Zurek G, Karst U
Westfälische Wilhelms-Universität Münster, Anorganisch-Chemisches Institut, Abteilung Analytische Chemie, Germany.
J Chromatogr A. 1999 Dec 24;864(2):191-7. doi: 10.1016/s0021-9673(99)01041-9.
A liquid chromatography-mass spectrometry method for the determination of aliphatic aldehydes after derivatization with acetylacetone or dimedone by means of the Hantzsch reaction is presented. Two molecules of a beta-diketone, one molecule of ammonia and an aliphatic aldehyde cyclisate under formation of colored and fluorescent reaction products. Atmospheric pressure chemical ionization (APCI) and electrospray ionization (ESI) in the positive mode are suitable to ionize the formed dihydropyridine and decahydroacridine derivatives under protonation of their basic secondary amine functionality. The method has been used to identify the oxidation product of the formaldehyde derivatives as side product. The acetaldehyde derivative, presumably formed in the reaction of residual acetaldehyde in the acetic acid or acetate reagents, is mainly responsible for the increasing fluorescence background of the reagent solutions.
本文介绍了一种液相色谱-质谱法，用于通过乙酰丙酮或二甲基乙二酮经汉茨希反应衍生化后测定脂肪醛。两分子的β-二酮、一分子的氨与脂肪醛发生环化反应，生成有色和荧光反应产物。正模式下的大气压化学电离（APCI）和电喷雾电离（ESI）适用于在其碱性仲胺官能团质子化的情况下，使形成的二氢吡啶和十氢吖啶衍生物离子化。该方法已用于鉴定甲醛衍生物的氧化产物作为副产物。乙醛衍生物可能是在乙酸或乙酸盐试剂中残留乙醛的反应中形成的，它是试剂溶液荧光背景增加的主要原因。
