Abstract We describe a mass-spectrometric method based on the fast atom bombardment ionization technique in the negative-ion mode for measuring pregnanediol-3 alpha-glucuronide in diluted urine from women. The procedure requires addition of testosterone-17 beta-D-glucuronide (2.5 micrograms/25 microL) to the urine sample as internal standard, and the sample is added directly to the fast atom bombardment target with no further manipulation. We have assessed and evaluated the method by the traditional criteria of reliability.
N-Demethylation and dehalogenation of chlorpromazine (CPZ) were compared in six psychotic inpatients and in rats orally treated for 4 weeks with a daily CPZ dose of 5.4 (mean value) and 20 mg X kg-1 body weight, respectively, by measuring drug and metabolite plasma levels by means of a gas-liquid chromatography-nitrogen/phosphorus detector method. In patients the major plasma metabolite was found to be promazine (PZ), as identified by capillary GC-MS analysis. In rats, on the contrary, PZ represented only a small proportion of the compounds detected in plasma. The mean [PZ]/[CPZ] ratio after 4 weeks of treatment was 1.64 in patients and 0.08 in rats. The relative frequency of the N-demethyl metabolites in plasma, however, was similar in the two species. The mean [N-monodemethylated CPZ]/[CPZ] and [N-didemethylated CPZ]/[CPZ] ratios after 4 weeks of treatment were 0.45 and 0.24 in patients and 0.56 and 0.25 in rats, respectively. These findings suggest that dechlorination of CPZ in psychotic patients represents an important metabolic pathway.
The electron impact (70 eV) mass spectra of 15 monoterpene esters, namely bornyl, 4-terpinenyl and α-terpinyl propionates, butyrates, isobutyrates, valerates and isovalerates are reported and discussed: the fragment ions of diagnostic value for structural analyses are described.
Abstract A sensitive and accurate method to quantitate 17 primary aromatic amines in tobacco smoke has been set up. two Italian commercial brands of cigarette were smoked in a home‐made smoking machine; the amines in the smoke were trapped in dilute hudrochloric acid (containing 2H5‐aniline, 13C1‐o‐toluidine and 2H9‐4‐aminobiphenyl as internal standards) and, after extraction and purification, derivatized as pentafluoropro‐pionamides and measured by gas chromatography/mass spectrometry in the selected‐ion‐monitoring mode. Our results confirmed that side‐stream smoke contains total levels of aromatic amines about 50–60 times higher than those of main‐stream smoke of black‐tobacco cigarettes is richer in aromatic amines compared to light‐tobacco cigarettes.
Aqueous mixtures of formaldehyde and glutathione react to form a variety of cyclized adducts in addition to S-hydroxymethylglutathione. The adducts are in labile equilibrium with each other and are not readily separated. The structures of two of the other major adducts were determined by concerted application of 13C-1H two-dimensional chemical-shift correlation, fast-atom-bombardment mass spectrometry and tandem mass spectrometry to the adduct mixtures in aqueous solution.
A cage compound containing six secondary amines and three pyrrolic rings has been synthesized and used to complex β-glucopyranosides. The cage compound is remarkable in that it shows exclusive binding of the β-anomer. The synthesis of the receptor is notable due to its simplicity. The first transformation is driven to completion by the precipitation of the insoluble product. Next, imine reduction occurs in near-quantitative yield.
