The Determination of Diacetyl and Acetylpropionyl in Aerosols From Electronic Smoking Devices Using Gas Chromatography Triple Quad Mass Spectrometry

A reliable and sensitive method for the measurement of the level of diacetyl (2,3-butanedione) and acetylpropionyl (2,3-pentanedione) in the aerosol (both the particles and the suspending gas) of electronic smoking devices (e-cigarettes) has been developed. The method uses a gas chromatographic separation on a Carbowax type column with the measurement of the analytes on a triplequadrupole mass spectrometer working in positive MRM mode. The method has been validated using standard requirements regarding selectivity, sensitivity, recovery, accuracy, and repeatability. The limit of quantitation (LOQ) for the method was determined to be 0.41 ng/mL for diacetyl and 0.21 ng/mL for acetylpropionyl as measured for standards. These values translate to an LOQ of 0.082 ng/puff for diacetyl and 0.042 ng/puff for acetylpropionyl as measured for an e-cigarette with 50 puffs placed in 10 mL acetone. The samples analyzed included collected aerosols from several e-cigarettes, and a number of liquids used in electronic cigarettes (e-liquids). 3R4F Kentucky reference cigarette was also analyzed for evaluating the accuracy of the procedure, with good agreement with data from the literature. Diacetyl and acetylpropionyl were distributed in both particulate phase and also in vapor phase. The levels of diacetyl and acetylpropionyl in particulate phase collected from 3R4F cigarettes were found to represent only about 22% for diacetyl and only 31% for acetylpropionyl, while the vapor phase for diacetyl represented 78% and for acetylpropionyl 69% of the total analyte. The levels of diacetyl and acetylpropionyl in the aerosols of most electronic smoking devices were found to be very low, with a few exceptions. The analysis of the two analytes in several e-liquids available on the market showed a very large range of levels. Some of the e-liquids from the market are likely to have diacetyl and/or acetylpropionyl intentionally added.