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CORESTA Meeting, Smoke Science/Product Technology, 2019, Hamburg, ST 38 (also presented at TSRC 2019)

Optimized method for determination of selective phenolic compounds in cigarette and cigar smoke by UHPLC-FLD

JIN X.C.; HURST T.J.; WAGNER K.A.
Altria Client Services, Research, Development & Regulatory Affairs, Richmond, VA, U.S.A.

Phenolic compounds, including phenol, catechol, and o-, m-, and p-cresol are included in the “Established List of the Chemicals and Chemical Compounds Identified by the FDA as Harmful and Potentially Harmful Constituents [HPHCs] in Tobacco Products and Tobacco Smoke”. CORESTA has developed and published a consensus standardized method for the determination of phenolic compounds in cigarette smoke, the CORESTA Recommended Method No. 78 (CRM 78): “Determination of selected phenolic compounds in mainstream cigarette smoke by HPLC-FLD”. CRM 78 has a run time of 34 minutes. We have developed a high throughput method that is based on CRM 78, which has a run time of ten minutes and uses Ultra-High Pressure Liquid Chromatography (UHPLC) and fluorescence detector (FLD) with a sub-2 µm pentafluoro-phenylpropyl phase analytical column. Data generated with the improved method were consistent with data generated using CRM 78. All requirements for method validation were met including linearity, accuracy, precision, limits of detection (LOD), limits of quantitation (LOQ), robustness, and standard and sample extract stability. For example, the repeatability for each analyte was less than 10 %, and the linearity was demonstrated with a coefficient of determination of > 0.995 for the calibration ranges of 0.05 µg/mL - 20 µg/mL for hydroquinone, catechol, and phenol, and 0.01 µg/mL - 4 µg/mL for resorcinol, p-cresol, m-cresol, and o-cresol. This optimized method provides a significant reduction in instrumental run time and larger dynamic range as compared to CRM 78. Furthermore, the method has been demonstrated to be fit-for-purpose for the analysis of cigar smoke where the levels of phenolic compounds are higher than in cigarette smoke. Data from commercial cigars and cigarettes will be presented.