Liquid Chromatographic Determination of the Herbicide Isoxaben and Its Soil Metabolite in Soil and Soil-Turf Samples

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.

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.


1987 ◽  
Vol 70 (4) ◽  
pp. 706-707 ◽  
Author(s):  
Tomoko Nagata ◽  
Masanobu Saeki

Abstract A liquid chromatographic (LC) method is described for determination of olaquindox residues in swine tissues. The drug is extracted from tissues with acetonitrile, and the extract is evaporated to dryness. This residue is cleaned up by alumina column chromatography. LC analysis is carried out on a Nucleosil C18 column, and olaquindox is quantitated by ultraviolet detection at 350 nm. The average recoveries of olaquindox added to tissues at levels of 0.2, 0.1, and 0.05 ppm were 74.0, 68.6, and 66.3%, respectively. The detection limit was 2 ng for olaquindox standard and 0.02 ppm in tissues.


1986 ◽  
Vol 69 (5) ◽  
pp. 856-859 ◽  
Author(s):  
Sheldon D West ◽  
Edgar W Day

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.


1995 ◽  
Vol 78 (3) ◽  
pp. 841-845 ◽  
Author(s):  
Bertil Lindgren ◽  
Tomas Berglöf ◽  
Åsa Ramberg ◽  
Anna Stepdmska ◽  
Malin Åkerblom

Abstract A method is presented for rapid determination of bromide ion in commodities and blood by paired-ion liquid chromatography with electrochemical detection. The method involves extraction of samples with water and filtration. Blood is passed through a Sep-Pak C18 minicolumn. Recoveries are usually close to 100%, with satisfactory precision. The detection limit is 1 mg/kg. The method needs little labor and uses no noxious solvents or reagents.


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).


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.


1979 ◽  
Vol 62 (5) ◽  
pp. 1146-1154
Author(s):  
Masatake Toyoda ◽  
Shunjiro Ogawa ◽  
Yoshio Ito ◽  
Masahiro Iwaida

Abstract A gas-liquid chromatographic (GLC) method was developed for the detection and determination of thiourea in citrus peels. After the peel is extracted with ethyl ether, the ether extract is adsorbed on sodium sulfate together with water. Thiourea is recovered from both the sodium sulfate and the peel residue with ethyl acetateacetone( 2+l). The extracted mixture is cleaned on an alumina column, the eluate is concentrated under vacuum, and thiourea is extracted from the concentrate with sodium carbonate solution. GLC was carried out on the prepared benzoyl derivative of thiourea. The average recoveries of thiourea from lemon peel were 85.3, 93.1, and 97.6% at the fortification levels of 1, 10, and 100 ppm, respectively. The detection limit was as low as 0.08 ppm.


1976 ◽  
Vol 59 (1) ◽  
pp. 1-4 ◽  
Author(s):  
Joseph J DiCecco

Abstract A simple and accurate method has been developed for the quantitative determination of capsaicin in capsicum spices and their oleoresins. Capsaicin is extracted with acetone and separated from interfering substances, using an activated alumina column. The column is first eluted with acetone, and then the capsaicin is eluted with acetone-methanol-water (75+25+2). The capsaicin is quantitated by gas-liquid chromatography, using a Carbowax 20M-Teflon column and piperine as an internal standard. Results can be calculated as per cent capsaicin or Scoville units. Recovery of added capsaicin averaged 101%.


1976 ◽  
Vol 59 (1) ◽  
pp. 162-164
Author(s):  
Samuel K Reeder

Abstract A method is presented for the quantitative analysis of o-phenylphenol residues in citrus oils, encapsulated flavors, and dried meal. The method utilizes high-speed liquid chromatography for the determination after specific sample preparations for each material. These preparations include hexane extraction of acidified basic extracts or steam distillation and extraction. The limit of the analysis is <1 ppm with an analysis time of <45 min.


1980 ◽  
Vol 63 (1) ◽  
pp. 49-55
Author(s):  
Iwao Okuno ◽  
Dennis L Meeker

Abstract An analytical method is described for the determination of Compound 1080 (sodium fluoroacetate) residues in 1–10 g tissue. Sample extracts of tissues are cleaned up with silica gel, and Compound 1080 (as fluoroacetic acid) is separated by a micro-distillation procedure. The fluoroacetic acid in the distillate is derivatized with pentafluorobenzyl bromide to form pentafluorobenzyl fluoroacetate which is measured by electron capture gas-liquid chromatography. Recoveries of sodium fluoroacetate from fortified tissue samples averaged about 25%. Despite the limited recoveries, results were quite reproducible, and levels as low at 2 ppm were determined in fortified 1 g samples, and 0.2 ppm in 10 g samples. The method is relatively simple and has been used routinely in our laboratory for the analysis of various types of samples such as grain, and tissues from birds, rodents, and larger animals.


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