Method for preparing palmatine by producing salting-out waste liquid by means of palmatine
A technology of patellogenin and salting out, applied in the field of preparing patellogenin, can solve problems such as waste of resources, and achieve the effects of low production cost, simple process engineering and high content
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Embodiment 1
[0018] Embodiment 1: Take 10L of the salting-out waste liquid from the production of palmetine, adjust the pH=9.5 with sodium hydroxide with a mass concentration of 40%, and filter; the filtrate passes through the AB-8 resin column with a flow rate of 1 column volume / h, and the filtrate goes After that, wash the resin column with 3 times the column volume of purified water to elute impurities, and then use an ethanol solution with a volume concentration of 60% to elute the alkaloid at a flow rate of 1 column volume per hour, and the eluent is detected by TLC spot plate , collect the alkaloid segment eluate; the alkaloid segment eluate is concentrated to obtain concentrate 20.2g; Minutes, add an equal volume of purified water to the reaction solution, mix well and pass through the AB-8 resin column to absorb, then wash the column with 2 times the column volume of purified water, and then elute the alkaloid with an ethanol solution with a volume concentration of 80%. Collect the...
Embodiment 2
[0019] Example 2: Take 10L of the salting-out waste liquid from the production of palmetine, adjust the pH=9 with sodium hydroxide with a mass concentration of 35%, and filter; the filtrate passes through the D101 resin column with a flow rate of 2 column volumes / h. After the filtrate is finished, , wash the resin column with 4 times the column volume of purified water to elute impurities, and then use an ethanol solution with a volume concentration of 70% to elute the alkaloids at a flow rate of 2 column volumes per hour. The eluent is detected by TLC spot plate, and collected The alkaloid section eluate; the alkaloid section eluent was concentrated to obtain 19.8g of a concentrate; the concentrate was dissolved in 179g of tetrahydrofuran, then 2.97g of DMAP was added, and 29g of methyl iodide was slowly added dropwise. After the addition was completed, continue to stir for 30 minutes. Add an equal volume of purified water to the reaction solution, mix it, and then absorb it t...
Embodiment 3
[0020] Embodiment 3: Get 100L of the salting-out waste liquid produced by palmetine, adjust the pH=10 with 45% sodium hydroxide in mass concentration, and filter; the filtrate passes through the AB-8 resin column, and the flow rate is 1.5 column volumes / h, After that, wash the resin column with 3.5 times the column volume of purified water to elute impurities, and then use an ethanol solution with a volume concentration of 65% to elute the alkaloid at a flow rate of 1.5 column volumes per hour, and the eluent is detected by TLC spot plate , collect the alkaloid segment eluate; the alkaloid segment eluate is concentrated to obtain concentrate 210g; the concentrate is dissolved with 2100g tetrahydrofuran, then 31g DMAP is added, 250g methyl iodide is slowly added dropwise, and after the dropwise addition is completed, continue to stir for 30 minutes. Add an equal volume of purified water to the reaction solution, mix well and pass through the AB-8 resin column for adsorption, the...
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