title: Selective determination of volatile N-nitrosamines by derivatization with diethyl chlorothiophosphate and gas chromatography with flame photometric detection.
abstract: A selective and sensitive method was developed for the determination of volatile N-nitrosamines by gas chromatography (GC). After denitrosation of N-nitrosamines with hydrobromic acid, the resulting secondary amines were converted into their N-diethylthiophosphoryl derivatives and then measured by GC using a DB-1701 capillary column with flame photometric detection. The calibration graphs for N-nitrosamines in the range 0.05-1 nmol were linear and sufficiently reproducible for quantitative determination. This method was successfully applied to cigarette smoke samples without prior clean-up. N-Nitrosamines and secondary amines were completely separated by extraction with diethyl ether containing 25% 2-propanol. Overall recoveries of N-nitrosamines added to cigarette smoke samples were 83-110%. By using this method, N-nitrosamines in these samples could be determined without any interference from coexisting substances. Analytical results for the contents of N-nitrosamines and secondary amines in mainstream and sidestream smokes of several cigarettes are presented.
authors.affiliation: Faculty of Pharmaceutical Sciences, Okayama University, Tsushima, Japan.
authors.forename: H
authors.initials: H
authors.lastname: Kataoka
authors.forename: S
authors.initials: S
authors.lastname: Shindoh
authors.forename: M
authors.initials: M
authors.lastname: Makita
mesh_terms: D000588:Amines / Q000032:analysis; D002273:Carcinogens / Q000032:analysis*; D002849:Chromatography, Gas / Q000379:methods*; D009602:Nitrosamines / Q000032:analysis* / Q000737:chemistry; D063086:Organothiophosphates / Q000737:chemistry*; D010947:Plants, Toxic; D012906:Smoke / Q000032:analysis*; D014026:Nicotiana
chemical_list: D000588:Amines; D002273:Carcinogens; D009602:Nitrosamines; D063086:Organothiophosphates; D012906:Smoke; C081941:O,O-diethyl chlorothiophosphate