethrin was 0.1 ppm in the cleaned up extracts of tomato plant and fruit and soil samples.


1965 ◽  
Vol 48 (4) ◽  
pp. 838-843 ◽  
Author(s):  
Rachel S Silk

Abstract Thin-layer chromatographic procedures have been developed by which most of the colors present in current commercial lipsticks can be separated. Most lipstick colors are separated on one plate with two solvent systems, but the presence of D&C Red No. 7 requires a slightly altered procedure. A plate with a buffered zone is added and an additional development step is used. The color recovery was determined by the analyses of 16 lipsticks from four manufacturers.


1979 ◽  
Vol 62 (4) ◽  
pp. 917-920 ◽  
Author(s):  
Irene Kushnir

Abstract A highly sensitive procedure has been developed to detect the undeclared addition of high fructose corn sirup (HFCS) to honey. Carbohydrates must be separated first to achieve the requisite degree of sensitivity: charcoal-Celite chromatography was used to isolate a fraction containing oligo- and polysaccharides. The fraction was then concentrated and examined by thin layer chromatography on silica gel. Pure honeys yielded only 1 or 2 blue-grey or bluebrown spots at Rf values >0.35; a series of spots or blue streaks extending from the origin characterized adulterated samples. The method detects HFCS and conventional honey adulterants at levels as low as 10% or less of the total mixture. In addition, the procedure detects the presence in honey of all starch-derived sugar sirups tested thus far, regardless of the plant source.


1975 ◽  
Vol 58 (1) ◽  
pp. 156-158
Author(s):  
Benedicte Hald ◽  
Palle Krogh

Abstract A simplified procedure has been developed to detect ochratoxin A in cereals which can be used in the field where equipment for thin layer chromatography is not available. The procedure includes extraction of the acidified sample with chloroform, purification over sodium bicarbonate, and minicolumn chromatography. Under longwave ultraviolet light ochratoxin A appears as a blue-green fluorescent band at the lower end of the column. Contamination levels as low as 12 ppb can be detected by this method.


1975 ◽  
Vol 21 (1) ◽  
pp. 76-80 ◽  
Author(s):  
H Kenneth Sleeman ◽  
James A Cella ◽  
Johnnie L Harvey ◽  
Douglas J Beach

Abstract A procedure for detecting methaqualone and identifying methaqualone metabolites in urine by thin-layer chromatography is described and evaluated. Urine is hydrolyzed with HCl or NalO4, adjusted to pH 9.5, and extracted with chloroform. The chloroform extract is evaporated, reconstituted in methanol, applied to fluorescent silica-gel plates, and developed with ethyl acetate:methanol:ammonium hydroxide (28%) (85:10:5 by vol). Methaqualone use is detected by a pattern of four metabolites, which can be seen under ultraviolet light or are made visible by acidified iodoplatinate reagent. Synthetic methaqualone metabolites are used for identification and to compensate for procedural variables. More than 250 positive urine specimens were correctly identified by this method. Hydrolyzed natural and synthetic metabolites were identical by several criteria.


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