RESUMEN
A GLC technique with selected-ion monitoring is described for chlorambucil determination in plasma using [2H]chlorambucil as the internal standard. Chlorambucil is extracted from plasma with methylene chloride at pH 3 and converted to a thiazane derivative by reaction with 0.1 M sodium sulfide at 80 degrees. The carboxylic group of the chlorambucil derivative is derivatized with allyl bromide using extractive alkylation. Analysis by selected-ion monitoring was performed by focusing at m/e 305 (M) and 313. The relative standard deviation was +/- 5% (n = 5) at the 10-ng/ml level.
Asunto(s)
Clorambucilo/sangre , Alquilación , Clorambucilo/análogos & derivados , Cromatografía de Gases/métodos , Deuterio , HumanosRESUMEN
Negative-ion chemical ionization mass spectrometry with a conventional combined gas chromatograph-mass spectrometer has been used for the analysis of amphetamine-like compounds. Ammonia was used as the reagent gas, which gives rise to few but specific sample-fragment ions, such as (M--1)- as the base peak, m/z 91, and a smaller peak corresponding to the end part of the side chain. Five reference compounds and a urine sample from an overdose case were analyzed. Comparative positive-ion chemical ionization reference spectra were also recorded.
Asunto(s)
Anfetaminas/análisis , Anfetaminas/orina , Aniones , Efedrina/análisis , Cromatografía de Gases y Espectrometría de Masas , Humanos , Metanfetamina/análisis , Fenmetrazina/análisis , Fentermina/análisis , Fenilpropanolamina/análisisRESUMEN
The individual variations in human metabolism of methaqualone were studied after oral administration of therapeutic doses. The effect of antabuse on the drug metabolism as well as metabolites in some autopsy cases were also studied. The metabolites were identified using the GC-MS computer technique, and the relative amounts of the indicated metabolites were calculated from the sum of the peak heights in the gas chromatogram. The results show that the individual variations were small in the cases of therapeutic doses and that antabuse did not interact with the metabolism of methaqualone. Large amounts of one single metabolite 2-methyl-3-[phenyl(2'-methyl-4-hydroxy)]-4(3H)-quinazolinone was found in the bile from the two autopsy cases where the bile was also collected.