CN102626430A - Method for preparing total alkaloid from daphniphyllum calycinum - Google Patents
Method for preparing total alkaloid from daphniphyllum calycinum Download PDFInfo
- Publication number
- CN102626430A CN102626430A CN201210115083XA CN201210115083A CN102626430A CN 102626430 A CN102626430 A CN 102626430A CN 201210115083X A CN201210115083X A CN 201210115083XA CN 201210115083 A CN201210115083 A CN 201210115083A CN 102626430 A CN102626430 A CN 102626430A
- Authority
- CN
- China
- Prior art keywords
- daphniphyllum calycinum
- temperature
- extract
- total alkaloids
- filtering
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 241001065375 Daphniphyllum calycinum Species 0.000 title claims abstract description 17
- 229930013930 alkaloids Natural products 0.000 title claims abstract description 16
- 150000003797 alkaloid derivatives Chemical class 0.000 title abstract 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound data:image/svg+xml;base64,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 data:image/svg+xml;base64,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 CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000011347 resin Substances 0.000 claims abstract description 16
- 229920005989 resin Polymers 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances data:image/svg+xml;base64,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 data:image/svg+xml;base64,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 O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 8
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- 238000001035 drying Methods 0.000 claims abstract description 3
- 239000002994 raw material Substances 0.000 claims abstract description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Chemical compound 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- 238000000194 supercritical-fluid extraction Methods 0.000 claims description 5
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- 235000008733 Citrus aurantifolia Nutrition 0.000 abstract description 2
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- 208000005392 Spasm Diseases 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound 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OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
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- 230000001476 alcoholic Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000003110 anti-inflammatory Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002481 ethanol extraction Methods 0.000 description 1
- 238000003810 ethyl acetate extraction Methods 0.000 description 1
- 241000411851 herbal medicine Species 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 238000003808 methanol extraction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000000552 rheumatic Effects 0.000 description 1
- 230000028327 secretion Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 230000002522 swelling Effects 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
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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
The present invention relates to a kind of method that from Daphniphyllum calycinum, prepares total alkaloids, particularly relate to a kind of method of utilizing supercritical CO 2 extraction and macroporous resin method from Daphniphyllum calycinum, to prepare total alkaloids.
Background technology
Daphniphyllum calycinum is tiger ear, southern mountain range Folium seu Semen Daphniphylli oldhami again; South of the Five Ridges Folium seu Semen Daphniphylli oldhami, false Lignum nanmu, the ears of an ox or cow bell, pig chin wood are Daphniphyllaceae Folium seu Semen Daphniphylli oldhami platymiscium, main product in Jiangxi, ground such as Guangdong, Guangxi, Fujian, Hainan, Yunnan; Be born under the mountain area sparse woods of height above sea level 100-700m, in the shrubbery or the small stream limes marginis; For area, Guangdong Chinese herbal medicine commonly used, wind-expelling pain-stopping is arranged, the effect of removing toxic substances and promoting subsidence of swelling.Length is used to treat diseases such as rheumatic ostalgia, sore swollen toxin, injury and bone fracture, venom.Modern medicine study finds that contain large number of biological alkali in the Daphniphyllum calycinum medical material, not only nerve toxicity can also significantly suppress enterokinesia, relieving spasm to stop pain, and antiinflammatory can also the gastric acid inhibitory secretion.The research latest find has anti-acetylcholinesterase activity, and senile dementia is had effect.
The alkaloidal method research of preparation is more from Daphniphyllum calycinum, employing ethanol or methanol extraction, after the extracting solution acidify again through organic reagent multitple extraction or ion exchange resin adsorption and purification.The method that is adopted like document " Chinese medicine Daphniphyllum calycinum alkaloids chemical constituent and activity research " is 95% alcohol reflux, and concentrated solution is regulated pH4, ethyl acetate extraction impurity, and re-adjustment pH10, chloroform extraction gets total alkaloids.
As stated, the existing method that from Daphniphyllum calycinum, prepares total alkaloids has been used more organic reagent, and efficient is lower, and waste liquid produces more, and contaminated environment is not suitable for commercial production.
Summary of the invention
The objective of the invention is to solve the deficiency and the defective of prior art, a kind of method that from Daphniphyllum calycinum, prepares total alkaloids is provided, this method is efficient, quick, can also reduce pollution.
The objective of the invention is to realize through following technical scheme:
Get the Daphniphyllum calycinum raw material pulverizing,, drop into supercritical extraction reactor, feed liquid CO 2 and entrainer with an amount of saturated limewater alkalization 2-3 hour; Under pressure 15-35MPa, temperature 40-50 ℃ condition, extracted 1-3 hour, under pressure 5-10MPa, temperature 40-60 ℃ condition, resolve extract, the gained extract reclaims reagent; Add the appropriate amount of acid water dissolution, filter to add in the macroporous resin and adsorb, the washed resin post is collected water lotion and lower column liquid; Regulate neutrality, concentrating under reduced pressure becomes extractum, uses 80% dissolve with ethanol solution; Filter, be concentrated into the small size crystallization, leach crystal and be drying to obtain.
The optional ethanol of described entrainer, methanol or acetone soln, consumption are that the 1-3 of material quantity doubly measures.
The optional ADS-21 of described macroporous resin model, NKA-9, HPD-600 or AB-8.
Advantage of the present invention is:
1. adopt the supercritical CO 2 extraction, extraction ratio is high, and is pollution-free, and the cycle is short;
2. adopt the macroporous resin remove impurity, easy and simple to handle, efficient is high.
The specific embodiment
To combine the specific embodiment to further specify the present invention below.
Embodiment 1:
Ramulus et Folium Daphniphylli calycini is pulverized 80 orders, gets 2kg and adds 1L saturated limewater alkalization 3 hours, drops into supercritical extraction reactor, and 40 ℃ of extracting pressure 15MPa, temperature are set; Feed liquid CO 2 with flow velocity 20kg/h, reach above-mentioned parameter after, feed 70% alcoholic solution with flow velocity 2kg/h and do entrainer, dynamic extraction 3 hours; Under pressure 7MPa, 60 ℃ of conditions of temperature, resolve extract, the gained extract reclaims reagent, with 1L1% hydrochloric acid water dissolution, filters; Add in the ADS-21 macroporous resin and adsorb, with 2L washed resin post, collect water lotion and lower column liquid, sodium hydroxide solution is regulated neutral; Concentrating under reduced pressure becomes extractum, uses 80% dissolve with ethanol solution, filters, and is concentrated into 1/4 volume; Crystallization leaches the crystal vacuum drying, gets total alkaloids, content detection 97.3%.
Embodiment 2:
Ramulus et Folium Daphniphylli calycini is pulverized 60 orders, gets 2kg and adds 1L saturated limewater alkalization 3 hours, drops into supercritical extraction reactor, and 50 ℃ of extracting pressure 30MPa, temperature are set; Feed liquid CO 2 with flow velocity 22kg/h, reach above-mentioned parameter after, feed 80% methanol solution with flow velocity 3kg/h and do entrainer, dynamic extraction 2 hours; Under pressure 6MPa, 50 ℃ of conditions of temperature, resolve extract, the gained extract reclaims reagent, with 1L0.5% sulphuric acid water dissolution, filters; Add in the NKA-9 macroporous resin and adsorb, with 3L washed resin post, collect water lotion and lower column liquid, sodium hydroxide solution is regulated neutral; Concentrating under reduced pressure becomes extractum, uses 80% dissolve with ethanol solution, filters, and is concentrated into 1/6 volume; Crystallization leaches the crystal vacuum drying, gets total alkaloids, content detection 95.4%.
Embodiment 3:
Ramulus et Folium Daphniphylli calycini is pulverized 20 orders, gets 2kg and adds 1L saturated limewater alkalization 2 hours, drops into supercritical extraction reactor, and 45 ℃ of extracting pressure 20MPa, temperature are set; Feed liquid CO 2 with flow velocity 20kg/h, reach above-mentioned parameter after, feed 70% acetone soln with flow velocity 1kg/h and do entrainer, dynamic extraction 3 hours; Under pressure 7MPa, 50 ℃ of conditions of temperature, resolve extract, the gained extract reclaims reagent, with 1L1% hydrochloric acid water dissolution, filters; Add in the AB-8 macroporous resin and adsorb, with 1.5L washed resin post, collect water lotion and lower column liquid, sodium hydroxide solution is regulated neutral; Concentrating under reduced pressure becomes extractum, uses 80% dissolve with ethanol solution, filters, and is concentrated into 1/8 volume; Crystallization leaches the crystal vacuum drying, gets total alkaloids, content detection 93.5%.
Claims (3)
1. a method that from Daphniphyllum calycinum, prepares total alkaloids is characterized in that: get the Daphniphyllum calycinum raw material pulverizing, with an amount of saturated limewater alkalization 2-3 hour, drop into supercritical extraction reactor; Feed liquid CO 2 and entrainer, under pressure 15-35MPa, temperature 40-50 ℃ condition, extracted 1-3 hour, under pressure 5-10MPa, temperature 40-60 ℃ condition, resolve extract; The gained extract reclaims reagent, adds the appropriate amount of acid water dissolution, filters to add in the macroporous resin to adsorb the washed resin post; Collect water lotion and lower column liquid, regulate neutrality, concentrating under reduced pressure becomes extractum, uses 80% dissolve with ethanol solution; Filter, be concentrated into the small size crystallization, leach crystal and be drying to obtain.
2. the method that from Daphniphyllum calycinum, prepares total alkaloids according to claim 1 is characterized in that the optional ethanol of described entrainer, methanol or acetone soln, and consumption is that the 1-3 of material quantity doubly measures.
3. the method that from Daphniphyllum calycinum, prepares total alkaloids according to claim 1 is characterized in that the optional ADS-21 of described macroporous resin model, NKA-9, HPD-600 or AB-8.
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| CN201210115083XA CN102626430A (en) | 2012-04-19 | 2012-04-19 | Method for preparing total alkaloid from daphniphyllum calycinum |
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| CN201210115083XA CN102626430A (en) | 2012-04-19 | 2012-04-19 | Method for preparing total alkaloid from daphniphyllum calycinum |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104887663A (en) * | 2015-05-12 | 2015-09-09 | 南京广康协生物医药技术有限公司 | Application of daphmalenine A ramification to preparing anti-inflammatory drugs |
| CN104906092A (en) * | 2015-05-27 | 2015-09-16 | 南京广康协生物医药技术有限公司 | Application of O-(diethylin)ethyl derivative of Daphmalenine A in preparing liver injury prevention and treatment drugs |
| CN104922119A (en) * | 2015-05-27 | 2015-09-23 | 南京广康协生物医药技术有限公司 | Application of O-(diethylin) ethyl derivative of Daphmalenine A to preparation of antiviral drug |
| CN106176829A (en) * | 2016-08-19 | 2016-12-07 | 集安森源食用菌发展有限公司 | The extracting method of Lentinus Edodes total alkaloids |
| CN113367242A (en) * | 2021-06-10 | 2021-09-10 | 中国农业科学院草原研究所 | Method for extracting alkaloid from nettle and application of alkaloid as growth promoting additive |
-
2012
- 2012-04-19 CN CN201210115083XA patent/CN102626430A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104887663A (en) * | 2015-05-12 | 2015-09-09 | 南京广康协生物医药技术有限公司 | Application of daphmalenine A ramification to preparing anti-inflammatory drugs |
| CN104906092A (en) * | 2015-05-27 | 2015-09-16 | 南京广康协生物医药技术有限公司 | Application of O-(diethylin)ethyl derivative of Daphmalenine A in preparing liver injury prevention and treatment drugs |
| CN104922119A (en) * | 2015-05-27 | 2015-09-23 | 南京广康协生物医药技术有限公司 | Application of O-(diethylin) ethyl derivative of Daphmalenine A to preparation of antiviral drug |
| CN106176829A (en) * | 2016-08-19 | 2016-12-07 | 集安森源食用菌发展有限公司 | The extracting method of Lentinus Edodes total alkaloids |
| CN106176829B (en) * | 2016-08-19 | 2019-10-29 | 集安森源食用菌发展有限公司 | The extracting method of mushroom total alkaloid |
| CN113367242A (en) * | 2021-06-10 | 2021-09-10 | 中国农业科学院草原研究所 | Method for extracting alkaloid from nettle and application of alkaloid as growth promoting additive |
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Application publication date: 20120808 |