Simultaneous Analysis of Nivalenol and Deoxynivalenol in Cereals by Liquid Chromatography

1987 ◽  
Vol 70 (3) ◽  
pp. 479-483 ◽  
Author(s):  
Denis R Lauren ◽  
Roy Greenhalgh
Keyword(s):  
Liquid Chromatography ◽  
Exchange Resin ◽  
Cation Exchange Resin ◽  
Reverse Phase ◽  
Reverse Phase Liquid Chromatography ◽  
Relative Standard ◽  
Phase Liquid ◽  
Cereal Samples ◽  
Sensitive Method

Abstract A sensitive method is described for determination of nivalenol (NIV) and deoxynivalenol (DON) in cereals by using reverse phase liquid chromatography and UV detection at 222 nm. The sample is extracted with acetonitrile-water (85 + 15) and an aliquot is purified by passage through a combined column of cation exchange resin and alumina-carbon (20 + 1). Analysis at this stage is possible with some samples but the method recommends passing an aliquot through a carbon minicolumn after evaporation and solubilization in methanol. Interference from coextracted compounds at this point is negligible. Recoveries of both NIV and DON from spiked extracts taken through the full method were in the range 83-94%. The relative standard deviation, based on 5 replicate determinations from each of 2 corn samples, was approximately 5% for both NIV and DON. With a 10 fiL injection, the minimum contamination (3 x signal/noise ratio) able to be detected in cereal samples was about 0.015 μ NIV/g and 0.05 μ DON/g. The cleaned up extracts are also suitable for analysis by gas chromatography.

Liquid Chromatographic Determination of Bromadiolone in Rodent Baits

1990 ◽  
Vol 73 (3) ◽  
pp. 429-430
Author(s):  
Benny Koppen
Keyword(s):  
Liquid Chromatography ◽  
Chromatographic Determination ◽  
Reverse Phase ◽  
Reverse Phase Liquid Chromatography ◽  
Relative Standard ◽  
Peak Areas ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract A method Is described for the determination of bromadiolone in rodent bait formulations. Samples are Soxhlet-extracted using methanol as extractant and analyzed by reverse-phase liquid chromatography with UV detection at 280 nm. Chromatography is performed using a ODS-Hypersll (5 fim) column, which enables separation of the 2 diastereolsomers of bromadlolone. The sum of the peak areas of the diastereolsomers Is used for quantitation. The method was tested for precision, linearity, and recovery. Duplicate analyses of 10 formulation samples gave a mean relative standard deviation of 4.1%. Linearity was very good (correlation coefficient 0.9997) In the relevant concentration range. Recovery from spiked samples was 88.9 ±2.3%. The method is applicable to rodent bait formulations with bromadiolone content 0.005% and 0.01%.

Determination of Diacetyl in Butter as 2,3-Diaminonaphthalene Derivative, Using a Fluorometric Procedure or Reverse Phase Liquid Chromatography with Fluorescence Detection

1988 ◽  
Vol 71 (3) ◽  
pp. 462-465
Author(s):  
Pietro Damiani ◽  
Giovanni Burini
Keyword(s):  
Liquid Chromatography ◽  
Fluorescence Detection ◽  
The Other ◽  
Reverse Phase ◽  
Reverse Phase Liquid Chromatography ◽  
Fluorescence Characteristics ◽  
Chromatographic Procedure ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract Two procedures, one fluorometric and the other reverse phase liquid chromatographic, for determination of a derivative of diacetyl are described. Exploratory work on diacetyl standard solutions to establish the best conditions for the derivatization with 2,3-diaminonaphthalene (DAN) to yield 2,3-dimethylbenzo[g]-quinoxaline (DMBQ) is discussed, as well as the fluorescence characteristics of the DMBQ derivative. Diacetyl was determined in 10 commercial butter samples by the proposed procedures and by other known methods (determination of o-phenylenediamine and 3,3-diaminobenzidinederivatives). Recoveries from butter samples spiked with known amounts of diacetyl ranged from 96.9 to 101.8% (with CVs ranging from 0.3 to 2.1%) for the fluorometric procedure and from 96.9 to 102.7% (with CVs ranging from 0.5 to 2.4%) for the chromatographic procedure. These results agree well with those obtained with o-phenylenediamine and 3,3-diaminobenzidine methods on the same butter samples. The proposed methods have the advantages of improved detectability and specificity.

Liquid Chromatographic Determination of Fluridone Aquatic Herbicide and Its Metabolite in Fish and Crayfish

1986 ◽  
Vol 69 (5) ◽  
pp. 856-859 ◽  
Author(s):  
Sheldon D West ◽  
Edgar W Day
Keyword(s):  
Liquid Chromatography ◽  
Detection Limit ◽  
Chromatographic Determination ◽  
Reverse Phase ◽  
Reverse Phase Liquid Chromatography ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Aquatic Herbicide ◽  
Liquid Chromatographic

Abstract A residue method is described for determination of the aquatic herbicide fluridone (1-methy1-3-phenyl-5-[3-(trifluoromethyl)phenyl]-4(1H)- pyridinone) and its metabolite (1-methy1-3-(4-hydroxyphenyl)-5-[3- (trifluoromethyl)phenyl]-4(1H)-pyridinone) in fish and crayfish tissues. Both compounds are extracted from tissues with methanol, and the extracts are subjected to acidic hydrolysis to release conjugated forms of fluridone and the metabolite. Sample extracts are purified by liquidliquid partitioning and Florisil Sep-Pak® column chromatography. Both compounds are separated and measured by reverse phase liquid chromatography with UV detection at 313 nm. In the absence of interfering peaks, the method has a detection limit of approximately 0.04 ppm of either compound. Overall, recoveries averaged 96% for fluridone and 78% for the metabolite for all tissue types combined.

Determination of Seven Artificial Sweeteners in Diet Food Preparations by Reverse-Phase Liquid Chromatography with Absorbance Detection

1988 ◽  
Vol 71 (5) ◽  
pp. 934-937 ◽  
Author(s):  
James F Lawrence ◽  
Claudette F Charbonneau
Keyword(s):  
Liquid Chromatography ◽  
Mobile Phase ◽  
Sorbic Acid ◽  
Artificial Sweeteners ◽  
Reverse Phase ◽  
Phase Gradient ◽  
Reverse Phase Liquid Chromatography ◽  
Absorbance Detection ◽  
Phase Liquid

Abstract The artificial sweeteners aspartame, saccharin, cyclamate, alitame, acesulfam-K, sucralose, and dulcin are determined in diet soft drinks and tabletop sweetener preparations. Samples are diluted, filtered, and analyzed directly by liquid chromatography on a C-18 reversephase column with a mobile phase gradient ranging from 3% acetonitrile in 0.02M KH2P04 (pH 5) to 20% acetonitrile in 0.02M KH2P04 (pH 3.5). Diet puddings and dessert toppings are extracted with ethanol, filtered, and diluted with mobile phase for analysis. The sweeteners, except sucralose and cyclamate, were detected by UV absorbance at either 200 or 210 nm. Sucralose was determined at 200 nm or by refractive index. Cyclamate was determined after post-column ion-pair extraction. The sweeteners stevioside and talin were not detected. Additives such as caffeine, sorbic acid, and benzoic acid did not interfere.

Determination of Thiamphenicol in Bovine Plasma by Liquid Chromatography

1988 ◽  
Vol 71 (6) ◽  
pp. 1156-1157 ◽  
Author(s):  
Lawrence Felice ◽  
El Hassane Abdennebi ◽  
Muhammed Ashraf
Keyword(s):  
Liquid Chromatography ◽  
Chromatographic Method ◽  
Reverse Phase ◽  
Reverse Phase Liquid Chromatography ◽  
Bovine Plasma ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Method ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method is described for the measurement of thiamphenicol in bovine plasma. The plasma (1 mL) is extracted with ethyl acetate. After the solvent is evaporated under a stream of nitrogen, the residue is reconstituted in methanol-water and analyzed by reverse-phase liquid chromatography with UV detection at 224 nm. The intra-day recoveries for bovine plasma spiked with 5 and 50 μg/mL of thiamphenicol were 102 and 101%, respectively, with coefficients of variation of 2.40 and 0.28%, respectively. The interday recoveries for the 5 and 50 μg/mL samples were 103 and 101%, respectively, with coefficients of variation of 3.40 and 0.94%, respectively. The sensitivity of the method allows quantitation to at least the 100 ng/mL level

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