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Method for preparing total alkaloid from daphniphyllum calycinum

A technology of total alkaloids and Niuerfeng, applied in the directions of drug combination, pharmaceutical formula, plant raw materials, etc., can solve the problems of unsuitability for industrial production, excessive waste liquid generation, environmental pollution, etc., and achieves short cycle, easy operation, and extraction rate. high effect

Inactive Publication Date: 2012-08-08
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] As mentioned above, the existing method for preparing total alkaloids from the eucalyptus uses more organic reagents, has low efficiency, produces more waste liquid, pollutes the environment, and is not suitable for industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Grind the branches and leaves of maple japonica to 80 meshes, take 2kg and add 1L saturated lime water to alkalinize for 3 hours, put it into a supercritical extraction kettle, set the extraction pressure to 15MPa, the temperature to 40°C, and flow in liquid CO2 at a flow rate of 20kg / h. After reaching the above parameters, use Flow rate of 2kg / h into 70% ethanol solution as entrainer, dynamic extraction for 3 hours, analyze the extract under the conditions of pressure 7MPa and temperature 60°C, the obtained extract was recovered reagent, dissolved in 1L of 1% hydrochloric acid water, filtered, added ADS- Adsorb in 21 macroporous resin, wash the resin column with 2L water, collect the washing liquid and the next column liquid, adjust the neutrality with sodium hydroxide solution, concentrate under reduced pressure to obtain an extract, dissolve with 80% ethanol solution, filter, and concentrate to 1 / 4 Volume, crystallization, and vacuum drying of the filtered crystals to...

Embodiment 2

[0017] Crush the branches and leaves of maple japonica to 60 meshes, take 2kg and add 1L saturated lime water to alkalinize for 3 hours, put it into a supercritical extraction kettle, set the extraction pressure to 30MPa, the temperature to 50°C, and flow in liquid CO2 at a flow rate of 22kg / h. After reaching the above parameters, use Flow rate 3kg / h into 80% methanol solution as entrainer, dynamic extraction for 2 hours, analyze the extract under the conditions of pressure 6MPa and temperature 50°C, the obtained extract was recovered as reagent, dissolved in 1L of 0.5% sulfuric acid water, filtered, added Adsorb in NKA-9 macroporous resin, wash the resin column with 3L water, collect the washing liquid and the next column liquid, adjust the neutrality with sodium hydroxide solution, concentrate under reduced pressure to obtain an extract, dissolve with 80% ethanol solution, filter, and concentrate to 1 / 6 volume, crystallized, and the crystals were filtered out and vacuum-drie...

Embodiment 3

[0019] Crush the branches and leaves of maple eucalyptus to 20 meshes, take 2kg and add 1L of saturated lime water to alkalinize for 2 hours, put it into a supercritical extraction kettle, set the extraction pressure to 20MPa, the temperature to 45°C, and flow in liquid CO2 at a flow rate of 20kg / h. After reaching the above parameters, use Flow rate 1kg / h into 70% acetone solution as entrainer, dynamic extraction for 3 hours, analyze the extract under the conditions of pressure 7MPa and temperature 50℃, the obtained extract was recovered reagent, dissolved in 1L 1% hydrochloric acid water, filtered, added AB- 8. Adsorb in macroporous resin, wash the resin column with 1.5L water, collect the washing liquid and the next column liquid, adjust the neutrality with sodium hydroxide solution, concentrate under reduced pressure to obtain an extract, dissolve with 80% ethanol solution, filter, and concentrate to 1 / 2 8 volumes, crystallized, and the crystals were filtered out and vacuum-...

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PUM

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Abstract

The invention discloses a method for preparing a total alkaloid from daphniphyllum calycinum. The method comprises the following steps of: smashing daphniphyllum calycinum serving as a raw material; alkalifying by using an appropriate amount of saturated lime water for 2-3 hours, putting into a supercritical extracting kettle, introducing liquid CO2 and an entrainer, extracting under the pressure of 15-35MPa and at the temperature of 40-50 DEG C for 1-3 hours; resolving an extract under the pressure of 5-10MPa and at the temperature of 40-60 DEG C; recovering a reagent from the extract; adding an appropriate amount of acid water for dissolving; filtering, and adding into macroporous resin for adsorbing; washing a resin column with water; collecting a water washing liquid and a lower column liquid; adjusting to neutral; concentrating into an extract under reduced pressure; dissolving with a 80 percent ethanol; filtering; concentrating to a small volume, and crystallizing; and filtering a crystal out, and drying to obtain the total alkaloid. The method has the advantages of high efficiency, short period, low pollution and high yield, and is suitable for industrial production.

Description

technical field [0001] The present invention relates to a method for preparing total alkaloids from eucalyptus, in particular to a method for preparing total alkaloids from eucalyptus by means of supercritical CO2 extraction and macroporous resin. Background technique [0002] Niu'er maple is also called tiger's ear, Nanling tiger's skin Nan, Lingnan tiger's skin, false nanmu, cow's ear bell, and pig's jaw. It is a plant of the tiger's skin family. It is mainly produced in Jiangxi, Guangdong, Guangxi, Fujian, In Hainan, Yunnan and other places, it grows under sparse forests, bushes or beside streams and ditches in mountainous areas at an altitude of 100-700m. It is a commonly used Chinese herbal medicine in Guangdong. It has the effects of dispelling wind, relieving pain, detoxifying and reducing swelling. It is long used to treat rheumatic bone pain, sores, swollen toxins, fractures from bruises, snake bites and other diseases. Modern medical research has found that the he...

Claims

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Application Information

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IPC IPC(8): A61K36/185A61P29/00A61P1/12A61P1/04A61P25/28
Inventor 刘东锋杨成东
Owner NANJING ZELANG MEDICAL TECH
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