Liquid Chromatographic Determination of Amprolium in Chicken Tissues, Using Post-Column Reaction and Fluorometric Detection

1986 ◽  
Vol 69 (6) ◽  
pp. 941-943
Author(s):  
Tomoko Nagata ◽  
Masanobu Saeki

Abstract A method is presented for determination of amprolium residues in chicken muscles by a liquid chromatographic post-column reaction system. The drug is extracted from muscles with methanol, and the extract is concentrated to 3-4 mL. This aqueous solution is rinsed with n-hexane and cleaned up by alumina column chromatography. The drug is separated from the interferences on a LiChrosorb RP-8 column, reacted with ferricyanide in alkaline solution, and quantitated by fluorometric detection at 367 nm (excitation) and 470 nm (emission). Recoveries of amprolium added to chicken muscles at levels of 0.1 and 0.2 ppm were 74.9 and 80.9%, respectively. The detection limit was 1 ng for amprolium standard and 0.01 ppm in chicken muscles.

1987 ◽  
Vol 70 (6) ◽  
pp. 1031-1032
Author(s):  
Yuuko S Endoh ◽  
Ryozo Yamaoka ◽  
Nobuo Sasaki

Abstract A liquid chromatographic (LC) method is described for the quantitative determination of sulfamoyldapsone (2-sulfamoyl-4,4'-diaminodiphenyl sulfone) in swine muscle, liver, kidney, and fat. Sulfamoyldapsone was extracted from tissues with acetonitrile saturated with n-hexane. The extract was washed with n-hexane saturated with acetonitrile, concentrated, and cleaned up by alumina column chromatography. Sulfamoyldapsone was separated on an ODS column by using acetonitrile-methanol-water (6 + 18 + 76) and was detected at 292 nm. Overall average recovery of sulfamoyldapsone added to tissues at levels of 0.1 and 0.5 /μg/g was 93.3% ± 6.0. Detection limit was 0.02 μg/g in these tissues.


1990 ◽  
Vol 73 (2) ◽  
pp. 287-289 ◽  
Author(s):  
Bonnie S Rutherford

Abstract A method Is described for the determination of residues of isoxaben and its principal soil metabolite In soil and soil-turf samples. Both compounds are extracted from samples by refluxing with methanol-water. An aliquot of the extract Is partitioned Into dichloromethane and purified by alumina column chromatography. Separate fractions containing isoxaben and metabolite are collected and subjected to liquid chromatography at conditions that are optimized for each compound. The detection limit for both compounds is 0.005 ppm. Residue identities are confirmed by chromatography on a different LC system.


1984 ◽  
Vol 67 (2) ◽  
pp. 334-336
Author(s):  
Canutte A Mtema ◽  
Hiroyuki Nakazawa ◽  
Eigo Takabatake

Abstract A simple, rapid, and sensitive liquid chromatographic method is described for the quantitative determination of trace amounts of clopidol (3,5- dichloro-2,6-dimethyl-4-pyridinol) in chicken muscles. Clopidol was extracted from tissues with acetonitrile and the extract was cleaned up on an alumina column and separated on an anion exchange column, using 0.5% acetic acid in methanol as eluant. The solvent in the eluate was evaporated and the residue was dissolved in methanol containing benzamide as internal standard. Clopidol was separated on a Zorbax ODS column (4.6 × 250 mm) by using acetonitrile–0.05M phosphate buffer, pH 7.0 (15 + 85 v/v%), and detected at 270 nm with 0.005 AUFS. Recoveries of clopidol added to chicken tissues at levels of 0.02, 0.05, and 0.1 μg/g were 94.8, 94.8, and 97.0%, respectively. This method is applicable to levels as low as 0.01 ppm clopidol in chicken muscle.


1980 ◽  
Vol 63 (6) ◽  
pp. 1211-1214
Author(s):  
Etsuko Suzuki ◽  
Mihoko Matsuda ◽  
Atsushi Momose ◽  
Masaya Namekata

Abstract A sensitive and specific gas-liquid chromatographic (GLC) method has been developed for determining low levels of clopidol in chicken tissues. Clopidol is extracted from the tissues with methanol, and cleaned up on an alumina column and an anion exchange resin column with 0.1% acetic acid–methanol as eluate. Clopidol is methylated with diazomethane, and then determined by GLC. 2,4-Dinitro-l-chlorobenzene is used as an internal standard. The method is applicable to levels as low as 2 ppb in chicken tissues. Recoveries of 2–20 ppb clopidol added to tissues averaged 87% for muscle, 84% for liver, 80% for kidney, and 76% for fat.


1986 ◽  
Vol 69 (4) ◽  
pp. 644-646
Author(s):  
Tomoko Nagata ◽  
Masanobu Saeki

Abstract A liquid chromatographic (LC) method is described for determination of spiramycin residues in chicken muscles. The drug is extracted from muscles with acetonitrile, the extract is concentrated to 3-4 mL and rinsed with n-hexane followed by ethyl ether, and the drug is extracted with chloroform. LC analysis is carried out on a Zorbax BP-C8 column, and spiramycin is detected spectrophotometrically at 231 nm. Recoveries of spiramycin added to chicken muscles at 0.2 and 0.1 ppm were 93.9 and 89.0%, respectively. The detection limit was 5 ng for spiramycin standard, and 0.05 ppm in chicken muscles.


1973 ◽  
Vol 56 (1) ◽  
pp. 66-67
Author(s):  
Harvey K Hundley

Abstract A GLC method for the determination of sorbitol has been collaboratively studied. Sugar and sugar alcohols are extracted from the bakery products by methanol and the solvent is evaporated. Acetate derivatives are then formed by addition of acetic anhydride in pyridine, and the derivatives are extracted from an aqueous solution with chloroform and analyzed by flame ionization GLC. Collaborative results show a recovery ranging from 90 to 102% sorbitol from bakery products containing 1.5 to 7% sorbitol. The method has been adopted as official first action.


1971 ◽  
Vol 54 (3) ◽  
pp. 551-554 ◽  
Author(s):  
N E Skelly ◽  
R F Cornier

Abstract A semiautomated ion exchange-ultraviolet procedure has been developed for the determination of clopidol in poultry feed at the 40–250 ppm level. A methanol extract of the feed is injected into an alumina precolumn to remove interferences. The clopidol passes through the alumina column and is collected on an ion exchange column. With a specially designed elution apparatus the clopidol is removed by an acetic acid-methanol gradient. The eluate proceeds through a flowcell mounted in an ultraviolet spectrophotometer. Response of the spectrophotometer is monitored by a recorder. Concentration is determined by comparing the peak area in the resulting chromatogram with that of a standard. Accuracy and precision of this method are ±5% relative to the amount present (100±5 ppm).


1985 ◽  
Vol 68 (4) ◽  
pp. 653-657
Author(s):  
Jose E Roybal ◽  
Robert K Munns ◽  
Wilbert Shimoda

Abstract A liquid chromatographic (LC) method for determining residues of carbadox in the 0.01-10 ppm range in swine feed is described. Carbadox is extracted from ground feed with 25% acidified methanol- CHCl3, removed from emulsion-forming coextractables via an alumina column, separated from highly colored pigments by acid-base liquid- , liquid partitioning, and finally isolated from interferences on a second | alumina column. Isocratic reverse phase LC at 305 nm is used for quantitation. The average overall recovery at the 0.1,0.5, and 1.0 ppm J spike levels was 83.0% with a standard deviation of 2.04% and a coefficient of variation of 2.46 %.


2018 ◽  
Vol 22 (1) ◽  
pp. 52-60
Author(s):  
Varga-Visi Éva ◽  
Ildikó Jócsák ◽  
Katalin Lóki ◽  
György Végvári

The proper quantification of serotonin and melatonin in different foods is indispensable to evaluate the significance of their dietary intake on blood and plasma levels in humans. This review summarizes the issues regarding the measurements of these compounds from sour cherry and sweet cherry. Sample preparation and analytical methods are discussed, mainly focusing on the liquid chromatographic determination of these compounds, with special respect to their parallel determination in one run. Keywords: indoleamine derivatives, LC-MS, electrochemical detection, fluorometric detection


1980 ◽  
Vol 63 (1) ◽  
pp. 27-32
Author(s):  
Lester L Lamparski ◽  
Marsha L Langhorst ◽  
Terry J Nestrick ◽  
Sergio Cutié

Abstract The determination of higher chlorinated benzenes and chlorinated phenols at parts per billion or parts per million levels in biological samples is described. The method includes sulfuric acid digestion, silica gel column chromatography, methylation, alumina column chromatography, and detection by electron capture gas chromatography. Recoveries are reported (or fish flesh, rabbit tissues, and duck tissues with detection limits of 10-15 ppb (ng/g tissue).


Sign in / Sign up

Export Citation Format

Share Document