Separation and quantitation of 3,3′,4,4′-tetrachlorobiphenyl and 3,3′,4,4′,5,5′-hexachlorobiphenyl in aroclors using florisil column chromatography and gas-liquid chromatography

1979 ◽  
Vol 23 (1) ◽  
pp. 51-56 ◽  
Author(s):  
LaVerne R. Kamops ◽  
William J. Trotter ◽  
Susan J. Young ◽  
Audrey C. Smith ◽  
John A. G. Roach ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Column Chromatography ◽  
Gas Liquid Chromatography ◽  
Florisil Column ◽  
Florisil Column Chromatography

Multiresidue Method for Determining Substituted Urea Herbicides in Foods by Liquid Chromatography

1987 ◽  
Vol 70 (4) ◽  
pp. 740-745
Author(s):  
Ronald G. Luchtefeld
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Column Chromatography ◽  
Food Products ◽  
Chemical Derivatization ◽  
Florisil Column ◽  
Average Recovery ◽  
Multiresidue Method ◽  
Florisil Column Chromatography ◽  
Substituted Urea

Abstract A method is described for determining substituted urea herbicides in foods. The residues are extracted from the product with methanol, and the food coextractives are removed by using solvent partitioning and Florisil column chromatography. The extract is analyzed using liquid chromatography with postcolumn photodegradation, chemical derivatization with orthophthalaldehyde, and spectrofluorometry. Recoveries were determined by spiking 8 different food products with 6 phenylureas—chlorbromuron, chloroxuron, diuron, fluometuron, linuron, and metobromuron—at 0.05 and 0.5 ppm. Three determinations were made at each level for each product. Average recovery at 0.05 ppm was 95% (with a standard deviation of 7.9%), and at 0.5 ppm, 98% (with a standard deviation of 6.9%).

Multiresidue Method for Determining Substituted Urea Herbicides in Foods by Liquid Chromatography

1987 ◽  
Vol 70 (4) ◽  
pp. 740-745
Author(s):  
Ronald G Luchtefeld
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Column Chromatography ◽  
Food Products ◽  
Chemical Derivatization ◽  
Florisil Column ◽  
Average Recovery ◽  
Multiresidue Method ◽  
Florisil Column Chromatography ◽  
Substituted Urea

Abstract A method is described for determining substituted urea herbicides in foods. The residues are extracted from the product with methanol, and the food coextractives are removed by using solvent partitioning and Florisil column chromatography. The extract is analyzed using liquid chromatography with postcolumn photodegradation, chemical derivatization with orthophthalaldehyde, and spectrofluorometry. Recoveries were determined by spiking 8 different food products with 6 phenylureas—chlorbromuron, chloroxuron, diuron, fluometuron, linuron, and metobromuron—at 0.05 and 0.5 ppm. Three determinations were made at each level for each product. Average recovery at 0.05 ppm was 95% (with a standard deviation of 7.9%), and at 0.5 ppm, 98% (with a standard deviation of 6.9%).

Collaborative Study of Three Methods for the Determination of Fluoride in Vegetation

1978 ◽  
Vol 61 (1) ◽  
pp. 150-153
Author(s):  
Jay S Jacobson ◽  
Laurence I Heller
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Polychlorinated Biphenyls ◽  
Collaborative Study ◽  
Bald Eagle ◽  
Gas Liquid Chromatography ◽  
Tissue Samples ◽  
Florisil Column ◽  
Average Recovery

Abstract A procedure is described for determining Kepone (decachlorooctahydro-l,3,4-metheno-2ffcyclobuta[ cd]pentalene-2-one) residues in avian egg, liver, and tissue. Samples were extracted with benzene-isopropanol, and the extract was cleaned up with fuming H2S04-concentrated H2SO4. Kepone was separated from organochlorine pesticides and polychlorinated biphenyls on a Florisil column and analyzed by electron capture gas-liquid chromatography (GLC). The average recovery from spiked tissues was 86%. The analyses performed on 14 bald eagle carcasses and livers, 3 bald eagle eggs, and 14 osprey eggs show measurable levels which indicate that Kepone accumulates in the tissues of fish-eating birds. Residues were confirmed by GLC-mass spectrometry

Determination of Chlorinated Pesticide Residues in Foods. III. Simultaneous Analysis of Chlorinated Pesticide and Phthalate Ester Residues by Using AgNO3-Coated Florisil Column Chromatography for Cleanup of Various Samples

1979 ◽  
Vol 62 (3) ◽  
pp. 689-694
Author(s):  
Takashi Suzuki ◽  
Kiyoshi Ishikawa ◽  
Nobutoshi Sato ◽  
Kei-Ichi Sakai
Keyword(s):  
Column Chromatography ◽  
Phthalate Esters ◽  
Ethanol Solution ◽  
Simultaneous Analysis ◽  
Phthalate Ester ◽  
Florisil Column ◽  
Vegetable Samples ◽  
Chemical Residues ◽  
Florisil Column Chromatography ◽  
Rice Samples

Abstract A simplified method suitable for simultaneous analysis of chlorinated pesticide and phthalate ester residues in various foods was developed. Chemical residues were quantitatively extracted from fatty and vegetable samples with acetonitrile as follows: Chemical standard in 0.5 mL ethanol solution was added to 10 g homogenized sample. After 3 hr, pork and beef were extracted 3 times with 20 mL portions of acetonitrile. The acetonitrile layers were diluted with water and extracted with n-hexane. Rice samples were combined with 10 mL water, 5 mL acetonitrile, and 1 mL ethanol and extracted 3 times with 20 mL portions of n-hexane. The re-hexane concentrate from each sample was submitted to AgNO3-coated Florisil column chromatography. The AgNO3 coating adequately adsorbed interfering coextractives. Extracts of fish and vegetable samples were separated into 2 fractions by the above column chromatography. Supplemental cleanup procedures were also developed to accurately determine phthalate esters eluted in the second fraction. Satisfactory gas chromatograms were obtained for most samples.

A Method for Fractional Determination of Soybean Sterols in Four Classes by Florisil Column Chromatography

1974 ◽  
Vol 38 (9) ◽  
pp. 1661-1667
Author(s):  
Masayuki Katayama ◽  
Ching Tsang Hou ◽  
Norman C. Chen ◽  
Takako Hirota ◽  
Toshiko Kiribuchi ◽  
...  
Keyword(s):  
Column Chromatography ◽  
Florisil Column ◽  
Florisil Column Chromatography

Gas-Liquid Chromatographic Determination of Permethrin in Bovine Tissues

1979 ◽  
Vol 62 (6) ◽  
pp. 1309-1311
Author(s):  
Delbert D Oehler
Keyword(s):  
Liquid Chromatography ◽  
Electron Capture ◽  
Chromatographic Determination ◽  
Chromatographic Column ◽  
Gas Liquid Chromatography ◽  
Florisil Column ◽  
Bonded Phase ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A method is presented for the determination of permethrin (m-phenoxybenzyl cis,trans-(±)-3-(2,2-dichlorovinyl) - 2,2 - dimethylcyclopropanecarboxylate) in bovine tissues. Fat and muscle samples were cleaned up first by liquid-liquid partition on a bonded phase chromatographic column. Final cleanup of fat and muscle was performed on a short Florisil column. Liver, kidney, spleen, and heart tissues only required cleanup on a Florisil column before quantitation of permethrin by electron capture gas-liquid chromatography.

Automated Sample Cleanup for Pesticide Multiresidue Analysis. Part II—Design and Evaluation of Column Chromatography Module

1984 ◽  
Vol 67 (4) ◽  
pp. 783-789
Author(s):  
Fred M Gretch ◽  
Joseph D Rosen
Keyword(s):  
Column Chromatography ◽  
Pesticide Residues ◽  
Continuous Flow ◽  
Flow System ◽  
Organophosphorus Pesticides ◽  
Multiresidue Analysis ◽  
Florisil Column ◽  
Continuous Flow System ◽  
Florisil Column Chromatography ◽  
Organochlorine And Organophosphorus Pesticides

Abstract An automated, continuous flow system is described for Florisil column chromatography of pesticide residues from food extracts. Evaluation of the system using 5 common organochlorine and organophosphorus pesticides in 2 crop matrices demonstrates essentially no difference in recovery or precision between automated and currently used manual analyses. The automated procedure uses only 20% of the solvents and adsorbents used in the manual procedure and is 3 times faster.

Phospholipids of a Bone Matrix Calcification Nucleator

1978 ◽  
Vol 57 (5-6) ◽  
pp. 731-734 ◽  
Author(s):  
J. Ennever ◽  
James J. Vogel ◽  
Linda J. Riggan
Keyword(s):  
Liquid Chromatography ◽  
Column Chromatography ◽  
Porous Glass ◽  
Bone Matrix ◽  
Phosphatidyl Serine ◽  
Gas Liquid Chromatography ◽  
Phospholipid Complex ◽  
Chromatography Analysis ◽  
Glass Column

Phospholipids of a bone matrix calcification nucleator wre identified as mono-and diphosphoinositides and phosphatidyl serine. The nucleator, a protein-phospholipid complex, was dissociated by acidified-solvent porous-glass column chromatography. Analysis was by gas-liquid chromatography.

Collaborative Study of the Determination of Endosulfan, Endosulfan Sulfate, Tetrasul, and Tetradifon Residues in Fresh Fruits and Vegetables

1976 ◽  
Vol 59 (1) ◽  
pp. 209-212
Author(s):  
Lawrence R Mitchell
Keyword(s):  
Liquid Chromatography ◽  
Petroleum Ether ◽  
Electron Capture ◽  
Fruits And Vegetables ◽  
Methylene Chloride ◽  
Collaborative Study ◽  
Gas Liquid Chromatography ◽  
Endosulfan Sulfate ◽  
Florisil Column

Abstract A method for the determination of endosulfan I, endosulfan II, endosulfan sulfate, tetrasul, and tetradifon residues in fresh fruits and vegetables was studied collaboratively. The method consists of extraction of the product with acetonitrile, extract cleanup by partition with petroleum ether and elution from a Florisil column with mixtures of hexane, methylene chloride, and acetonitrile, and determination of the residues by electron capture gas-liquid chromatography. This method was studied by 8 collaborators, using apples and cucumbers as the samples. Each sample was spiked with 2 levels of each pesticide. The average per cent recoveries for apples and cucumbers, respectively, were as follows: endosulfan I, 103.6 and 101.5; endosulfan II, 102.9 and 100.0; endosulfan sulfate, 100.9 and 92.9; tetrasul, 98.8 and 102.2; and tetradifon, 106.4 and 101.9. The method has been adopted as official first action.

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