Faculty of Chemistry, Warsaw University, Warsaw, Poland.
J Chromatogr A. 2011 Oct 14;1218(41):7264-74. doi: 10.1016/j.chroma.2011.08.061. Epub 2011 Aug 25.
A novel three-step analytical method was developed which enables the simultaneous detection and identification of multifunctional oxygenated products resulting from the reaction of α-pinene with ozone. The method consists of the following steps: conversion of carbonyl groups to methyloximes using methyloxyamine, conversion of carboxylic acids to methyl esters using trimethylsilyldiazomethane (TMSD), and conversion of alcohols to trimethylsilyl ethers using N,O-bis(trimethylsilyl)-trifluoroacetamide (BSTFA). The derivatization procedure at each stage was optimized yielding the appropriate amount of derivatization reagent, reaction temperature and time. The newly developed analytical procedure manages without processes of extraction and evaporation to dryness at any stage. Total time for sample analysis is short ca. 3h. The characteristic ions of derivatives and common pattern for ion fragmentation in capillary gas chromatography electron impact mass spectrometry (GC-EI-MS) analysis were elucidated and discussed.
开发了一种新颖的三步分析方法,可同时检测和鉴定α-蒎烯与臭氧反应生成的多功能含氧产物。该方法包括以下步骤:使用甲氧基羟胺将羰基转化为甲肟,使用三甲基硅基重氮甲烷(TMSD)将羧酸转化为甲酯,以及使用 N,O-双(三甲基硅基)-三氟乙酰胺(BSTFA)将醇转化为三甲基硅基醚。在每个阶段,优化了衍生化程序,以获得适当量的衍生化试剂、反应温度和时间。新开发的分析程序在任何阶段都无需进行提取和蒸发至干的过程。样品分析的总时间较短,约 3 小时。阐明并讨论了衍生物的特征离子和在毛细管气相色谱电子轰击质谱(GC-EI-MS)分析中离子碎裂的常见模式。