Glycidol, 3-chloropropane-1,2-diol (3-MCPD), and 2-chloropropane-1,3-diol (2-MCPD), known as thermal processing contaminants, have been identified in heated tobacco product (HTP) aerosol, raising significant health concerns. Therefore, it is necessary to establish a quantitative analytical method for the release of them. In this study, ethyl acetate was used to extract the aerosol of HTP collected by Cambridge filter pad (CFP), the extract was derivatized with heptafluorobutyrylimidazole (HFBI), washed and dried before being analyzed by gas chromatography-mass spectrometry (GC-MS). The retention index and mass spectral characteristics of glycidol-HFBI derivative were characterized for the first time. The limits of quantification (LOQs) for glycidol, 3-MCPD and 2-MCPD were 58.32, 37.51 and 55.88 ng/cigarette respectively;the intra- and inter-day precision were less than 10% with recoveries ranging from 89% to 111%. The analysis results of eight domestic and foreign HTPs showed that: (1) The three target compounds were detected in all eight samples, indicating their widespread presence in HTP aerosol. (2) Significant variations in per-puff emission among samples suggested formulation and heating mode significantly impact glycidol and MCPDs release. (3) Glycidol and 3-MCPD were the major released substances, accounting for about 80% of the total three compounds emission. This study establishes a sensitive, reliable method for determining glycidol, 3-MCPD and 2-MCPD in HTP aerosol, providing critical technical support for health risk assessments.
A sensitive and selective gas chromatography–tandem mass spectrometry method was developed for the identification and quantification of five potential genotoxic impurities (PGIs), i.e., chloromethane, 2-chloropropane, 2-bromopropane, 4-chloro-1-butanol and diethyl sulfate, in abiraterone acetate. The method was validated according to the International Council for Harmonisation (ICH) guidelines. The linearity was established for the concentration range of 30–480 ng/mL (2-chloropropane, 2-bromopropane, 4-chloro-1-butanol and diethyl sulfate) and 90–1440 ng/mL (chloromethane). The correlation coefficient of each PGIs was >0.995. The extraction recoveries ranged from 90.49 to 106.79% for the five PGIs. The quantitation limit, detection limit, accuracy, precision, repeatability and stability of the method demonstrated that the method was an adequate quality control tool for quantitation and identification of chloromethane, 2-chloropropane, 2-bromopropane, 4-chloro-1-butanol and diethyl sulfate at trace levels in drug substances and drug products.
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