scholarly journals Methods for the Quantitative Determination of Biocides in Tobacco and Tobacco Products: Part VI: A Modified Procedure for Organochlorine, Organophosphorus and Carbamate Insecticide Residues in Tobacco

Author(s):  
E. Nesemann ◽  
F. Seehofer

AbstractThe screening procedure for the determination of pesticide residues in tobacco (organochlorine, organophosphorus and carbamate insecticides) published in 1970 has been improved by introduction of the dry-column chromatography as cleanup procedure. A new procedure has been developed for the detection of carbaryl and propoxur by gas chromatography. The extraction and cleanup method developed can be used to determine 11 organochlorine, 11 organophosphorus and 3 carbamate insecticides. The procedure can be applied to determine further insecticides and, in addition, fungicides, herbicides and metabolites. The recoveries of added pesticides at 0.5 ppm level are between 75 and 102 %. The coefficient of variation detected with parathion is 4.4 %

Author(s):  
E. Nesemann ◽  
F. Seehofer

AbstractThe method used in our laboratories since 1965 for the determination of menthol in tobacco and tobacco products has meanwhile been improved and made suitable for series analyses. Menthol is isolated from the mentholated material to be investigated by steam distillation The distillate containing the menthol in question (dissolved in acetone) is directly subjected to gas chromatography for quantitative determination. The recovery was found to amount to 97 %, the coefficient of variation to 1.45 %, and the detection limit to 0.002 mg of menthol per mI.


1965 ◽  
Vol 48 (5) ◽  
pp. 952-954
Author(s):  
Alfred D Thruston

Abstract The qualitative and quantitative determination of chlordane residues on raw agricultural products has been best achieved by gas chromatography techniques. While good recoveries (90–100% at the 0.1 ppm level) have been obtained from plant extracts with added standard chlordane, weathered chlordane residues show changes in number and size of gas chromatographic peaks. Chlordane at the 50 µg level, when exposed to the air at room temperature over a period of time, showed progressive decomposition and loss of the many components that make up chlordane.


Author(s):  
E. Nesemann ◽  
F. Seehofer

AbstractDuring the attempt to transfer to tobacco a method commonly used to determine metobromuron in foodstuffs, it became apparent that only very small amounts of metobromuron and less than 0.1 ppm 4-bromoanilin were found. Nor did the modification of this method produce better results, because metobromuron, apparently linked to tobacco components, cannot be extracted with aqueous acetonitrile. The tobacco was then distilled under hydrolysing conditions and the 4-bromoanilin released was bound as hydrochloride. After gas-chromatographic separation 4-bromoanilin is determined specifically with the microcoulometer (bromine) and with the Coulson detector (nitrogen). The amount of metobromuron is calculated from the 4-bromoanilin. With this method no difference can be made between intact metobromuron and 4-bromoanilin already metabolised from metobromuron. Recovery is 90 % for 4-bromoanilin and 92 % for metobromuron, the coefficient of variation is 3.0 %. In cigarettes whose tobacco had grown in soil which had been treated with 4 kg of Patoran per hectare before transplanting, a mean of 5.8 ppm metobromuron was found by this procedure.


Author(s):  
E. Nesemann ◽  
H. Rabitz ◽  
F. Seehofer

AbstractThe author's method (developed in 1966) for the determination of maleic hydrazide in tobacco has been improved by the introduction of a purification step using activated carbon. Interferences produced by reactive compounds other than maleic hydrazide can thus be eliminated. The procedure proved to be suitable for routine analysis. The coefficient of variation was found to range from 1 to 7 %. Added amounts of maleic hydrazide have been recovered at the 90-105 % level. The accuracy of the procedure could be confirmed by results comparatively obtained in three laboratories


1985 ◽  
Vol 68 (3) ◽  
pp. 419-421
Author(s):  
George Yip

Abstract Eleven collaborators participated in this study of a gas chromatographic method for the determination of pentachlorophenol (PCP) in gelatin. Following acid hydrolysis of a 2 g sample, PCP is extracted with hexane and partitioned into KOH solution. After reacidification, PCP is again extracted with hexane for determination by electron capture gas chromatography on a 1 % SP-1240DA column. Three duplicate practice samples (0.0, 0.5, and 1.5 ppm) and 5 blind duplicate collaborative samples (0.0, 0.02, 0.1, 0.5, and 2.0 ppm) were analyzed by each collaborator. Mean recoveries of PCP in the collaborative samples ranged from 88% at the 0.02 ppm fortification level to 102% at the 0.1 ppm level; the overall mean recovery was 96%. Interlaboratory coefficients of variation ranged from 16.4% for the 0.1 ppm fortification level to 22.9% for the 0.5 ppm level; the overall interlaboratory coefficient of variation was 19.5%. The method has been adopted official first action.


Author(s):  
E. Nesemann ◽  
F. Seehofer

AbstractA screening method has been developed for the qualitative and quantitative determination of vanillin, ethylvanillin, coumarin and dihydrocoumarin. The compounds are qualitatively determined by thin-layer chromatography after extraction of tobacco and purification of the extract. The quantitative determination is made by gas chromatography: Coumarin and dihydrocoumarin are determined directly and vanillin and ethylvanillin after silylation in the form of trimethylsilyl derivatives. Detection limit: thin-layer chromatography = 1 µg, gas chromatography = 0.02 µg. The coefficient of variation of the results obtained amounts to 2.4 % for vanillin and to 6.7 % for coumarin


1971 ◽  
Vol 54 (3) ◽  
pp. 711-712
Author(s):  
Martha Fuzesi

Abstract A gas chromatographic method is described for the quantitative determination of N-butyl-N-ethyl-α,α,α-trifluoro-2,6-dinitro-p-tolindine and α,α,α-trifluoro-2,6-dinitro-N,N-dipropyI-p-toluidine herbicides in formulations. The sample is extracted with benzene, and equal amounts of sample and reference solution in the same concentration range are analyzed by gas chromatography, using an electron capture detector and an SE-30/Diatoport S column. The method has been applied successfully to laboratory-prepared and commercial samples.


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