0-(2,3,4,5,6-Pentafluorobenzyl)Hydroxylamine Hydrochloride as a Sensitive Derivatizing Agent for the Electron Capture Gas Liquid Chromatographic Analysis of Keto Steroids

1975 ◽  
Vol 13 (2) ◽  
pp. 97-104 ◽  
Author(s):  
K. T. Koshy ◽  
D. G. Kaiser ◽  
A. L. VanDerSlik
Keyword(s):  
Electron Capture ◽  
Chromatographic Analysis ◽  
Hydroxylamine Hydrochloride ◽  
Derivatizing Agent ◽  
Liquid Chromatographic Analysis ◽  
Liquid Chromatographic

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
Keyword(s):  
Mass Spectrometry ◽  
Electron Capture ◽  
Methyl Iodide ◽  
Chromatographic Analysis ◽  
Sodium Hydride ◽  
Full Scale ◽  
Chemical Derivatization ◽  
Liquid Chromatographic Analysis ◽  
Liquid Chromatographic ◽  
Full Scale Deflection

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.

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