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

Gas-Liquid Chromatographic Determination of Kepone in Field-Collected Avian Tissues and Eggs

1978 ◽  
Vol 61 (1) ◽  
pp. 08-14 ◽  
Author(s):  
Charles J Stafford ◽  
William L Reichel ◽  
Douglas M Swineford ◽  
Richard M Prouty ◽  
Martha L Gay
Keyword(s):  
Mass Spectrometry ◽  
Chromatographic Determination ◽  
Bald Eagle ◽  
Gas Liquid Chromatography ◽  
Tissue Samples ◽  
Florisil Column ◽  
Average Recovery ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A procedure is described for determining Kepone (decachlorooctahydro-l,3,4-metheno-2H-cyclobuta [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 H2SO4-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.

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.

Collaborative Study of the Determination of Poly chlorinated Biphenyls in Paperboard

1974 ◽  
Vol 57 (3) ◽  
pp. 518-521
Author(s):  
Charles E Finsterwalder
Keyword(s):  
Potassium Hydroxide ◽  
Collaborative Study ◽  
Gas Liquid Chromatography ◽  
Florisil Column ◽  
Average Recovery ◽  
Alcoholic Potassium Hydroxide ◽  
Aroclor 1242 ◽  
The Mean ◽  
Ppm Level

Abstract Eleven laboratories collaboratively studied a method for the determination of polychlorinated biphenyls (PCBs) (Aroclors 1242 and 1254) in paperboard, which involves alcoholic potassium hydroxide extraction, Florisil column cleanup, and electron capture gas-liquid chromatography. Blank paperboard spiked with 2 levels of each Aroclor and paperboard which had Aroclor 1242 incorporated during manufacture were analyzed. Average recovery of Aroclor 1242 at the 12.5 ppm level was 80.8%; at the 8.2 ppm level, 87.8%. Average recovery of Aroclor 1254 at the 12.3 ppm level was 87.0% ; at the 8.9 ppm level, 85.4%. The mean recovery of Aroclor 1242 from the specially prepared paperboard was 5.6 ppm, with a standard deviation of 15.8%. The method has been adopted as official first action.

Quantitative Determination of Sorbic Acid in Cheddar Cheese by Gas-Liquid Chromatography

1971 ◽  
Vol 54 (2) ◽  
pp. 361-363
Author(s):  
D E LaCroix ◽  
N P Wong
Keyword(s):  
Liquid Chromatography ◽  
Ethylene Glycol ◽  
Quantitative Determination ◽  
Sorbic Acid ◽  
Cheddar Cheese ◽  
Gas Liquid Chromatography ◽  
Glycol Adipate ◽  
Average Recovery ◽  
Ethylene Glycol Adipate

Abstract A rapid method is described for the extraction and quantitative determination of sorbic acid in Cheddar cheese. Cheddar cheese is impregnated onto a Celite 545 column, extracted with acetonitrile, and analyzed for sorbic acid by gas-liquid chromatography, using a 7.5% ethylene glycol adipate + 2% H3PO4 column. Average recovery values for known amounts of sorbic acid were 107%.

Gas-Liquid Chromatographic Determination of Sodium Fluoroacetate (Compound 1080)

1980 ◽  
Vol 63 (1) ◽  
pp. 49-55
Author(s):  
Iwao Okuno ◽  
Dennis L Meeker
Keyword(s):  
Liquid Chromatography ◽  
Tissue Sample ◽  
Chromatographic Determination ◽  
Gas Liquid Chromatography ◽  
Tissue Samples ◽  
Fluoroacetic Acid ◽  
Pentafluorobenzyl Bromide ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

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.

Gas-Liquid Chromatographic Determination of Choline in Low and High Potency Multiple Vitamin Tablets and Liver Preparations

1974 ◽  
Vol 57 (2) ◽  
pp. 341-342
Author(s):  
Caesar B Garavelli
Keyword(s):  
Liquid Chromatography ◽  
Quantitative Determination ◽  
Chromatographic Determination ◽  
Gas Liquid Chromatography ◽  
High Potency ◽  
Average Recovery ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A procedure is described for the quantitative determination of 0.020—6.0 mg choline in low and high potency reference multiple vitamin tablets and standard liver preparations. The trimethylamine quantitatively produced in a sealed tube by treatment with aqueous 5 0% alkali is simultaneously extracted with 0.200—0.500 ml of an isobutanol-ethanol (1+1) mixture and determined by gas-liquid chromatography. An average recovery of 100 ± 3 % was obtained.

Monitoring drug concentrations in a case of combined overdosage with primidone and methsuximide.

1976 ◽  
Vol 22 (6) ◽  
pp. 915-921 ◽  
Author(s):  
G F Johnson ◽  
C J Least ◽  
J W Serum ◽  
E B Solow ◽  
H M Solomon
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Liquid Chromatography ◽  
Gas Chromatography Mass Spectrometry ◽  
Gas Liquid Chromatography ◽  
Therapeutic Decision ◽  
Serum Samples ◽  
Monitoring Drug ◽  
Drug Concentrations

Abstract We describe a case of fatal overdosage with primidone and methsuximide. During the early phase of the patient's hospital course we found concentrations of methsuximide, N-desmethylmethsuximide, and primidone in serum that far exceeded the usual therapeutic concentrations, as determined by gas-liquid chromatography. Determination of N-desmethylmethsuximide in peritoneal fluid demonstrated concentrations comparable to those in serum. This led to the therapeutic decision to manage the patient by dialysis. Subsequently, serum samples collected during the course of hospitalization were analyzed quantitatively by gas-liquid chromatography for methsuximide, N-desmethylmethsuximide, primidone, phenobarbital, and diphenylhydantoin. Selected serum specimens were also analyzed by gas chromatography-mass spectrometry, and N-methyl-2-hydroxymethyl-2-phenylsuccinimide, a metabolite of methsuximide not previously described in human serum, was identified by analysis of its mass spectrum.

UV Determination of Naphthaleneacetic Acid in Apples and Potatoes

1970 ◽  
Vol 53 (1) ◽  
pp. 149-151
Author(s):  
Robert C Randall
Keyword(s):  
Spectrophotometric Method ◽  
Collaborative Study ◽  
Naphthaleneacetic Acid ◽  
Florisil Column ◽  
Average Recovery

Abstract Six collaborators studied a spectrophotometric method in which the chopped product is extracted with CHCl3, the extract is cleaned up on a Florisil column, and the residue is determined spectrophotometrically in the UV region (283 nm). The overall average recovery of the collaborative study was 93%. It is recommended that the method be adopted as official first action.

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