CN102626430A - Method for preparing total alkaloid from daphniphyllum calycinum - Google Patents

Method for preparing total alkaloid from daphniphyllum calycinum Download PDF

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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
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China
Prior art keywords
daphniphyllum calycinum
temperature
extract
total alkaloids
filtering
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Pending
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CN201210115083XA
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Chinese (zh)
Inventor
刘东锋
杨成东
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Nanjing Zelang Medical Technology Co Ltd
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Nanjing Zelang Medical Technology Co Ltd
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Priority to CN201210115083XA priority Critical patent/CN102626430A/en
Publication of CN102626430A publication Critical patent/CN102626430A/en
Pending legal-status Critical Current

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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

A kind of method that from Daphniphyllum calycinum, prepares total alkaloids
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.
CN201210115083XA 2012-04-19 2012-04-19 Method for preparing total alkaloid from daphniphyllum calycinum Pending CN102626430A (en)

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Application Number Priority Date Filing Date Title
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Cited By (5)

* Cited by examiner, † Cited by third party
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

Cited By (6)

* Cited by examiner, † Cited by third party
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