Determination of Citrinin in Corn and Barley on Thin Layer Chromatographic Plates Impregnated with Glycolic Acid

1984 ◽  
Vol 67 (1) ◽  
pp. 194-196
Author(s):  
Alberto Gimeno
Keyword(s):  
Thin Layer ◽  
Glycolic Acid ◽  
Detection Method ◽  
Minimum Detectable Concentration ◽  
Extraction Solvent ◽  
Detectable Concentration ◽  
Tlc Plates ◽  
Limit Detection ◽  
Layer Chromatography

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.

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

1983 ◽  
Vol 66 (3) ◽  
pp. 565-569
Author(s):  
Alberto Gimeno
Keyword(s):  
Thin Layer ◽  
Detection Method ◽  
Chromatographic Determination ◽  
Minimum Detectable Concentration ◽  
Spray Reagent ◽  
Detectable Concentration ◽  
Limit Detection ◽  
Layer Chromatography ◽  
Spray Reagents

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

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
Keyword(s):  
Thin Layer ◽  
Chromatographic Determination ◽  
Minimum Detectable Concentration ◽  
Penicillic Acid ◽  
Detectable Concentration ◽  
Mixed Feeds ◽  
Limit Detection ◽  
Layer Chromatography ◽  
General Method

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.

Notizen: Improved 2,4-Dinitrophenylhydrazine, Thin Layer Chromatography Methods for the Determination of Micro- and Macroamounts of Ascorbic Acid

1974 ◽  
Vol 29 (11-12) ◽  
pp. 777-780 ◽  
Author(s):  
A. Navon ◽  
H. Z. Levinson
Keyword(s):  
Acetic Acid ◽  
Vitamin C ◽  
Thin Layer ◽  
Condensation Reaction ◽  
Dehydroascorbic Acid ◽  
Previous Method ◽  
Aqueous Acetic Acid ◽  
Tlc Plates ◽  
Layer Chromatography

Microamounts of vitamin C could be readily determined in 20 μl-samples using the 2,4-dinitrophenylhydrazine method together with separation by thin layer chromato­graphy. The condensation reaction was carried out for 5 min at 100 °C on a glass fibre disc. Purification of vitamin C hydrazones was accomplished by repeated separation on TLC plates. An aqueous solution of 65% acetic acid was em­ployed to dissolve the vitamin C hydrazones, providing maxi­mal absorbance at 500 nm. The minimum amount detectable by this method is 0.4 μg of dehydroascorbic acid. The macrodetermination of vitamin C was improved by simpli­fying a previous method and employing 65% aqueous acetic acid as a solvent for the hydrazones.

scholarly journals Determination of New Antidepressants in Pharmaceuticals by Thin-Layer Chromatography with Densitometry

2010 ◽  
Vol 93 (3) ◽  
pp. 778-782 ◽  
Author(s):  
Tatána Gondová ◽  
Iveta Petríková
Keyword(s):  
Thin Layer ◽  
Stationary Phase ◽  
Thin Layer Chromatography ◽  
Mobile Phase ◽  
Pharmaceutical Formulations ◽  
Simultaneous Separation ◽  
Tlc Plates ◽  
Precision And Accuracy ◽  
Layer Chromatography

Abstract A new and simple TLC-densitometry method has been developed for the simultaneous separation of the two noradrenergic and specific serotonergic antidepressants mirtazapine and mianserine and validated for their determination in commercially available tablets. The method used TLC plates precoated with silica gel 60F254 as the stationary phase, and the mobile phase consisted of hexaneisopropanol25 ammonia (70 + 25 + 5, v/v/v). Densitometric analysis was carried out in the absorbance mode at 280 nm. The method was validated in accordance with International Conference on Harmonization guidelines in terms of linearity, LOD, LOQ, precision, and accuracy. Calibration curves were linear (R2 > 0.9970) with respect to peak area in the concentration range of 5002500 and 5005000 ng/spot for mirtazapine and mianserine, respectively. The LODs were 20 and 35 ng/spot for mirtazapine and mianserine, respectively. The described method was successfully applied to the determination of mirtazapine and mianserine in their pharmaceutical formulations with recovery ranging from 99.83 to 101.20 of the labeled amount of the compounds. The proposed method can be used in routine QC of these drugs in pharmaceutical formulations.

scholarly journals Simultaneous Identification and Quantitative Determination of Selected Aminoglycoside Antibiotics by Thin-Layer Chromatography and Densitometry

2009 ◽  
Vol 92 (4) ◽  
pp. 1068-1075 ◽  
Author(s):  
Urszula Hubicka ◽  
Jan Krzek ◽  
Hanna Woltyska ◽  
Boóena Stachacz
Keyword(s):  
Thin Layer ◽  
Quantitative Determination ◽  
Mobile Phase ◽  
High Sensitivity ◽  
Good Separation ◽  
Fluorescent Indicator ◽  
Tlc Plates ◽  
Simultaneous Identification ◽  
Layer Chromatography

Abstract A TLCdensitometric method has been developed for simultaneous identification and quantitative determination of amikacin, gentamicin, kanamycin, neomycin, netilmicin, and tobramycin. This separation of antibiotics was achieved on silica gel TLC plates without a fluorescent indicator and with methanol25 ammoniachloroform (3 + 2 + 1, v/v/v) as the mobile phase. The densitometric measurements were made at 500 nm after detection with a 0.2 ninhydrin solution in ethanol. Under these conditions, good separation of the chosen aminoglycosides was obtained. The method is distinguished by high sensitivity, with the LOD from 0.25 g for amikacin to 1.00 g for gentamicin and the LOQ from 0.5 g for amikacin to 1.65 g for gentamicin, and a wide linearity range 0.756.25 g/spot for amikacin and netilmicin and 1.512.50 g/spot for other antibiotics. The precision of the determination was very good; RSD varied in the range 0.30.6.

scholarly journals Dihydrochalcones and Chalcones of Some Flavanone Glycosides: Qualitativeand Quantitative Determinations

1975 ◽  
Vol 30 (11-12) ◽  
pp. 940-942 ◽  
Author(s):  
Harald A. B. Linke ◽  
Douglas E. Eveleigh
Keyword(s):  
Thin Layer ◽  
Quantitative Determination ◽  
Thin Layer Chromatography ◽  
Spectrophotometric Method ◽  
Detection Method ◽  
Alcoholic Solution ◽  
Agar Media ◽  
Layer Chromatography

The chalcones and dihydrochalcones of the flavanone glycosides naringin, neohesperidin and hesperidin were separated and identified by thin-layer chromatography; a similar procedure was utilized to perform preparative TLC for purification of these compounds. A new spectrophotometric method for the quantitative determination of dihydrochalcones in the concentration range from 0.005 to 0.100% in aqueous or alcoholic solution is described as well as a detection method of these compounds in agar media for microbiological studies.

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
Keyword(s):  
Thin Layer ◽  
Aflatoxin B1 ◽  
Detection Method ◽  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Early Spring ◽  
Corn Silage ◽  
Mixed Feeds ◽  
Layer Chromatography

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.

Rapid Thin Layer Chromatographic Determination of Patulin, Citrinin, and Af latoxin in Apples and Pears, and Their Juices and Jams

1983 ◽  
Vol 66 (1) ◽  
pp. 85-91 ◽  
Author(s):  
Alberto Gimeno ◽  
Maria Ligia Martins
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Chemical Reactions ◽  
Aflatoxin B1 ◽  
Detection Method ◽  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Layer Chromatography ◽  
Spray Reagents

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.

Dilution Errors in Aflatoxin Determinations Caused by Compounds Extracted from Peanuts

1983 ◽  
Vol 66 (5) ◽  
pp. 1059-1062
Author(s):  
James W Dickens ◽  
Thomas B Whitaker
Keyword(s):  
Solvent Extraction ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Extraction Solvent ◽  
Water Slurry ◽  
Tlc Plates ◽  
Slurry Method ◽  
Layer Chromatography

Abstract Several methods have been developed to analyze peanuts for aflatoxin by using thin layer chromatography (TLC). These methods depend on solvent extraction of aflatoxin from a sample of the product. Unfortunately, solvent solutions used to extract aflatoxin from peanuts also extract measurable quantities of other compounds such as oils, fats, sugars, and protein. The volume of these extracted compounds causes error in measuring the proportion of the solvent solution analyzed for aflatoxin. Also, because the cleanup procedures for some methods are inadequate, the volume of some of these extracted compounds also causes error in measuring the proportion of the extracted aflatoxin placed on TLC plates. These 2 errors cause underestimation of aflatoxin concentrations by approximately 11,14, and 57c for the CB method, the modified version of the BF method generally used for raw peanuts, and a water slurry method, respectively. The correction specified bytheCB method for fats in the extraction solvent reduces the approximate error for the CB method from 11 to 1%.

Oscillopolarographic Determination of Parathion, Paraoxon, and p-Nitrophenol in Fortified Canned Peaches Following Thin Layer Chromatography

1968 ◽  
Vol 51 (3) ◽  
pp. 690-697
Author(s):  
Fred E Hearth ◽  
Daniel E Ott ◽  
Francis A Gunther
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Internal Standard ◽  
Tlc Plates ◽  
Layer Chromatography

Abstract A procedure combining thin layer chromatography and oscillopolarography has been developed for the separation and microdetermination of parathion, paraoxon, and p-nitrophenol in admixture as residues in fortified canned peach extractives. The use of anthracene as an internal standard for aiding in the location of these compounds on TLC plates is proposed and discussed. This method responds to about 0.5 ppm each for the three compounds with a starting sample of 10 g peaches. While the oscillopolarograph is a very precise instrument, the precision obtainable from the total method is TLC dependent.

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