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TSRC, Tob. Sci. Res. Conf., 2015, 69, abstr. 71

Determination of diacetyl in e-vapor products using gas chromatography and mass spectrometry

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

While diacetyl is approved for food use, the United States National Institute for Occupational Safety and Health (US NIOSH) has suggested it may be associated with respiratory disease when heated and inhaled. NIOSH has defined safety limits for occupational exposure to diacetyl. Farsalinos and coworkers recently (2015) investigated 159 sweet-flavored e-vapor refill formulations where they observed that 110 contained measurable amounts of diacetyl with many exceeding NIOSH limits. Farsalinos and coworkers used a modified method developed for the analysis of carbonyls in mainstream cigarette smoke to quantify diacetyl in e-vapor formulations. This method was validated for e-vapor formulations and involved derivatization using 2,4-dinitrophenylhydrazine (DNPH) followed by high performance liquid chromatography (HPLC) with an ultraviolet (UV) detector. The purpose of this work was to develop a more sensitive and selective method for the analysis of diacetyl using gas chromatography and mass spectrometry (GC/MS). This method does not require derivatization, uses a labeled internal standard, and the MS is operated in the selected ion monitoring (SIM) mode to maximize selectivity and sensitivity. All requirements for method validation were met such as linearity, accuracy, precision, limits of detection (LOD), and limits of quantitation (LOQ). For example, the coefficient of determination is greater than 0.990, the calibration ranged from 0.1 µg/g to 16.2 µg/g of e-cigarette formulation and the recovery ranged from 90 to 110%. The method is suitable for potential regulatory reporting and the quality control purposes that may be needed in this product category.