Search PubMed⌕ Search

Biomedical subjects

J F Lawrence

Publications and source records attributed to J F Lawrence.

At least 73 records · Page 4Linked to original sources

Comparison of electron-capture and electrolytic conductivity detection for the gas-liquid chromatographic analysis of some perfluoro derivatives of four agricultural chemicals.

The gas chromatographic response of four perfluoro derivatives, of four agricultural chemical [diethylstilbestrol] (DES) clopidol, linuron and carbofuran] was examined. The derivatives varied in fluorine content from 3 to 30 atoms per molecule. The sensitivities of the derivatives were found to be ca. 10-100 times greater by electron-capture detection than by electrolytic conductivity detection (halogen mode). The sensitivity also was found to increase with increasing fluorine content for all derivatives by electrolytic conductivity, whereas by electron capture, DES and clopidol exhibited similar responses with either the penta-, hepta-, or pentadeca-fluoro derivatives. The sensitivity of linuron and carbofuran derivatives by electron capture varied with increasing fluorine content. For detection by electron capture, the hepta-fluorobutyryl derivatives were preferred for DES and clopidol, and either the hepta-fluorobutyryl or the pentadecafluorooctanoyl derivatives for linuron and carbofuran. For detection by electrolytic conductivity, the pentadecafluorooctanoyl derivatives were superior for all four compounds.

Carbofuran↗

Evaluation of electrolytic conductivity detection for gas-liquid chromatographic screening of some organonitrogen herbicides and fungicides in foods.

Electrolytic conductivity detection for the gas-liquid chromatographic (GLC) screening of 15 organonitrogen herbicides and fungicides was investigated. Spiked samples of crop material was extracted with acetone and the filtered sample extracts were partitioned with methylene chloride-petroleum ether (1+1) followed by second and third extractions with methylene chloride. The combined organic extracts were evaporated to dryness and the residues were dissolved in hexane for cleanup on a 2% deactivated Florisil column. The pesticide fractions were determined directly by GLC. All pesticides could be detected at 0.1 ppm in the foods studied.

Chromatography, Gas↗

Gas chromatographic analysis of heptafluorobutyryl derivatives of some carbamate insecticides.

The gas chromatography (GC) of a number of carbamate insecticides as their heptafluorobutyryl derivatives has been studied. The reaction makes use of heptafluorobutyric anhydride with trimethylamine in benzene as a catalyst. Conversion of the insecticides to their products is complete in 15-20 min at room temperature. The same reaction proved satisfactory for trifluoroacetylation. The excess reagent and trimethylamine are removed by partitioning with water in the reaction test tube. An aliquot of the organic phase is used for analysis. The heptafluorobutyryl derivatives are stable for several days on the lab bench without removal of the aqueous phase from the test tube. GC detection was carried out with a Coulson conductivity detector in the halogen (reductive) mode. About 1.0 ng produced a 50% full-scale response for most of the carbamates (3 min retention time) on 3% OV-1. This method was applied to the analysis of several carbamates spiked in corn, mustard greens, turnip greens, lettuce and cabbage.

Butyrates↗

A comparison of electron-capture GLC, electrolytic-conductivity GLC and UV-absorption HPLC for the analysis of some herbicides in foods.

A comparison of gas chromatography with electron-capture or electrolytic-conductivity (nitrogen mode) detection, and high-pressure liquid chromatography (HPLC) with UV-absorption detection (254 nm) was carried out for the analysis of several herbicides in foods. Linuron, propanil, terbacil, benzoylprop-ethyl, and the fungicide DCNA in samples of cabbage, corn, potato, and wheat spiked at 2 and 0.2 ppm were examined. The pesticides were extracted with acetone, partitioned into petroleum ether-methylene chloride, and cleaned up on a 2% deactivated Florisil column before direct chromatographic analysis. Electron-capture gas-liquid chromatography (GLC) was most suitable for DCNA and benzoylprop-ethyl while UV-absorption HPLC was best for terbacil analysis. Linuron and propanil gave similar results for both electron-capture GLC and HPLC. Electrolytic-conductivity GLC could detect all pesticides at the 0.2 ppm level and exhibited the least number of extraneous peaks in the chromatograms.

Aniline Compounds↗

Gas-liquid chromatographic analysis and chemical confirmation of azodrin (monocrotophos) residues in strawberries.

A gas-liquid chromatographic (GLC) method is described for the analysis and confirmation of azodrin (monocrotophos, 3-(dimethoxyphosphinyl)-N-methyl-cis-crotonamide) residues in strawberrires. The strawberries are extracted with acetone, and the filtrate is partioned with a mixture of methylene chloride and petroleum ether followed by further extraction with methylene chloride. The organic phases are combined, dried with anhydrous sodium sulfate, and concentrated to a small volume for GLC analysis on a 3% OV-210 column with flame photometric detection. Identity of the compound is confirmed by chromatography on the same column after trifluoroacetylation of an aliquot of the strawberry extract. The detection limit is about 2 ppb. The types of strawberry samples analyzed were fresh, frozen, pureed, and jam.

Chromatography, Gas↗

Evaluation and confirmation of an alkylation-gas-liquid chromatographic method for the determination of carbamate and urea herbicides in foods.

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.

Alkylation↗

High-pressure liquid chromatographic analysis of urea herbicides in foods.

A method is described for the direct analysis of the urea herbicides linuron, monuron, diuron, chlorbromuron, fluometuron, chloroxuron, and fenuron in cabbage, corn, potatoes, turnip, and wheat at 0.01-1.0 ppm. The samples are extracted with acetone; the filtrate is partitioned with hexane-methylene chloride (1+1) followed by 2 other extractions with methylene chloride. The organic phases are dried and concentrated for column chromatographic cleanup on 2% deactivated Florisil. The column fractions are evaporated just to dryness and redissolved in 10 ml isooctane for high-pressure liquid chromatography on a 25 cm silica gel (5 mum) column. Isopropanol in isooctane is the mobile phase, and compounds are measured by ultraviolet absorption at 254 nm. Recoveries are greater than 80% in most cases. These results are confirmed by alkylation with sodium hydride-methyl iodide in dimethyl sulfoxide to form the methyl products which are analyzed by the same chromatographic system or by gas-liquid chromatography.

Chromatography, High Pressure Liquid↗

Analysis of the diazinon metabolites G 27550 and GS 31144 by gas-liquid chromatography with nitrogen-specific detection after derivatization.

The alkylation and silylation of the diazinon metabolites G 27550 (2-isopropyl-4-methyl-6-hydroxypyrimidine) and GS 31144 [2-(1'-hydroxy-1'-methyl)-ethyl-4-methyl-6-hydroxypyrimidine] with methyl iodide/sodium hydride and bis-(trimethylsilyl)-trifluoroacetamide, respectively, were examined for use as confirmation techniques for these metabolites in sample material. The methods proved to be rapid and simple. The derivatives chromatographed well on 4% SE-30/6% QF-1. Electrolytic conductivity detection proved satisfactory for the derivatives with minimum cleanup. The techniques were successfully applied to the analysis of the two metabolites in dog urine in the range of 1 ppm.

Alkylation↗

Gas-liquid chromatographic determination of technical chlordane residues in food crops: interpretation of analytical data.

An interlaboratory investigation of technical chlordane residues in food crops was carried out to determine the most practical and consistent method of reporting results. Using a technical chlordane reference standard, 8 gas chromatographic stationary phases were studied for their resolution capabilities. The best separations were obtained with SE-30 and its OV-1 equivalent. Using these columns and electron capture detection, potatoes and carrots from supervised field experiments were analyzed in duplicate and quantitated by using 4 methods of calculation. The data were statistically treated to determine the precision and bias for each method. Also, 1 sample was analyzed in duplicate on 2 different occasions by 6 laboratories to substantiate the initial conclusions. Based on the criterion of high precision it is suggested that a comparison of total area under the chromatogram of the sample with total area of standard technical chlordane be the method of quantitation. Only peaks which are common to both standard and sample have any significance in this type of calculation.

Chlordan↗