CN102600215A - Method for extracting peganum harmala alkaloid - Google Patents
Method for extracting peganum harmala alkaloid Download PDFInfo
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- CN102600215A CN102600215A CN201110026192XA CN201110026192A CN102600215A CN 102600215 A CN102600215 A CN 102600215A CN 201110026192X A CN201110026192X A CN 201110026192XA CN 201110026192 A CN201110026192 A CN 201110026192A CN 102600215 A CN102600215 A CN 102600215A
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- macroporous resin
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Abstract
The invention relates to a method for extracting peganum harmala alkaloid, which comprises the steps that 1) peganum harmala raw materials are smashed and mixed with acid water to be percolated to obtain diacolation liquid; 2) the diacolation liquid is filled into a macroporous resin column to be adsorbed, liquid passing through the macroporous resin column is filtered by an ultrafiltration membrane, and the liquid passing through the ultrafiltration membrane is concentrated by a nanofiltration membrane to obtain concentration liquid; and 3) a pH value of the concentration liquid is adjusted to 7.5 to 8 by adding ammonia, then the mixed solution is adsorbed by the macroporous resin column, the pH value is adjusted by water washing to neutral, then 4 to 7BV 60 to 80 percent of ethanol is used for elution, the elution liquid is collected, decompressed and concentrated, and the concentration liquid is vacuum dried to obtain a product. By adopting the method to produce the peganum harmala alkaloid, the technique is simple to operate, energy consumption is low, and pollution is small. By adopting the technique, the industrialized production is easy to realize.
Description
Technical field:
The present invention relates to the alkaloidal method of a kind of extraction Herba pegani harmalae, particularly relate to a kind of employing macroporous resin adsorption and membrance separation and extract the alkaloidal method of purification Herba pegani harmalae.
Background technology:
Herba pegani harmalae Peganum harmala L. cry camel Artemisia, bitter maror, Herba rutae, Caulis et folium clerodendri bungei again, belongs to the herb of Peganum herbaceos perennial for zygophyllaceae ZygopHyllaceae plant Herba pegani harmalae.Its property is flat, bitter in the mouth, and suffering, poisonous, it has firm muscle arteries and veins, supporing yang warm the moon, eliminates the functions such as gas of sticky body fluid, dissipation cold-damp.Cure mainly diseases such as muscle weak pulse, joint osteodynia, cough with copious phlegm, hemiplegia are forgetful, coma headache, menoxenia.
The Herba pegani harmalae herb contains compositions such as alkaloid, steroidal, flavone, anthraquinone, aminoacid.Alkaloid most species wherein, its content distributes in plant and is followed successively by seed＞root＞kind of shell＞stem＞leaf; Florescence, content was the highest, was mainly banisterine and yageine; Overground part contains alkaloid 0.77%, and can rise to 5.77% florescence; Contain alkaloid 5.4%～6.3% in the mature fruit; Contain alkaloid 0.3%～0.4% in the leaf; Contain alkaloid 2.3%～2.5% in the root.Aspect biological activity, early stage research concentrates on the inhibitory action of Herba pegani harmalae alkaloid to central nervous system and monoamine oxidase, MAO.The Herba pegani harmalae alkaloid also has strong effect to cardiovascular system, respiratory system and immune system; Also have anticancer, analgesia, antiinflammatory and antifungal, kill effects such as antibacterial, antiviral and anthelmintic, document " the bioactive progress of Herba pegani harmalae alkaloid " has been done detailed elaboration to this.
Mostly the existing Herba pegani harmalae alkaloid method of extracting is sour water, alkali alcohol or supercritical extraction, cationic resin separation again, chloroform extraction or heavy metal precipitation.Like patent " a kind of spent ion exchange resin separates the method for Herba pegani harmalae total alkaloids ", the method that this patent adopts is for getting the Herba pegani harmalae extracting solution, and the adjustment pH value filters; Get filtrating and be added on the cation exchange resin column,, soak resin column with saline solution more earlier with the water elution remove impurity; To contain acid or alcoholic acid saline solution eluting, till the inspection inanimate object alkali, collect eluent again; Add the alkali neutralization, through desalting processing, concentrate drying gets middle peganum harmalaL total alkaloids.Patent " a kind of Semen pegani harmalae effective site and the monomeric preparation method and its usage of yageine " for another example; This patent disclosed method is carried out roguing and is handled at first adopting carbon dioxide supercritical fluid extraction to carry out defat and alkaline water merceration; Adopt acid alcohol-water solution to extract then, after acid is dissolved, alkali deposited, purification, drying under reduced pressure and get.Patent " a kind of production method " based on harmel alkaloid physical and chemical properties, this patent disclosed method is an alcohol reflux, concentrated solution chloroform extraction, reuse HgI separate with aluminium oxide and obtain banisterine and yageine monomer.
As stated, existing method exists: the defective workmanship that energy consumption is high, seriously polluted, the toxic agent consumption is big.
Summary of the invention:
The technical problem that the present invention will solve provides a kind of low energy consumption, the alkaloidal method of oligosaprobic extraction Herba pegani harmalae.
In order to solve the problems of the technologies described above, the present invention adopts following technical scheme to realize:
The alkaloidal method of a kind of extraction Herba pegani harmalae is characterized in that may further comprise the steps:
1) gets the Herba pegani harmalae raw material pulverizing, add the sour water percolation, get percolate;
2) the absorption of above-mentioned percolate adding macroporous resin column, post adds ultrafiltration membrance filter through liquid, and permeate adds NF membrane again and concentrates, and gets concentrated solution;
3) add ammonia to above-mentioned concentrated solution and regulate pH7.5-8, add macroporous resin column absorption again, washing is to neutral, and reuse 4-7BV60-80% ethanol elution is collected the eluent concentrating under reduced pressure, and the concentrated solution vacuum drying promptly gets product.
Sour water in the said step 1) is 0.05-0.5% hydrochloric acid or sulphuric acid water, and consumption is that the 15-20 of medical material doubly measures.
Said step 2) a kind of among the optional NK-9 of macroporous resin model, HZ806 or the S-8 in.
Said step 2) the hollow cellulose film of the optional molecular cut off 3000-6000 of the ultrafilter membrane in, the hollow cellulose film of the optional molecular cut off 100-200 of NF membrane.
A kind of among the optional SPD100 of macroporous resin model, AB-8 or the HZ818 in the said step 3).
Advantage of the present invention is: adopt the sour water percolation to extract, energy consumption is low, and the stripping that reduces impurity simultaneously helps purification; Adopt purification by macroporous resin twice, substituted chloroform extraction and ion changes resin, can reduce waste liquid and produce, adopt nanofiltration to concentrate simultaneously, the sour water that sees through can utilize once more, has reduced pollution, and membrance concentration process energy consumption is low.
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
Get seed of peganum harmala and pulverize, get 5kg, add 100kg0.05% salt sour water percolation 20 hours, percolate filters, and adds 2LNK-9 macroporous resin column absorption impurity; Collect post through liquid, add the hollow cellulose membrane ultrafiltration of molecular cut off 3000, room temperature, inlet pressure 0.6-0.8MPa; Add the suitable quantity of water dialysis, collect the hollow cellulose membrance concentration that permeate adds molecular cut off 200 again, get concentrated solution, concentrated solution adds ammonia and regulates pH7.5; Add the absorption of 3L SPD100 macroporous resin column again, washing is to neutral, and reuse 21L60% ethanol elution is collected the eluent concentrating under reduced pressure; The concentrated solution vacuum drying gets Herba pegani harmalae alkaloid 670g, and titration detects, content 98.2%.
Embodiment 2
Get the Herba pegani harmalae herb and pulverize, get 5kg, add 75kg0.5% salt sour water percolation 15 hours, percolate filters; Add 2LHZ806 macroporous resin column absorption impurity, collect the hollow cellulose membrane ultrafiltration of post, room temperature, inlet pressure 0.5-0.6MPa through liquid adding molecular cut off 6000; Add the suitable quantity of water dialysis, collect the hollow cellulose membrance concentration that permeate adds molecular cut off 100 again, get concentrated solution, concentrated solution adds ammonia and regulates pH8; Add the absorption of 3L AB-8 macroporous resin column again, washing is to neutral, and reuse 12L80% ethanol elution is collected the eluent concentrating under reduced pressure; The concentrated solution vacuum drying gets Herba pegani harmalae alkaloid 135g, and titration detects, content 95.2%.
Embodiment 3:
Get the Herba pegani harmalae root and pulverize, get 5kg, add 100kg0.05% sulphuric acid water percolation 20 hours, percolate filters, and adds 2L S-8 macroporous resin column absorption impurity; Collect post through liquid, add the hollow cellulose membrane ultrafiltration of molecular cut off 3000, room temperature, inlet pressure 0.6-0.8MPa; Add the suitable quantity of water dialysis, collect the hollow cellulose membrance concentration that permeate adds molecular cut off 200 again, get concentrated solution, concentrated solution adds ammonia and regulates pH7.5; Add the absorption of 3L HZ818 macroporous resin column again, washing is to neutral, and reuse 18L70% ethanol elution is collected the eluent concentrating under reduced pressure; The concentrated solution vacuum drying gets Herba pegani harmalae alkaloid 162g, and titration detects, content 97.2%.
Embodiment 4:
Get seed of peganum harmala and pulverize, get 10kg, add 200kg0.1% sulphuric acid water percolation 20 hours, percolate filters, and adds 5L S-8 macroporous resin column absorption impurity; Collect post through liquid, add the hollow cellulose membrane ultrafiltration of molecular cut off 3000, room temperature, inlet pressure 0.5-0.8MPa; Add the suitable quantity of water dialysis, collect the hollow cellulose membrance concentration that permeate adds molecular cut off 200 again, get concentrated solution, concentrated solution adds ammonia and regulates pH7.5; Add the absorption of 6L AB-8 macroporous resin column again, washing is to neutral, and reuse 35L70% ethanol elution is collected the eluent concentrating under reduced pressure; The concentrated solution vacuum drying gets Herba pegani harmalae alkaloid 1453g, and titration detects, content 98.8%.
Embodiment 5:
Get the Herba pegani harmalae herb and pulverize, get 20kg, add 400kg0.1% salt sour water percolation 20 hours, percolate filters, and adds 10LHZ806 macroporous resin column absorption impurity; Collect post through liquid, add the hollow cellulose membrane ultrafiltration of molecular cut off 3000, room temperature, inlet pressure 0.5-0.8MPa; Add the suitable quantity of water dialysis, collect the hollow cellulose membrance concentration that permeate adds molecular cut off 200 again, get concentrated solution, concentrated solution adds ammonia and regulates pH7.5; Add the absorption of 6L AB-8 macroporous resin column again, washing is to neutral, and reuse 70L75% ethanol elution is collected the eluent concentrating under reduced pressure; The concentrated solution vacuum drying gets Herba pegani harmalae alkaloid 563g, and titration detects, content 96.3%.
Claims (5)
1. one kind is extracted the alkaloidal method of Herba pegani harmalae, it is characterized in that may further comprise the steps:
1) gets the Herba pegani harmalae raw material pulverizing, add the sour water percolation, get percolate;
2) the absorption of above-mentioned percolate adding macroporous resin column, post adds ultrafiltration membrance filter through liquid, and permeate adds NF membrane again and concentrates, and gets concentrated solution;
3) add ammonia to above-mentioned concentrated solution and regulate pH7.5-8, add macroporous resin column absorption again, washing is to neutral, and reuse 4-7BV60-80% ethanol elution is collected the eluent concentrating under reduced pressure, and the concentrated solution vacuum drying promptly gets product.
2. according to the alkaloidal method of the said extraction Herba pegani harmalae of claim 1, it is characterized in that the sour water in the said step 1) is 0.05-0.5% hydrochloric acid or sulphuric acid water, consumption is that the 15-20 of medical material doubly measures.
3. according to the alkaloidal method of the said extraction Herba pegani harmalae of claim 1, it is characterized in that said step 2) in the optional NK-9 of macroporous resin model, HZ806 or S-8 in a kind of.
4. according to the alkaloidal method of the said extraction Herba pegani harmalae of claim 1, it is characterized in that said step 2) in the hollow cellulose film of the optional molecular cut off 3000-6000 of ultrafilter membrane, the hollow cellulose film of the optional molecular cut off 100-200 of NF membrane.
5. according to the alkaloidal method of the said extraction Herba pegani harmalae of claim 1, it is characterized in that a kind of among the optional SPD100 of macroporous resin model, AB-8 or the HZ818 in the said step 3).
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| CN201110026192XA CN102600215A (en) | 2011-01-25 | 2011-01-25 | Method for extracting peganum harmala alkaloid |
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| CN201110026192XA CN102600215A (en) | 2011-01-25 | 2011-01-25 | Method for extracting peganum harmala alkaloid |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104382964A (en) * | 2014-10-27 | 2015-03-04 | 上海中医药大学 | Method for preparing peganum harmala linn total alkaloid extract and peganum harmala linn total flavone extract from peganum harmala linn |
| CN104628731A (en) * | 2015-01-27 | 2015-05-20 | 中国农业科学院兰州畜牧与兽药研究所 | Method for extracting peganum harmala alkaloid under microwave assistance |
| CN109884194A (en) * | 2017-12-06 | 2019-06-14 | 新疆维吾尔药业有限责任公司 | A kind of separation method of medicinal plant and products thereof and application |
| CN109879872A (en) * | 2017-12-06 | 2019-06-14 | 新疆维吾尔药业有限责任公司 | A kind of separation method of peganum harmala L and products thereof and application |
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| CN1970530A (en) * | 2006-11-28 | 2007-05-30 | 广西大学 | Method for separating and purifying capsaicin compound using membrane separation technology |
| CN101513466A (en) * | 2009-03-18 | 2009-08-26 | 裴刚 | Method for preparing quinoline alkaloid from zanthoxylum dissitum Hemsl |
| CN101697983A (en) * | 2007-05-31 | 2010-04-28 | 北京和润创新医药科技发展有限公司 | Method for separating pegamun harmala total alkaloids by ion exchange resin |
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| CN1970530A (en) * | 2006-11-28 | 2007-05-30 | 广西大学 | Method for separating and purifying capsaicin compound using membrane separation technology |
| CN101697983A (en) * | 2007-05-31 | 2010-04-28 | 北京和润创新医药科技发展有限公司 | Method for separating pegamun harmala total alkaloids by ion exchange resin |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104382964A (en) * | 2014-10-27 | 2015-03-04 | 上海中医药大学 | Method for preparing peganum harmala linn total alkaloid extract and peganum harmala linn total flavone extract from peganum harmala linn |
| CN104382964B (en) * | 2014-10-27 | 2017-07-28 | 上海中医药大学 | A kind of method that the careless total alkaloid extract of harmel and the careless extractive of general flavone of harmel are prepared by harmel grass |
| CN104628731A (en) * | 2015-01-27 | 2015-05-20 | 中国农业科学院兰州畜牧与兽药研究所 | Method for extracting peganum harmala alkaloid under microwave assistance |
| CN104628731B (en) * | 2015-01-27 | 2017-02-22 | 中国农业科学院兰州畜牧与兽药研究所 | Method for extracting peganum harmala alkaloid under microwave assistance |
| CN109884194A (en) * | 2017-12-06 | 2019-06-14 | 新疆维吾尔药业有限责任公司 | A kind of separation method of medicinal plant and products thereof and application |
| CN109879872A (en) * | 2017-12-06 | 2019-06-14 | 新疆维吾尔药业有限责任公司 | A kind of separation method of peganum harmala L and products thereof and application |
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Application publication date: 20120725 |