He P, Ackman R G
Canadian Institute of Fisheries Technology, DalTech, Dalhousie University, Halifax, Nova Scotia, Canada.
J Agric Food Chem. 2000 Aug;48(8):3069-71. doi: 10.1021/jf991193g.
2,6-Dihydro-2,2,4-trimethyl-6-quinolone (QI) and 1,8'-bis(1, 2-dihydro-6-ethoxy-2,2,4-trimethylquinoline) (DM) are two oxidation products of 1,2-dihydro-6-ethoxy-2,2,4-trimethylquinoline (ethoxyquin, EQ). This paper describes several methods for the purification of technical grade EQ and for the production of pure QI and DM as standards with the purity required (>99%) for calibration of quantitative determination methods. EQ of high purity was obtained through vacuum distillation followed by a quick column chromatographic purification on silica gel. Preparative scale purity DM could be obtained through recrystallization from methanol, but QI could be purified only by a high-pressure liquid chromatographic method.
2,6 - 二氢 - 2,2,4 - 三甲基 - 6 - 喹啉酮(QI)和1,8'-双(1,2 - 二氢 - 6 - 乙氧基 - 2,2,4 - 三甲基喹啉)(DM)是1,2 - 二氢 - 6 - 乙氧基 - 2,2,4 - 三甲基喹啉(乙氧喹,EQ)的两种氧化产物。本文描述了几种纯化工业级EQ以及制备纯QI和DM作为标准品的方法,这些标准品的纯度需满足定量测定方法校准所需的要求(>99%)。通过减压蒸馏,然后在硅胶上进行快速柱色谱纯化,可获得高纯度的EQ。制备规模纯度的DM可通过从甲醇中重结晶获得,但QI只能通过高压液相色谱法进行纯化。