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TSRC, Tob. Sci. Res. Conf., 2015, 69, abstr. 29

A single step solid-phase extraction method for gc/ms analysis of aromatic amines in mainstream cigarette smoke

HUANG C.B.; FLORA J.W.; WAGNER K.A.
Altria Client Services, Richmond, VA USA

As stated in the Federal Register (Vol. 77, No. 64) Docket No. FDA-2012-N-0143, Aromatic Amines (AAs) are included in the “Established List of the Chemicals and Chemical Compounds Identified by FDA as Harmful and Potentially Harmful Constituents [HPHCs] in Tobacco Products and Tobacco Smoke.” To date, no standardized method for AA determination in mainstream cigarette smoke has been developed. The two previously reported techniques for AA determination require either 2 or 3 solid phase cartridge extractions and the use of a solid phase extraction (SPE) manifold because of the complexity of the matrix and the trace amounts of AAs in cigarette smoke (ng per cigarette). These multistage techniques are time consuming and difficult to automate. The purpose of this work was to develop a simplified and automated extraction technique for 3 AAs (1-aminonaphthalene, 2-aminonaphthlene and 4-aminobiphenyl) in mainstream cigarette smoke without compromising analyte recovery. The method uses solid-phase mixed-mode cationic exchange cartridges (e.g., Waters Oasias® MCX or Phenomenex Strata™-X-C), is compatible with the RapidTrace® automation, eliminates multiple classes of interferences and samples can be analyzed by gas chromatography with mass spectrometry (GC/MS). Recovery of AAs was evaluated using labeled internal standards and ranged from 48.2 to 52.4% for 1-aminonaphthalene, 2-aminonaphthlene and 4-aminobiphenyl with the cigarette smoke matrix and ranged from 77.7 to 85.0% without the sample matrix. Recovery yields were consistent with the previously proposed methodologies.