Extraction and derivatization in single drop coupled to MALDI-FTICR-MS for selective determination of small molecule aldehydes in single puff smoke.
Extraction and derivatization in single drop coupled to MALDI-FTICR-MS for selective determination of small molecule aldehydes in single puff smoke.
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DOI：
10.1016/j.aca.2009.02.036
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发表时间：
2009-04
影响因子：
6.2
通讯作者：
Jianping Xie;Jie Yin;Shihao Sun;F. Xie;Xiang Zhang;Yinlong Guo
中科院分区：
文献类型：
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作者：
Jianping Xie;Jie Yin;Shihao Sun;F. Xie;Xiang Zhang;Yinlong Guo
单滴萃取和衍生化 (EDSD) 与基质辅助激光解吸/电离傅里叶变换离子回旋共振质谱 (MALDI-FTICR-MS) 相结合，用于测定单口烟雾中的小分子醛 (SMA)。使用二苯胺、2,5-二羟基苯甲酸的甲醇溶液提取/衍生SMA，并将含有SMA离子衍生产物的提取溶液的微滴直接沉积在MALDI靶中，以通过MALDI-FTICR-MS测量卷烟烟气中的SMA。从而实现了样品前处理和MALDI样品板制备的连续操作。通过与二苯胺反应衍生化SMA，转化为带有季铵基团的稳定席夫碱，SMA分析的灵敏度显着提高。通过在 EDSD 溶剂中添加二苯胺，实现了良好的点内样品均匀性，并获得了令人满意的 MALDI-FTICR-MS 信号重复性（甲醛的 R.S.D.=7.3%，n=5）。这种溶剂和试剂最少化的方法具有自动电位，为烟雾中 SMA 的测定提供了简单、快速且准确的程序。
Extraction and derivatization in single drop (EDSD) coupled to matrix-assisted laser desorption/ionization Fourier transform ion cyclotron resonance mass spectrometry (MALDI-FTICR-MS) was utilized to determine small molecular aldehydes (SMAs) in single puff smoke. A methanol solution of diphenylamine, 2,5-dihydroxybenzoic acid was used for extraction/derivatization of SMAs and a microdrop of the extraction solution containing the ionic derivatization products of SMAs could be directly deposited in the MALDI target to perform the measurement of SMAs in the cigarette smoke on puff level by MALDI-FTICR-MS. As a result, a consecutive operation of sample pre-treating and MALDI sample plate preparation was achieved. SMAs were derivatized by the reaction with diphenylamine and transformed a stable Schiff base bearing a quaternary ammonium group, and the sensitivity of analysis for SMAs was significantly improved. Good sample homogeneity in in-dot was achieved by adding diphenylamine into the solvent for EDSD and a satisfying repeatability (R.S.D.=7.3% for formaldehyde, n=5) of MALDI-FTICR-MS signals was obtained. This solvent- and reagent-minimized approach with an automatic potential provided a simple, rapid, and accurate procedure for the determination of SMAs in smoke.