Thin Layer Chromatographic Determination of Deoxynivalenol in Processed Grain Products

1986 ◽  
Vol 69 (1) ◽  
pp. 35-36
Author(s):  
Mary W Trucksess ◽  
Michael T Flood ◽  
Samuel W Page
Keyword(s):  
Thin Layer ◽  
Chromatographic Determination ◽  
Reverse Phase ◽  
Breakfast Cereals ◽  
Limit Of Determination ◽  
Anhydrous Ethyl Ether ◽  
Tlc Plates ◽  
Grain Products ◽  
Phase Column

Abstract The thin layer chromatographic (TLC) method of Trucksess et al. (J. Assoc. Off. Anal. Chem. (1984) 67, 40-43) was modified for the determination of deoxynivalenol (DON) in high-sugar breakfast cereals, corn syrup, and beer. Celite was added to the substrate before extraction with acetonitrile-water (84 + 16). After filtration through an aluminacharcoal-Celite (0.5 + 0.7 + 0.3) column, the filtrate was evaporated to dryness and redissolved in water, which was passed through an octylsilyl reverse phase column. DON was eluted with anhydrous ethyl ether. The residue remaining after the eluate was evaporated to dryness was dissolved in CHCl3-acetonitrile (4 + 1) and chromatographed on AlCVimpregnated silica gel TLC plates. The blue fluorescent DON spot was quantitated fluorodensitometrically after the TLC plate was heated at 120°C for 7 min. Recoveries of DON added to breakfast cereals at 100, 200, and 400 ng/g levels and to syrup and beer at 50, 100, and 200 ng/g levels averaged 86%. The limit of determination in these products was about 50 ng/g.

Thin Layer Chromatographic Detection and Liquid Chromatographic Determination of Stevioside and Rebaudioside A in Beverages and Foods Following Reverse Phase Column Chromatography

1986 ◽  
Vol 69 (5) ◽  
pp. 799-802
Author(s):  
Kenji Fujinuma ◽  
Kazuo Saito ◽  
Mitsuo Nakazato ◽  
Yoko Kikuchi ◽  
Akihiro Ibe ◽  
...  
Keyword(s):  
Thin Layer ◽  
Chromatographic Determination ◽  
Rebaudioside A ◽  
Reverse Phase ◽  
Reverse Phase Column ◽  
Chromatographic Procedure ◽  
Acid Reagent ◽  
Liquid Chromatographic ◽  
Phase Column

Abstract A method for the detection and determination of stevioside and rebaudioside A in beverages and foods by thin layer chromatography (TLC) and liquid chromatography (LC) is presented. Stevioside and rebaudioside A are extracted with water from a sample and purified by a reverse phase column chromatographic procedure using a silica gel 60 silanized column. The eluate from the column is concentrated to dryness, and the resulting residue is dissolved in 80% ethanol. For the detection, TLC is used, and spots of stevioside and rebaudioside A are visualized with anisaldehyde sulfuric acid reagent. Stevioside and rebaudioside A detected in samples are determined by LC with a Finepak SIL NH2 column and a mobile phase of acetonitrile-water (200 + 45) containing tetrabutylammonium phosphate, which is added to achieve the separation from some interfering compounds. Recoveries from samples spiked at 10 and 100 ppm ranged from 97.8 to 100.3% (stevioside) and 96.3 to 99.7% (rebaudioside A).

Thin Layer Chromatographic Determination of Citrinin

1979 ◽  
Vol 62 (1) ◽  
pp. 201-202 ◽  
Author(s):  
Robert D Stubblefield
Keyword(s):  
Acetic Acid ◽  
Thin Layer ◽  
Linear Relationship ◽  
Silica Gel ◽  
Coefficient Of Variation ◽  
Ethylenediaminetetraacetic Acid ◽  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Tlc Plates

Abstract Clearly defined zones of citrinin can be obtained on thin layer chromatographic (TLC) plates and measured by fluorodensitometry. Silica gel plates were prepared as a slurry with aqueous 0.05M Na2EDTA (ethylenediaminetetraacetic acid), spread at 0.5 mm wet thickness, and activated at 105°C for 1 hr. Plates were developed in acetic acid-benzene (5+95). The limit of detection was 10 ng citrinin/zone. Densitometric analysis (365 nm excitation, 505 nm emission) revealed that a linear relationship exists for levels of 10 ng to at least 100 ng/zone wtih a coefficient of variation of ±5%.

Liquid Chromatographic Determination of Sodium Fluoroacetate (Compound 1080) in Meat Baits and Formulations

1984 ◽  
Vol 67 (6) ◽  
pp. 1058-1061
Author(s):  
Harvey L Kramer
Keyword(s):  
Crown Ether ◽  
Chromatographic Determination ◽  
Reverse Phase ◽  
Ultraviolet Absorbance ◽  
Reverse Phase Column ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Phase Column

Abstract A liquid chromatographic (LC) method is described for the determination of sodium fluoroacetate in meat baits and formulations. Baits were extracted with water, ultrafiltered, partitioned into butanone, back-partitioned into dilute base, and diluted with acetonitrile. Aqueous formulations of 1080 were diluted with acetonitrile. The solutions were esterified with p-bromophenacyl bromide, using crown ether catalysis, and chromatographed on a 10 μm reverse phase column. Ultraviolet absorbance was monitored at 260 nm. Samples spiked to contain 1 mg and 10 mg 1080/100 g meat gave recoveries of 84.0-103.4%.

Liquid Chromatographic Determination of Olaquindox in Medicated Feeds and in Contents of Porcine Gastrointestinal Tract

1988 ◽  
Vol 71 (6) ◽  
pp. 1106-1109
Author(s):  
Theo J Spierenburg ◽  
Henk Van Lenthe ◽  
Gertjan De Graaf ◽  
Lowie P Jager
Keyword(s):  
Gastrointestinal Tract ◽  
Chromatographic Determination ◽  
Detector Response ◽  
Minimum Detectable Concentration ◽  
Reverse Phase ◽  
Reverse Phase Column ◽  
Liquid Chromatographic ◽  
Medicated Feeds ◽  
Phase Column

Abstract A liquid chromatographic method for the determination of olaquindox in both medicated feeds and porcine gastrointestinal tract is described. Samples are extracted with water and cleaned on a disposable reverse-phase column. The eluate is chromatographed on a reverse-phase column under isocratic conditions. Olaquindox is detected by UV absorption at 260 nm. The minimum amount detected by this method was 0.075 ng. The corresponding minimum detectable concentration in a 1 g sample was 0.3 mg/kg. The detector response was linear within the interval of 0-500 ng. Mean recovery of olaquindox in spiked gastrointestinal samples was 89 ± 5% (mean ± standard deviation, n = 43). Concentration profiles of olaquindox in the gastrointestinal tract of pigs fed medicated feed were used to evaluate the preventive potency against Treponema hyodysenteriae. The presence of some N-O reduced metabolites of olaquindox in the gastrointestinal tract was assessed

Liquid Chromatographic Determination of Strychnine in Stomach Contents

1985 ◽  
Vol 68 (6) ◽  
pp. 1131-1133
Author(s):  
Jacobus J L Hoogenboom ◽  
Colin G Rammell
Keyword(s):  
Phosphoric Acid ◽  
Stomach Contents ◽  
Chromatographic Determination ◽  
Chloroform Extract ◽  
Acid Extract ◽  
Reverse Phase ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Phase Column

Abstract A chloroform extract of stomach contents at basic pH is concentrated and then extracted with 0.1M phosphoric acid. The acid extract is chromatographed on a 10 cm reverse phase column, using 0.005M phosphate buffer (pH 3.0)-acetonitrile-tetrahydrofuran (750 + 135 + 115) containing 0.01M octanesulfonic acid at a flow rate of 1.0 raL/ min for elution. Strychnine eluted in 7.3 min. Recoveries from spiked stomach contents averaged 92%. The method can be used without modification for other alkaloids.

Liquid Chromatographic Determination of Clobetasone-17-Butyrate in Ointments

1990 ◽  
Vol 73 (6) ◽  
pp. 893-895 ◽  
Author(s):  
Ajay G Patel ◽  
Ramanbhai B Patel ◽  
Mukeshbhai R Patel
Keyword(s):  
Sodium Salt ◽  
Mobile Phase ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Reverse Phase ◽  
Reverse Phase Column ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Phase Column

Abstract A liquid chromatographic (LC) method has been developed for determination of clobetasone-17-butyrate In ointment using clobetasone propionate as an internal standard. Separation was carried out on a C18 reverse-phase column using water-methanol as a mobile phase. Methylparaben and propylparaben (both sodium salt) used as preservatives did not Interfere with separation. Compounds are detected photometrically at 235 nm. Mean assay results for 0.05% commercial ointments were 100.36% (n = 5). Mean recovery of clobetasone-17-butyrate added to commercial ointment was 99.89%.

High-performance thin-layer chromatographic determination of rosiglitazone in its dosage form

2002 ◽  
Vol 15 (3) ◽  
pp. 192-195 ◽  
Author(s):  
Ramesh Sane ◽  
Mary Francis ◽  
Atul Moghe ◽  
Sachin Khedkar ◽  
Ajit Anerao
Keyword(s):  
Thin Layer ◽  
High Performance ◽  
Dosage Form ◽  
Chromatographic Determination

Liquid Chromatographic Determination of Zoalene in Medicated Feeds

1984 ◽  
Vol 67 (5) ◽  
pp. 861-862 ◽  
Author(s):  
John Morawski ◽  
Glenn Kyle
Keyword(s):  
Colorimetric Method ◽  
Chromatographic Determination ◽  
Activated Alumina ◽  
Reverse Phase ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Aoac Official ◽  
Liquid Chromatographic ◽  
Medicated Feeds

Abstract A rapid, reliable separation and quantitation of zoalene (3,5-dinitroo-toluamide) from feeds is accomplished by using reverse phase liquid chromatography (LC) and ultraviolet detection. An extraction technique which is similar to the present AOAC official colorimetric method is used before chromatographic analysis. This extraction is followed by an activated alumina cleanup and LC to separate zoalene from feed matrix. The methodology was applied to a variety of spiked feed matrices, and yielded good recoveries. Liquid chromatographic results were shown to correlate with colorimetric determinations.

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