RESUMO
Samples of belladonna pilular and powdered extract and tincture from two suppliers were analyzed by GLC as a cooperative effort between two laboratories to develop methodology with substantial improvements in sensitivity, specificity, precision, and working time over the present official method. This goal was achieved, but marked differences in response of the individual extracts to different isolation schemes were noted.
Assuntos
Alcaloides de Belladona/análise , Atropina/análise , Cromatografia Gasosa , Métodos , Escopolamina/análiseRESUMO
Gas-liquid chromatography GLC) coupled with column chromatography was used to accurately determine as little as 25 ppm p-chloroacetanilide in acetaminophen. p-Chloroacetanilide was eluted from a pH 8 phosphate-buffered diatomite partition column by using purified tetrachloroethylene (acetaminophen was retained). This solution was concentrated, internal standard (docosane) was added, and p-chloroacetanilide was determined by using a 0.9 m X 2 mm glass column packed with 3% Poly A 103 on Supelcoport and a flame ionization detector with electronic integration. Standard curves were linear for 10-100 ppm p-chloroacetanilide. Various chromatographic materials were investigated for optimal retention characteristics. High pressure liquid chromatography (HPLC) was also evaluated as an alternative; however, lack of reproducibility of the HPLC column favored the GLC procedure.