SUMMARYAmong the more than 5000 chemicals reported in cigarette smoke condensate (CSC), heterocyclic aromatic amines (HAAs) are considered to be a contributor to observed biological activity. HAAs are non-volatile and are reported at ppb levels in CSC. A new method for HAA analysis at the trace level is reported here. N, O-Bis(trimethylsilyl)trifluoroacetamide (BSTFA) containing 1% trimethylchlorosilane was employed to derivatize amino groups by heating the reagent containing a sample of CSC at 80 °C for 30 min followed by analysis employing gas chromatography-mass spectroscopy (GC-MS) in the selected-ion-monitoring (SIM) mode. This derivatization method afforded symmetrical peak shapes on a ZB-50 stationary phase and achieved instrumental limits of quantification (LOQ) at 10:1 S/N from -1 ng/mL for AαC to120 ng/mL for Glu-P-1. The chemical identity of each derivative was confirmed by comparison of retention time and mass spectra of standards. The latter were characterized by the following ions:, and m/z 73 (i.e., trimethylsilyl). CSC and its base sub-fractions were studied using the GC-MS method. Ten HAAs were screened and five were quantified in cigarette smoke condensate, while 2-5 HAAs were quantified in each of three base sub-fractions. . Diese Derivatisierungsmethode führte zu symmetrischen Peakformen auf einer stationä-ren ZB-50-Phase und erreichte instrumentelle Bestimmungsgrenzen (LOQ) bei S/N 10:1 von -1 ng/ml für AαC bis 120 ng/ml für Glu-P-1.
A procedure has been developed for filter analysis whereby the cellulose acetate is dissolved in acetonitrile to release any trapped nicotine. Dissolving the filter eliminates time consuming steam distillation or solvent extraction steps and assures that the recovery of nicotine is complete. After the filter is dissolved, the cellulose acetate is precipitated by addition of an amine-phosphate buffer and an aliquot of the filtered solution is analysed by high-pressure liquid chromatography (HPLC). Two methods of HPLC analysis are described. In both cases the separation is achieved on a cyano-bonded silica column and detection is by ultra-violet absorption at 254 nm. Different mobile phases are used in the two methods. In the first procedure, a diethylamine-phosphate buffer at pH 7.56 is used while in the second procedure, a dimethylamine-phosphate buffer at pH 3.00 is used. Analytical results are equivalent for both chromatographic methods, but the second procedure may offer extended analytical column life. Results of a study relating the structure of the amine in the mobile phase to nicotine retention are presented. The amount of nicotine trapped on cellulose acetate filters during smoking was determined with increasing intervals between smoking and analysis. These results demonstrate that nicotine is stable on filters and previous problems of analysis were caused by difficulty in removal from aged filters.
scite is a Brooklyn-based organization that helps researchers better discover and understand research articles through Smart Citations–citations that display the context of the citation and describe whether the article provides supporting or contrasting evidence. scite is used by students and researchers from around the world and is funded in part by the National Science Foundation and the National Institute on Drug Abuse of the National Institutes of Health.
hi@scite.ai
10624 S. Eastern Ave., Ste. A-614
Henderson, NV 89052, USA
Copyright © 2024 scite LLC. All rights reserved.
Made with 💙 for researchers
Part of the Research Solutions Family.