Christian Doppler Laboratory for Microwave Chemistry (CDLMC) and Institute of Chemistry, Karl-Franzens-University Graz, Heinrichstrasse 28, A-8010 Graz, Austria.
J Chromatogr A. 2010 Jan 1;1217(1):167-70. doi: 10.1016/j.chroma.2009.11.071. Epub 2009 Dec 3.
Parallel microwave-assisted gas chromatography (GC) derivatization protocols utilizing a silicon carbide (SiC)-based microtiter plate platform fitted with screw-capped GC vials were developed. For three selected standard derivatization protocols such as acetylation (exemplified for morphine), pentafluoropropionylation (for 6-monoacetylmorphine) and trimethylsilylation (for Delta(9)-tetrahydrocannabinol) complete derivatization was achieved within 5min at 100 degrees C in a dedicated multimode microwave instrument using online temperature monitoring. Microwave irradiation leads to rapid and homogeneous heating of the strongly microwave-absorbing SiC plate, with minimal deviations in the temperature recorded at different positions of the plate. The current platform allows the simultaneous derivatization of 80 reaction mixtures under strictly controlled temperature conditions. Similar results can also be obtained using a standard hotplate as heating source, although heating to the target temperature of 100 degrees C is slightly slower. The results demonstrate that parallel microwave derivatization procedures can significantly reduce the overall analysis time and increase sample throughput for GC-MS-based analytical methods.
开发了一种基于碳化硅 (SiC) 的微孔板平台的平行微波辅助气相色谱 (GC) 衍生化方案,该平台配备有带螺旋盖的 GC 小瓶。对于三种选定的标准衍生化方案,如乙酰化(以吗啡为例)、五氟丙酰化(用于 6-单乙酰吗啡)和三甲基硅烷化(用于 Delta(9)-四氢大麻酚),在专用的多模微波仪器中,在 100°C 下仅需 5 分钟即可完成衍生化,同时在线监测温度。微波辐射导致强烈吸收微波的 SiC 板快速且均匀地加热,板上不同位置记录的温度偏差最小。当前的平台允许在严格控制温度条件下同时衍生化 80 个反应混合物。使用标准热板作为加热源也可以获得类似的结果,尽管加热到 100°C 的目标温度稍慢。结果表明,平行微波衍生化程序可以显著缩短整体分析时间并增加基于 GC-MS 的分析方法的样品通量。