RESUMO
The identification of residues of polychlorinated biphenyls in a test sample of Flores Chamomillae could be achieved by the retention behavior at gas chromatographic analyses on packed and capillary columns compared with reference standard Clophen A 60, respectively as well as well by capillary GC/MS using single ion monitoring of substance-characteristic ion mass.
Assuntos
Contaminação de Medicamentos , Plantas Medicinais/análise , Bifenilos Policlorados/análise , Cromatografia Gasosa , Cromatografia Gasosa-Espectrometria de MassasRESUMO
For the GC analysis of DDT isomers and metabolites in extracts of Flores Chamomillae end Radix Valerianae the separation on a packed QF-1/OV-17 column was compared with various capillary columns of the CP-Sil type. Identification of the individual compounds could be achieved by comparing the retention behavior, chemical transformation of DDT and DDE, as well as by capillary GC-MS using single ion monitoring of substance-characteristic ion mass. In this way, residues of p,p'-DDT, o,p'-DDE and p,p'-TDE could be identified.
Assuntos
DDT/análise , Contaminação de Medicamentos/análise , Resíduos de Praguicidas/análise , Plantas Medicinais/análise , Cromatografia Gasosa , Cromatografia Gasosa-Espectrometria de Massas , Extratos Vegetais/análiseRESUMO
A method for the identification and determination of HCH-and DDT-isomers and their respective metabolites in vegetable drugs is presented. The plant material is extracted with hexane in a Soxhlet apparatus in the presence of silicagel and sodium sulfate. For removing interfering endogenous plant constituents a Celite oleum column cleanup and usually and acetonitrile partitioning to follow are necessary. A mixed stationary phase OV-17/QF-1 has proved effective for the gc separation on packed columns. 3H-ECD is used for detection. For the quantitative determination by using an external standard the peak height measurement is recommended. Recoveries of all insecticides were in the order of 70-105% with coefficients of variation between 6 and 20%. To ensure the results the alkaline treatment and oxidation of extracts are proposed.