Determination of Polynuclear Aromatic Hydrocarbons in Seafood by Liquid Chromatography with Fluorescence Detection

1992 ◽  
Vol 75 (5) ◽  
pp. 872-877 ◽  
Author(s):  
Gracia A Perfetti ◽  
Patricia J Nyman ◽  
Sheryl Fisher ◽  
Frank L Joe ◽  
Gregory W Diachenko
Keyword(s):  
Liquid Chromatography ◽  
Fluorescence Detection ◽  
Aromatic Hydrocarbons ◽  
Solid Phase ◽  
Reversed Phase ◽  
Polynuclear Aromatic Hydrocarbons ◽  
Matrix Interferences ◽  
Phase Liquid ◽  
Certified Values

Abstract Modification of a previously published method for determination of polynuclear aromatic hydrocarbons (PAHs) produces very clean seafood extracts in less than half the time. After alkaline digestion of the seafood, PAHs were partitioned into 1,1,2- trichlorotrifluoroethane. The resulting extract was cleaned up by solid-phase extraction on alumina, silica, and C18 adsorbents and then analyzed by gradient reversed-phase liquid chromatography with programmable fluorescence detection. Average recoveries of 12 PAHs [acenaphthene, anthracene, fluoranthene, pyrene, benz(a)anthracene, chrysene, benzo(b)fluoranthene, benzo(k)- fluoranthene, benzo(a)pyrene, dibenz(a,h)anthracene, benzo(ghi)perylene, and indeno(1,2,3-cd)pyrene] from 5 different matrixes (mussels, oysters, clams, crabmeat, and salmon) spiked at low partsper- billion levels ranged from 76 to 94%. Estimated limits of quantitation ranged from 0.01 to 0.6 ppb PAHs in extracts that were free of matrix interferences. Results of analyses of a mussels standard reference material obtained from the National Institute of Standards and Technology were in good agreement with the certified values.

Determination of Avilamycin in Poultry Feeds by Liquid Chromatography

1999 ◽  
Vol 82 (3) ◽  
pp. 579-585 ◽  
Author(s):  
Charles A Scott ◽  
Durand W Yordy ◽  
Mark R Coleman
Keyword(s):  
Liquid Chromatography ◽  
Solid Phase ◽  
Reversed Phase ◽  
Reversed Phase Liquid Chromatography ◽  
Poultry Feeds ◽  
Matrix Interferences ◽  
Relative Standard ◽  
Phase Liquid ◽  
Feed Samples

Abstract Avilamycin was extracted from feed with acetonitrile. Isolation of avilamycin factors from feed matrix interference was accomplishedby normal phase solid-phase extraction with silica as sorbent. Reversed-phase liquid chromatography was subsequently used to separate and quantitate the primary biologically activefactors A and B for determination of chemical potency. This method combines specificity for avilamycins A and B in poultry feeds with simple sample preparation that removes matrix interferences. Recoveries of factor A ranged from 93.29 to 97.26%, with precision (relative standard deviation) ranging from 1.1to 3.4%. Avilamycin factors in feed samples tested ranged from 4.45 to 17.82 μg/g for factor A and from 0.80 to 3.18 μg/g for factor B.

scholarly journals Multiresidue Determination of Fluoroquinolones in Eggs

2000 ◽  
Vol 83 (6) ◽  
pp. 1306-1312 ◽  
Author(s):  
Marilyn J Schneider ◽  
Dan J Donoghue
Keyword(s):  
Liquid Chromatography ◽  
Fluorescence Detection ◽  
Small Volume ◽  
Reversed Phase ◽  
Reversed Phase Liquid Chromatography ◽  
Trace Enrichment ◽  
On Line ◽  
Phase Liquid ◽  
Multiresidue Determination

Abstract A multiresidue method was developed for the determination of fluoroquinolones in eggs. Extraction of eggs with ammoniacal acetonitrile was followed by liquid–liquid defatting, solvent evaporation, and redissolution in a small volume of buffer. The fluoroquinolones were further purified by on-line microdialysis, concentrated on a trace enrichment column, and separated by reversed-phase liquid chromatography with fluorescence detection. Norfloxacin (NOR), ciprofloxacin (CIP), and sarafloxacin (SAR) were extracted from fortified eggs over a range of 2–200 μg/kg, with recoveries of 65.7–78.9%, 65.6–77.1%, and 67.6–110%, respectively. Enrofloxacin (ENRO) was extracted over a range of 1–100 μg/kg, with recoveries of 71.5–86.7%, whereas desethylene ciprofloxacin (DCIP) and danofloxacin (DANO) were extracted over a range of 0.2–20 μg/kg, with recoveries of 68.7–90.7% and 76.0–93.8%, respectively. The limits of quantitation for the 6 fluoroquinolones were as follows: DCIP and DANO, 0.3 μg/kg; ENRO, 1 μg/kg; NOR and CIP, 2 μg/kg; and SAR, 3 μg/kg. Both SAR and ENRO incurred eggs were also successfully analyzed using this method.

scholarly journals Determination of Tylosin in Feeds by Liquid Chromatography with Solid-Phase Extraction

2004 ◽  
Vol 87 (2) ◽  
pp. 341-345 ◽  
Author(s):  
Matthew J Gramse ◽  
Paul E Jacobson ◽  
James C Selkirk
Keyword(s):  
Liquid Chromatography ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Reversed Phase ◽  
Phase Extraction ◽  
Column Temperature ◽  
Solid Phase Extraction Cartridge ◽  
Relative Standard ◽  
Phase Liquid

Abstract A method was developed for the determination of tylosin in feeds. The method involves extraction of tylosin with methanol, concentration under a stream of nitrogen, and cleanup using Phenomenex C18 solid-phase extraction cartridge. Analyte separation and quantitation were achieved by gradient reversed-phase liquid chromatography and UV absorbance at 285 nm with a reference wavelength of 320 nm with column temperature of 45°C. Average spike recoveries for samples prepared at 4 spiking levels (22.7, 181, 907, and 1000 g/ton) were 111.0, 94.9, 96.2, and 98.6%, respectively. The overall method precision at each of the 4 spiking levels was ≤ 7.85% relative standard deviation. The limits of detection and quantitation (g/ton) were 2.16 and 7.20 g/ton, respectively.

Determination of Phenol Sulfone, Phenol Sulfoxide, and Phenol Sulfonic Acid Metabolites of Fenamiphos in Soil by Liquid Chromatography

1995 ◽  
Vol 78 (5) ◽  
pp. 1286-1293
Author(s):  
Gregory C Mattern ◽  
Gilbert D Parker ◽  
Debra L Green ◽  
Gregory L Yeutter
Keyword(s):  
Liquid Chromatography ◽  
Solid Phase Extraction ◽  
Sulfonic Acid ◽  
Solid Phase ◽  
Reversed Phase ◽  
Uv Detection ◽  
Phase Extraction ◽  
Soil Matrix ◽  
Phase Liquid

Abstract An analytical method has been developed to quantitate fenamiphos phenol sulfone, phenol sulfoxide, and phenol sulfonic acid in soil. Both control and analyte-fortified soil samples from Fresno, CA, were extracted with methanol–water (2 + 1) and partitioned with ethyl acetate. Fenamiphos phenol sulfone and phenol sulfoxide were determined by re-versed-phase liquid chromatography (LC) with UV detection at 240 nm after cleanup by silica solid-phase extraction. Fenamiphos phenol sulfonic acid was determined by reversed-phase ion-pairing LC with UV detection at 240 nm after cleanup by amino solid-phase extraction. Recoveries of fenamiphos phenol sulfoxide ranged from 88.2 to 111.0%, with an average of 97.4%. Recoveries of fenamiphos phenol sulfone ranged from 101.6 to 107.0%, with an average of 104.6%. Recoveries of fenamiphos phenol sulfonic acid ranged from 76.0 to 99.9%, with an average of 86.0%. Responses for analysis of analytes in both solvent and soil matrix were linear over the tested range of 10 to 500 ppb. Limits of determination of each analyte in soil were less than 10 ppb.

Analysis of 5-Vinyl-l,3-Oxazolidine-2-Thione by Liquid Chromatography

1992 ◽  
Vol 75 (3) ◽  
pp. 529-536 ◽  
Author(s):  
Alain Quinsac ◽  
Daniel Ribaillier ◽  
Patrick Rollin ◽  
Michel Dreux
Keyword(s):  
Liquid Chromatography ◽  
Solid Phase ◽  
Internal Standard ◽  
Rapeseed Meal ◽  
Reversed Phase ◽  
Mercury Acetate ◽  
Phase Liquid ◽  
Biological Environment ◽  
Liquid Chromatographic

Abstract 5-Vlnyl-1,3-oxazolldlne-2-thlone (5-VOT) Is a goltrlgenlc compound released by enzymatic degradation of progoltrln, the major glucoslnolate occurring In rapeseed meal. A liquid chromatographic (LC) method for determination of 5-VOT in a biological environment Is presented. Complete extraction of 5-VOT has been carried out by complexatlon with phenyl mercury acetate under cyclohexanlc conditions, and then by decomplexation using an aqueous sodium thlosulfate solution. These reactions displace 5-VOT from an aqueous to an organic medium, and then back again to the aqueous condition, thus assuring high selectivity of the extraction. Precise quantitation of 5-VOT Is completed in 10 mln by reversed-phase liquid chromatography using an isocratic elutlon with UV detection and a specially made synthetic Internal standard. Concentration steps by solid-phase chromatography and evaporation can be introduced In the analytic procedure to lower the detection limit of 5-VOT in the sample used from 100 to 0.5 ppb. Using sow milk samples, the method was tested by small measured additions of 5-VOT. The recovery rate of the product was very good (>97%). Different phases used to achieve a sensitive, rapid, and precise method are described.

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