Extraction and derivatization in single drop （EDSD） coupled to matrix-assisted laser desorp- tion/ionization Fourier transform ion cyclotron resonance mass spectrometry （MALDI-FTICR-MS） was utilized to determine small molecular aldehydes in single puff smoke. Through employing Girard＇s reagent T as derivatization reagent, small molecular aldehydes （SMAs） transformed into quaternary ammonium salt, and the sensitivity of analysis for SMAs was significantly improved. Using this method, acetaldehyde and acrolein in single puff smoke were easily determined. This approach with an automatic potential provided a simple, rapid, and accurate procedure for the determination of SMAs in smoke.%本实验利用单液滴衍生化萃取技术（EDSD），并与基质辅助激光解吸一傅立叶变换离子回旋共振质谱方法（MALDI—FTICR—MS）结合起来，建立了一种用于分析烟气中小分子醛类物质的方法．选择吉拉尔特试剂工作为衍生化试剂，烟气中的小分子醛类物质可以形成季铵盐，其在MALDI—FTMS中的灵敏度显著提高．采用上述方法实现了对单口烟气中乙醛和丙烯醛的含量的分析．该分析方法易于实现自动化，为检测卷烟烟气中小分子醛类物质提供了一种简单、快速、准确的分析方法．
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