RESUMO
The response of the electron-capture detector to organic compounds is poorly defined, and the steroids are no exception to this observation. For those steroids which are naturally electron-capturing, the structures of the electrophores will be defined. Other steroids can be made electron-capturing by the formation of appropriate derivatives. Some new or infrequently used reagents for this purpose (flophemesyl ethers, t-bulflophemesyl ethers, pentafluorophenylhydrazone derivatives and halogen-substituted aromatic boronic acids) are described.
Assuntos
Esteroides/análise , Animais , Cromatografia Gasosa/métodos , Ecdisona/análise , Fluorocarbonos , Humanos , Indicadores e Reagentes , Acetato de Melengestrol/análise , Silício , Relação Estrutura-AtividadeRESUMO
Acrylamide in biological samples can be determined by gas chromatography with electron-capture detection after conversion to its 2,3-dibromopropionamide derivative. The derivatization is carried out in aqueous solution, plasma or tissue homogenates by ionic bromination and the reaction conditions and sample clean-up are described. The detection limit corresponds to 9.5.10(-12)g of acrylamide on column or 8.4.10(-9)g in the final biological extract (0.5 ml). The overall recovery of acrylamide spiked samples at the nanogram level exceeds 80%. It was found that the accumulation of free acrylamide in the sciatic nerve distal region of rats intoxicated with acrylamide was less than 2-8 ppm.