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

1982 ◽  
Vol 65 (5) ◽  
pp. 1102-1105 ◽  
Author(s):  
Iwao Okuno ◽  
Dennis L Meeker ◽  
Robert R Felton
Keyword(s):  
Ethyl Acetate ◽  
Animal Tissue ◽  
Gas Liquid Chromatography ◽  
Tissue Samples ◽  
Fluoroacetic Acid ◽  
Acetone Water ◽  
Liquid Chromatographic Method ◽  
Special Apparatus ◽  
Liquid Chromatographic

Abstract A method capable of determining 0.1 ppm 1080 (sodium fluoroacetate) in 1 g animal tissue was developed. It involves extraction of 1080 from the sample with acetone-water, and then evaporation of the acetone followed by extraction of 1080 as fluoroacetic acid from water with ethyl acetate. Ethyl acetate is removed by volatilization from fluoroacetic acid which is retained as the triethanolammonium fluoroacetate salt. Fluoroacetic acid is subsequently derivatized with α-bromo-2,3,4,5,6-pentafluorotoluene and quantitated by gas-liquid chromatography with an electron capture detector. The method is rapid and requires no special apparatus or equipment and no more than 12 ml of any one solvent. Recoveries of 1080 from tissue samples fortified with 0.1-100 ppm averaged about 85%.

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.

Rapid Gas-Liquid Chromatographic Method for Determining Residues of Ethephon (2-Chloroethyl Phosphonic Acid) in Tomatoes

1976 ◽  
Vol 59 (5) ◽  
pp. 1185-1187
Author(s):  
George F Ernst ◽  
Marcia J P T Anderegg
Keyword(s):  
Liquid Chromatography ◽  
Ethyl Acetate ◽  
Phosphonic Acid ◽  
Growth Regulator ◽  
Chromatographic Method ◽  
Gas Liquid Chromatography ◽  
Flame Photometric Detector ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Abstract A rapid method is described for the determination of the growth regulator ethephon (2-chloroethyl phosphonic acid) in tomatoes. Samples are extracted with ethyl acetate. The extract is methylated, decolorized with carbon, and analyzed by gas-liquid chromatography on a column packed with 15% QF-1/10% DC-200 on Chromosorb W (HP). A flame photometric detector is used. Recoveries from tomatoes fortified with 0.1–11.0 ppm ethephon were 78—98%. The sensitivity of this method is about 0.1 ppm.

High-performance liquid-chromatographic separation and fluorescence measurement of biogenic amines in plasma, urine, and tissue.

1978 ◽  
Vol 24 (8) ◽  
pp. 1317-1324 ◽  
Author(s):  
T P Davis ◽  
C W Gehrke ◽  
C W Gehrke ◽  
T D Cunningham ◽  
K C Kuo ◽  
...  
Keyword(s):  
Ethyl Acetate ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Fluorescence Measurement ◽  
Tissue Samples ◽  
Liquid Chromatographic Separation ◽  
Exciting Wavelength ◽  
Liquid Chromatographic Method ◽  
Stepwise Gradient ◽  
Liquid Chromatographic

Abstract We describe a high-performance liquid-chromatographic method for measuring histamine, norepinephrine, octopamine, normetanephrine, dopamine, serotonin, and tyramine in plasma (2 ml), brain (0.2 g), or urine. These amines are modifed by pre-column derivatization with o-phthalaldehyde, which stabilizes the molecules, facilitates extraction, and improves detection of nanogram amounts. Before separation, samples were neutralized with KOH and immediately derivatized and extracted into ethyl acetate, in which derivatives were stable for longer than 24 h. Interfering amino acids were removed from ethyl acetate by partitioning twice with Na2HPO4 buffer (pH 10.0). Separation was complete in about 90 min on a "mu Bondapak/phenyl" column, with which a stepwise gradient of methanol/phosphate buffer (pH 5.1) was used. A variable-wavelength fluorometer was used (exciting wavelength, 340 nm; emission wavelength, 480 nm). Amount and response were linearly related from 1 to 200 pmol. Precision (CV) for retention times was 1%, for derivatization and injection 2.5%. Analytical recoveries of the seven amines from 2 ml of plasma fortified with 200 pmol averaged 65% (CV approximately 8%). Data on rat-brain tissue samples are compared with results by the trihydroxyindole method. Application of the method to urine from normal persons and a patient with a brain tumor is demonstrated.

Quantitative Determination of L-Ascorbic Acid by Gas-Liquid Chromatography

1974 ◽  
Vol 57 (6) ◽  
pp. 1346-1348
Author(s):  
Janis E Schlack
Keyword(s):  
Ascorbic Acid ◽  
Lead Acetate ◽  
Chromatographic Method ◽  
Ethanol Solution ◽  
Lead Salt ◽  
Gas Liquid Chromatography ◽  
Trimethylsilyl Derivative ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Abstract A gas-liquid chromatographic method for L-ascorbic acid in foods and food products has been devised. Ascorbic acid is extracted into an ethanol solution, precipitated with lead acetate, regenerated from the lead salt as its trimethylsilyl derivative, and chromatographed on an SE- 30 column. Recoveries averaged 100.1%; the standard deviation was ±0.23%.

High-Pressure Liquid Chromatographic Method for the Determination of Patulin in Apple Butter

1975 ◽  
Vol 58 (4) ◽  
pp. 754-756 ◽  
Author(s):  
George M Ware
Keyword(s):  
High Pressure ◽  
Acetic Acid ◽  
Liquid Chromatography ◽  
Ethyl Acetate ◽  
Chromatographic Method ◽  
High Pressure Liquid Chromatographic ◽  
Ultraviolet Detector ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Abstract Patulin is extracted from apple butter samples with ethyl acetate and the extract is cleaned up on a silica gel column, using benzene-ethyl acetate (75+25) as the eluant. High-pressure liquid chromatography, using a 25 cm Zorbax-Sil column, isooctane-ethyl ether-acetic acid (750+250+0.5) as the mobile solvent, and a 254 nm ultraviolet detector, is used for the determinative step. Under these conditions, patulin is eluted before 5-hydroxymethylfurfural, a component of apple butter which interferes with other liquid chromatographic and thin layer chromatographic methods. Recoveries of patulin added at levels of 34.6, 138.4, and 276.8 μg/kg ranged from 89.0 to 112.1%.

Evaluation and Confirmation of an Alkylation-Gas-Liquid Chromatographic Method for the Determination of Carbamate and Urea Herbicides in Foods

1976 ◽  
Vol 59 (5) ◽  
pp. 1061-1065
Author(s):  
James F Lawrence
Keyword(s):  
Sodium Methoxide ◽  
Chromatographic Method ◽  
Parent Compound ◽  
Sodium Hydride ◽  
Food Type ◽  
Gas Liquid Chromatography ◽  
Liquid Chromatographic Method ◽  
Herbicide Concentration ◽  
Liquid Chromatographic

Abstract An alkylation technique using methyl iodide and sodium hydride in dimethyl sulfoxide has been evaluated for 3 carbamate and 7 urea herbicides in 9 foods. Recoveries ranged from 56 to 113%, depending on herbicide, concentration, and food type. Reproducibility was about ±6% at 0.1 and 1.0 ppm. Identities of the herbicides were confirmed at these and lower levels by cleaving the aniline moiety from the alkylated herbicides with sodium methoxide in methanol, followed by gas-liquid chromatography on the same column as the parent compound. An electrolytic conductivity detector in the nitrogen mode was used for all analyses. Minimum detectable levels were in the range of 0.005–0.01 ppm in the foods studied.

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.

Gas-Liquid Chromatographic Method for the Determination of Fat-Soluble Vitamins. I. Application to Vitamin E

1964 ◽  
Vol 47 (2) ◽  
pp. 371-376
Author(s):  
David A Libby ◽  
Alan J Sheppard
Keyword(s):  
Vitamin E ◽  
Response Curve ◽  
Stationary Phases ◽  
Individual Response ◽  
Gas Liquid Chromatography ◽  
Liquid Chromatographic Method ◽  
Fat Soluble Vitamins ◽  
Liquid Chromatographic ◽  
Acetate Form

Abstract Current methods for the determination of vitamin E are unsatisfactory for many preparations. Since the majority of food and pharmaceutical fortification with vitamin E is in the acetate form, it is essential to be able to measure this and the other forms accurately. Gas-liquid chromatography was used to separate and quantify certain major tocopherol forms, to separate the acetate form from the alcohol form, and to measure microgram quantities accurately. Individual and mixed tocopherol standards have been used, and responses and sensitivities determined. Calibration studies show that each tocopherol exhibits an individual response curve. Vitamin E can be chromatographed on a variety of stationary phases.

Gas-Liquid Chromatographic Determination of Nifursol in Frozen Turkey Tissues to Ten Parts Per Billion

1975 ◽  
Vol 58 (4) ◽  
pp. 694-699
Author(s):  
Larry J Frahm ◽  
Glenn M George ◽  
J Patrick Mcdonnell
Keyword(s):  
Ethyl Acetate ◽  
Chromatographic Determination ◽  
Peak Height ◽  
Gas Liquid Chromatography ◽  
Method Performance ◽  
Florisil Column ◽  
Column Eluate ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Nifursol (3,5-dinitrosalicylic acid (5-nitrofurfurylidene) hydrazide) is extracted into ethyl acetate from 10 g tissue in the presence of sodium sulfate. Tissue interferences are removed from the tissue extract by washing with petroleum ether after the extract has been transferred into an aqueous solution by evaporation of ethyl acetate. The drug is hydrolyzed under acid conditions to form 5-nitro-2-furaldehyde (5NF). After partition of 5NF from the aqueous phase into benzene the extract is further cleaned up on a Florisil column. The 5NF is eluted from the Florisil column with benzeneethyl acetate. Electron capture gas-liquid chromatography of a 10 μl injection of the concentrated column eluate is the determinative step. Quantitation is accomplished by comparison of the peak height of the sample to the peak height of the standard which is carried through the method simultaneously. Studies of method performance on turkey muscle, liver, kidney, and skin tissues fortified to contain 10 ppb nifursol show a recovery range of 87.4–95.0% and a coefficient of variation range of 5.7–11.2%.

High Pressure Liquid Chromatographic Determination of Imazalil Residues in Gtrus Fruit

1978 ◽  
Vol 61 (6) ◽  
pp. 1469-1474
Author(s):  
Shirley M Norman ◽  
David C Fouse
Keyword(s):  
High Pressure ◽  
Ethyl Acetate ◽  
Citrus Fruit ◽  
Chromatographic Determination ◽  
Fruit Peel ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract A high pressure reverse phase liquid chromatographic method is described for determining the fungicide imazalil (1-[2,4-dichlorophenyl) -2- (2-propenyloxy)ethyl] -1H-imidazole) residues in whole citrus fruit, peel, and pulp. Imazalil is extracted from the fruit with ethyl acetate, partitioned into acid and back into ethyl acetate for cleanup, and detected by ultraviolet absorbance at 202 nm. Recovery from whole ground fruit of known amounts of imazalil applied to the surface of intact fruit averaged 84% 24 hr after application and 80% after the fruit had been stored 4 weeks at 15°C.

Sign in / Sign up

Export Citation Format

Share Document