万寿菊干花中叶黄素的实验室制备

Laboratory-scale Preparation of Lutein from Marigold Dried Flower

用正己烷萃取万寿菊干花粉末多遍至萃取液无色,合并过滤萃取液。负压旋转蒸发浓缩萃取液至其中总类胡萝卜素含量为5%(W/V)。向浓缩液中加入等体积的10%(W/V)氢氧化钾乙醇溶液,在室温条件下,充氮,搅拌,皂化12h。用乙醚和2%(W/V)的氯化钠水溶液液—液萃取皂化反应产物。用氯化钠溶液多次洗涤乙醚相至氯化钠洗液的pH为7。收集乙醚相,负压旋转蒸发除去其中的乙醚,并进一步负压加热干燥除去水分至恒重。测定产物的总类胡萝卜素含量及类胡萝卜素组成。收集色谱图上叶黄素组分的质谱图作为对其定性的依据。

The dried powders of marigold flower were extracted by hexane for a few times until the extract was colorless. After filtration, the extract was collected and concentrated by a rotary evaporator until its total carotenoid amount （TCA） was 5% （W/ V）. The concentrate was saponified by the addition of an equal volume of 10% （W/V） KOH-EtOH. This reaction usually took more than 12 hours at room temperature with stirring and N2 filling. The product of saponification was isolated by a liquid-liquid phase separation with the upper phase of di-ether and the lower phase of 2% （W/V） NaCl solution. The ether phase was washed by the NaCI solution for many time until its pH was 7. The ether phase was then evaporated to remove di-ethcr and water. The TCA and carotenoid composition （CC） assessments of final concentrate were performed, A mass spectroscopy of lutein fraction was undertaken to support its identification by HPLC,