Gas-Liquid Chromatographic Analysis of N-(4-Chlorophenyl-N′-2,6-difluorobenzoyl)urea Insecticide After Chemical Derivatization

1976 ◽  
Vol 59 (4) ◽  
pp. 938-941
Author(s):  
James F Lawrence ◽  
Kanth M S Sundaram

Abstract The gas-liquid chromatographic analysis of TH 6040 (N-(4-chlorophenyl)-N′-(2,6-difluorobenzoyl)urea) was carried out after the insecticide was converted to its N,N′-dimethyl analog (N-methyl-N-(4-chlorophenyl)-N′-methyl-N′-(2, 6-difluorobenzoyl)urea). The methylation was accomplished in DMSO with sodium hydride and methyl iodide. The derivative was thermally stable and chromatographed as a single peak on 3% OV-1 at 235°C. Support for the structure of the product was given by mass spectrometry. The sensitivity of the product to electrolytic conductivity detection was approximately 50 ng for 50% full-scale deflection in the nitrogen mode and 70 ng for the same response in the chloride (reductive) mode. About 0.25 ng was required for 50% full-scale deflection by electron capture (at 1 × 10−9 amp standing current). Foliage samples were analyzed for TH 6040, using the proposed method.

1981 ◽  
Vol 45 (1) ◽  
pp. 159-165 ◽  
Author(s):  
G. P. Hazlewood ◽  
A. J. Northrop ◽  
R. M. C. Dawson

1. A method for gas-liquid chromatographic analysis of the dimethyl esters of a homologous series of diabolic acids is described.2. Only when combined with low-resolution mass spectrometry could the method be used to show unequivocally the existence of diabolic acids in natural products.3. Diabolic acids occurred naturally in rumen and faecal lipids of all ruminants examined but could not be detected in a number of ruminant tissue samples.4. Infused 14C-labelled (C16:0)2 diabolic acid was poorly absorbed by both simple-stomached and ruminant animals. Oxidation was more extensive in the ruminant, but there was no evidence of deposition of diabolic acid in the tissues of either animal.


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