Method for purifying sesamin and sesamolin
A technology of sesamolin and purification method, which is applied in the direction of anti-toxins, digestive system, metabolic diseases, etc., can solve problems such as complex, unsuitable for industrial application, single active ingredient or purification method, etc., and achieve strong process stability and simple operation Effect
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Embodiment 1
[0021] Take 100g of sesame oil extracted with petroleum ether, add 500mL of methanol, reflux and extract at 90°C for 20min, after cooling to room temperature, freeze at -30°C for 8h, triglycerides solidify, and suction filter at -20°C to obtain lignans The extract of the mixture of compounds was removed from methanol under reduced pressure to obtain a light yellow paste.
[0022] Add 20mL of ethanol solution of potassium hydroxide with a mass concentration of 5% to the paste, saponify at 90°C for 10min, add 100mL of water after cooling and transfer to a 500mL separatory funnel, extract with ether, wash with water, anhydrous sodium sulfate Drying, suction filtration and removal of the solvent under reduced pressure yielded a light yellow semi-solid paste.
[0023] Add 20mL of diethyl ether to the light yellow semi-solid paste, shake it fully, seal it and place it at 5°C for 6h, a white powdery sesamin solid is precipitated, and the filtrate and white powdery solid are obtained ...
Embodiment 2
[0025] Take 200mL of commercially available roasted sesame oil, add it to an alumina column (40cm×4cm i.d., 150g of alumina), and elute with petroleum ether, use 2mL of the eluent to add 1mL of concentrated hydrochloric acid containing 2% (wt%) sucrose to heat The reaction was monitored for 5 minutes, and the eluent was replaced with ethyl acetate for elution when a reddish color appeared in the reaction until no color reaction occurred. Ethyl acetate eluate was evaporated under reduced pressure to obtain a yellow semi-solid paste.
[0026] The paste is crystallized and recrystallized successively with ether, chloroform, petroleum ether, ethanol, etc. to obtain 0.68 g and 0.33 g of sesamin and sesamolin with a purity of more than 95 percent, respectively. The ether used was 25mL, the chloroform was 4mL, the ethanol used for the recrystallization of sesamin and sesamolin was 10mL and 6mL respectively, and others were the same as in Example 1.
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