Purification method of augustum alkaline
A purification method and technology of Augustus base, applied in the fields of organic chemistry, bulk chemical production, etc., can solve the problems of rare Augustus base research reports, etc., and achieve a short preparation cycle, short extraction time and high efficiency. Effect
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Embodiment 1
[0015] Take 1kg of the whole plant of Manjusri orchid Augustus, crush it, add 90% ethanol with pH 9 to infiltrate for 6 hours, add it to the extraction kettle, and use supercritical CO 2 Extraction, adjust the extraction temperature to 40°C, the extraction pressure to 38MPa, CO 2 The flow rate is 38L / h, extract for 3 hours, adjust the temperature of the separation kettle Ⅰ to 35°C, the pressure to 10MPa, the temperature of the separation kettle Ⅱ to 25°C, and the pressure to 6MPa, collect the extract in the separation kettle, dissolve it with 3% hydrochloric acid aqueous solution, and filter , the filtrate was adjusted to pH 9 with ammonia water, the precipitate was collected, carbon tetrachloride, methanol, and water were mixed according to the ratio (18:18:3), the following phase was the stationary phase, the upper phase was the mobile phase, and high-speed countercurrent chromatography was started instrument, adjust the rotating speed to 900r / min, take the dissolved precipi...
Embodiment 2
[0017] Take 1 kg of the whole plant of Manjusri orchid Augustus, crush it, add 99% ethanol with pH 12 to infiltrate for 2 hours, add it to the extraction kettle, and use supercritical CO 2 Extraction, adjust the extraction temperature to 60°C, the extraction pressure to 25MPa, CO 2 The flow rate is 20L / h, extract for 1h, adjust the temperature of the separation kettle Ⅰ to 45°C, the pressure to 18MPa, the temperature of the separation kettle Ⅱ to 35°C, and the pressure to 10MPa, collect the extract in the separation kettle, dissolve it with 3% hydrochloric acid aqueous solution, and filter , the filtrate was adjusted to pH 8 with ammonia water, the precipitate was collected, carbon tetrachloride, methanol, and water were mixed according to the ratio (18:20:2), the following phase was the stationary phase, the upper phase was the mobile phase, and high-speed countercurrent chromatography was started instrument, adjust the rotating speed to 950r / min, take the dissolved precipita...
Embodiment 3
[0019] Take 10kg of the whole plant of Manjusri orchid Augustus, crush it, add 95% ethanol with pH 10 to infiltrate for 4 hours, add it to the extraction kettle, and use supercritical CO 2 Extraction, adjust the extraction temperature to 50°C, the extraction pressure to 35MPa, CO 2 The flow rate is 35L / h, extract for 2 hours, adjust the temperature of the separation kettle Ⅰ to 38°C, the pressure to 15MPa, the temperature of the separation kettle Ⅱ to 28°C, and the pressure to 8MPa, collect the extract in the separation kettle, dissolve it with 3% hydrochloric acid aqueous solution, and filter , the filtrate was adjusted to pH 9 with ammonia water, the precipitate was collected, carbon tetrachloride, methanol, and water were mixed according to the ratio (18:17:2), the lower phase was the stationary phase, the upper phase was the mobile phase, and high-speed countercurrent chromatography was started Instrument, adjust the rotating speed to adjust 850r / min, take the dissolved pr...
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