CN102309576A - Preparation method of uncaria total alkaloids - Google Patents
Preparation method of uncaria total alkaloids Download PDFInfo
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- CN102309576A CN102309576A CN201110186246A CN201110186246A CN102309576A CN 102309576 A CN102309576 A CN 102309576A CN 201110186246 A CN201110186246 A CN 201110186246A CN 201110186246 A CN201110186246 A CN 201110186246A CN 102309576 A CN102309576 A CN 102309576A
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- total alkaloids
- ramulus uncariae
- cum uncis
- uncariae cum
- membrane
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Abstract
The invention relates to a preparation method of an uncaria total alkaloids. The method comprises the following steps: crushing a medicinal material of uncaria; dipping with acid dip; extracting; filtering an extract; and adding into an ultrafiltration membrane system for ultrafiltration; adding a permeate into a macroporous resin column; collecting a lower column liquid and concentrating by a nanofiltration membrane system; adjusting a pH of a concentrated solution to 9-10 with ammonia; extracting by chloroform; recovering a reagent from the extract; and drying. The method employs a membrane filtration technology to reduce pollution and realize cyclic utilization of acid water in a production process, has a low energy consumption and is suitable for industrialized production.
Description
Technical field
The present invention relates to a kind of method for preparing of Ramulus Uncariae Cum Uncis total alkaloids, particularly relate to a kind of method of utilizing membrane separation technique to prepare the Ramulus Uncariae Cum Uncis total alkaloids.
Background technology
Ramulus Uncariae Cum Uncis is the Maguireothamnus speciosus Ramulus Uncariae Cum Uncis
Uncaria rhynchophylla(Miq.) Jacks., Ramulus Uncariae macrophyllae
Uncaria macrophyllaWall., Ramulus Uncariae Cum Uncis
Uncaria hirsutaHavil., Uncaria sinensis (Oliv.) Havil.
Uncaria sinensis(Oliv.) Havil. or stockless fruit Ramulus Uncariae Cum Uncis
Uncaria sessilifructusRoxb. dry stem and branch with belt hook.Traditional medicine thinks that the Ramulus Uncariae Cum Uncis nature and flavor are sweet, cool.Return liver, pericardium channel, have the heat clearing away suppressing the hyperactive liver, the effect of dispelling wind and relieving convulsion.Be usually used in that treatment headache is dizzy, dysphoric cold, infantile convulsion tic, pregnant eclamposia, hypertension etc.Modern study shows, contains a large amount of isorhynchophyllines in the Ramulus Uncariae Cum Uncis, and alkaloids such as Ramulus Uncariae cum Uncis alkali have spasmolytic, blood pressure lowering, analgesic effect.
Existing from Ramulus Uncariae Cum Uncis the alkaloidal method of preparation more, chloroform extraction method and resin column method are arranged.Liang Yong etc. think that Ramulus Uncariae Cum Uncis alkaloid ethanol extraction, strong acidic ion resin extract, separating total alkaloids is a kind of economical and convenient, the higher method of efficient.Huang Yonglin etc. think D-101 macroporous adsorbent resin extraction separation Ramulus Uncariae macrophyllae total alkaloids well, and technology stability test products content reaches 36.7%.The patent method of separating total alkaloids " a kind of from Chinese medicine Ramulus Uncariae Cum Uncis extracting solution ", the method for this Patent publish is a hook taking rattan extracting solution, adjustment pH value 1 to 7; Filter, get filtrating and be added on the cation exchange resin column, earlier with the water elution remove impurity; Reuse 0.5%～15% acid solution eluting till the inspection inanimate object alkali, is collected eluent; Add the alkali neutralization, through desalting processing, concentrate drying gets the Ramulus Uncariae Cum Uncis total alkaloids.The method that patent " a kind of method and purposes of from Ramulus Uncariae Cum Uncis leaf, stem and branch with belt hook or herb, extracting alkaloid valid target " discloses is in Ramulus Uncariae Cum Uncis leaf, stem and branch with belt hook or herb, to add aqueous alcohol solutions merceration, percolation or hot reflux to extract, and filters, and reclaim under reduced pressure is to there not being the alcohol flavor; Add entry or alcoholic solution in the concentrated extracting solution, filter, filtrating is through being filled with the adsorption column of adsorbing material; It is colourless selecting washing adsorption column to effluent before the eluting for use; With containing 20～75% alcoholic solution eluting, collect eluent, decompression and solvent recovery; Get thick paste, get alkaloid valid target after the drying.
As stated, the following problem of the existing preparation alkaloidal method of Ramulus Uncariae Cum Uncis:
1. resin column separates, and produces more waste water, and especially ion exchange resin separates, and is unfavorable for environmental protection, does not meet current expanding economy requirement.
2. extraction uses toxic and volatile reagent such as a large amount of chloroforms, and is volatile, and operator are endangered seriously, also has potential safety hazard.
Summary of the invention
The objective of the invention is provides a kind of method for preparing of Ramulus Uncariae Cum Uncis total alkaloids in order to overcome the deficiency of prior art, and method both can reduce the generation of waste liquid, can reduce the consumption of organic reagent again.
Technical solution of the present invention is following: a kind of method for preparing of Ramulus Uncariae Cum Uncis total alkaloids is characterized in that: hook taking rattan pulverizing medicinal materials, sour water soaking and extracting; Behind the extracting liquid filtering, add the ultrafiltration membrane system ultrafiltration, permeate adds macroporous resin column; Collect lower column liquid reuse NF membrane system and concentrate, concentrated solution ammonia is regulated pH9-10, chloroform extraction; Extract reclaims reagent, is drying to obtain.
Described ultrafilter membrane is that molecular cut off is the hollow NF membrane of 3000-10000.A kind of in the optional Fypro of material, polyether sulfone, the politef.
Optional polarity of described macroporous resin or non-polar macroporous resin.
Described NF membrane is the hollow NF membrane of molecular cut off 100-200, a kind of in the optional Fypro of material, polyether sulfone, politef or the composite.
Described ultrafiltration, nanofiltration are all carried out at normal temperatures.
The sour water that adopts in the method can select sulphuric acid or the aqueous hydrochloric acid solution of pH1-2, soak time 6-12 hour, soaks 2-3 time.
Advantage of the present invention is: method adopts membrane separation technique, belongs to physical method, does not use reagent, and the water reusable edible that nanofiltration simultaneously produces reduces the generation of waste liquid; Process using membrance separation and macroporous resin combine, and have remedied the undesirable and more defective of macroporous resin generation waste liquid of the inhomogeneous impurity-eliminating effect of membrane aperture of membrance separation; Whole technology behaviour is simple, has realized low pollution and low energy consumption.
To combine the specific embodiment to further specify the present invention below, but the scope that the present invention requires to protect is not limited to following embodiment.
The specific embodiment:
Embodiment 1
The Ramulus Uncariae Cum Uncis pulverizing medicinal materials becomes granule, gets the hydrochloric acid water loggings bubble 6 hours that 10kg adds 6 times of amount pH1, extracts 3 times; Behind the extracting liquid filtering, add the hollow amilan ultrafiltration membrane system ultrafiltration of molecular cut off 3000, permeate adds D101 non-polar macroporous resin post; Collect lower column liquid, suitable quantity of water eluant solution resin column, the hollow Fypro NF membrane system that merges liquid adding molecular cut off 200 concentrates; Concentrated solution ammonia is regulated pH10, chloroform extraction 3 times, and extract reclaims reagent; Drying obtains total alkaloids 105g, content 84.6%.
Embodiment 2
The Ramulus Uncariae Cum Uncis pulverizing medicinal materials becomes granule, gets the sulphuric acid water loggings bubble 8 hours that 10kg adds 10 times of amount pH2, extracts 2 times; Behind the extracting liquid filtering, add the hollow poly (ether-sulfone) ultrafiltration membrane system ultrafiltration of molecular cut off 10000, permeate adds the polar macroporous resin column of NKA-9; Collect lower column liquid, suitable quantity of water eluant solution resin column, the hollow polyether sulfone filtering film system that merges liquid adding molecular cut off 100 concentrates; Concentrated solution ammonia is regulated pH9, chloroform extraction 4 times, and extract reclaims reagent; Drying obtains total alkaloids 112g, content 81.3 %.
Embodiment 3
The Ramulus Uncariae Cum Uncis pulverizing medicinal materials becomes granule, gets the sulphuric acid water loggings bubble 8 hours that 10kg adds 10 times of amount pH2, extracts 2 times; Behind the extracting liquid filtering, add the hollow politef ultrafiltration membrane system ultrafiltration of molecular cut off 3000, permeate adds AB-8 low pole macroporous resin column; Collect lower column liquid, suitable quantity of water eluant solution resin column, the hollow politef NF membrane system that merges liquid adding molecular cut off 200 concentrates; Concentrated solution ammonia is regulated pH10, chloroform extraction 3 times, and extract reclaims reagent; Drying obtains total alkaloids 131g, content 84.3%.
Embodiment 4
The Ramulus Uncariae Cum Uncis pulverizing medicinal materials becomes granule, gets the hydrochloric acid water loggings bubble 8 hours that 100kg adds 10 times of amount pH2, extracts 2 times; Behind the extracting liquid filtering, add the hollow politef ultrafiltration membrane system ultrafiltration of molecular cut off 3000, permeate adds X-5 low pole macroporous resin column; Collect lower column liquid, suitable quantity of water eluant solution resin column, the hollow politef NF membrane system that merges liquid adding molecular cut off 200 concentrates; Concentrated solution ammonia is regulated pH10, chloroform extraction 3 times, and extract reclaims reagent; Drying obtains total alkaloids 1253g, content 83.8%.
Claims (5)
1. the method for preparing of a Ramulus Uncariae Cum Uncis total alkaloids is characterized in that: hook taking rattan pulverizing medicinal materials, sour water soaking and extracting; Behind the extracting liquid filtering, add the ultrafiltration membrane system ultrafiltration, permeate adds macroporous resin column; Collect lower column liquid reuse NF membrane system and concentrate, concentrated solution ammonia is regulated pH9-10, chloroform extraction; Extract reclaims reagent, is drying to obtain.
2. according to the method for preparing of the said Ramulus Uncariae Cum Uncis total alkaloids of claim 1, it is characterized in that described ultrafilter membrane is that molecular cut off is the hollow NF membrane of 3000-10000, a kind of in the optional Fypro of material, polyether sulfone, the politef.
3. according to the method for preparing of the said Ramulus Uncariae Cum Uncis total alkaloids of claim 1, it is characterized in that optional polarity of described macroporous resin or non-polar macroporous resin.
4. according to the method for preparing of the said Ramulus Uncariae Cum Uncis total alkaloids of claim 1, it is characterized in that described NF membrane is the hollow NF membrane of molecular cut off 100-200, a kind of in the optional Fypro of material, polyether sulfone, politef or the composite.
5. according to the method for preparing of the said Ramulus Uncariae Cum Uncis total alkaloids of claim 1, it is characterized in that described ultrafiltration, nanofiltration all carry out at normal temperatures.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110186246A CN102309576A (en) | 2011-07-05 | 2011-07-05 | Preparation method of uncaria total alkaloids |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110186246A CN102309576A (en) | 2011-07-05 | 2011-07-05 | Preparation method of uncaria total alkaloids |
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| CN102309576A true CN102309576A (en) | 2012-01-11 |
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| CN201110186246A Pending CN102309576A (en) | 2011-07-05 | 2011-07-05 | Preparation method of uncaria total alkaloids |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110003197A (en) * | 2019-04-23 | 2019-07-12 | 南京久安源环保科技有限公司 | A kind of extraction process of tropane alkaloids |
| CN113149857A (en) * | 2021-05-10 | 2021-07-23 | 山东中医药大学 | Amide compound and preparation method and application thereof |
| CN113975322A (en) * | 2020-07-27 | 2022-01-28 | 北京大学 | Uncaria rhynchophylla total alkaloids and extraction and purification method and application thereof |
| CN116854690A (en) * | 2023-06-28 | 2023-10-10 | 河南中医药大学 | Indole uncaria alkaloid substance extraction method and application thereof |
-
2011
- 2011-07-05 CN CN201110186246A patent/CN102309576A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110003197A (en) * | 2019-04-23 | 2019-07-12 | 南京久安源环保科技有限公司 | A kind of extraction process of tropane alkaloids |
| CN110003197B (en) * | 2019-04-23 | 2021-08-06 | 南京久安源环保科技有限公司 | Extraction process of tropane alkaloids |
| CN113975322A (en) * | 2020-07-27 | 2022-01-28 | 北京大学 | Uncaria rhynchophylla total alkaloids and extraction and purification method and application thereof |
| CN113975322B (en) * | 2020-07-27 | 2022-08-30 | 北京大学 | Uncaria rhynchophylla total alkaloids and extraction and purification method and application thereof |
| CN113149857A (en) * | 2021-05-10 | 2021-07-23 | 山东中医药大学 | Amide compound and preparation method and application thereof |
| CN113149857B (en) * | 2021-05-10 | 2021-10-29 | 山东中医药大学 | Amide compound and preparation method and application thereof |
| CN116854690A (en) * | 2023-06-28 | 2023-10-10 | 河南中医药大学 | Indole uncaria alkaloid substance extraction method and application thereof |
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Application publication date: 20120111 |