废弃烟叶中茄尼醇对照品的制备

Preparation of reference material of solanesol from waste tobacco leaves

建立从废弃烟叶中分离高纯度茄尼醇对照品的方法。首先采用石油醚萃取烟叶,动态皂化法皂化,硅胶柱层析进行粗分。制备型高效液相色谱采用甲醇∶乙醇=60∶40进行精制纯化。通过以上方法所得产物经ESI-MS1、H-NMR和13 C-NMR鉴定结构,高效液相色谱法测得纯度为99.7%,满足对照品的要求。本方法简便快捷,重现性好,所得产物纯度高,适合茄尼醇对照品的制备。

This paper is to establish an approach to separate high-purity reference material of solanesol from tobacoo leaves.We initially obtained crude reference material of solanesol with petroleum ether extraction,dynamic saponification and silica gel chromatography.We then employed preparative high-performance liquid chromatography whose ingredient ratio was 60% methanol and 40% ethanol to refine and purify the acquired crude reference material of solanesol.The purified product whose structure was identified with ESI-MS,IR,1H-NMR and 13C-NMR and whose purity of 99.7% was determined with HPLC satisfied the requirement of reference material.Such an approach is simple,rapid and reproductive and its product has quite high purity so it is suitable for the preparation of reference material of solanesol.