CN101857526A - Method for preparing galactitol or galactitol extract from cistanche or waste residue liquid of cistanche glycoside extraction and application of galactitol and galactitol extract - Google Patents
Method for preparing galactitol or galactitol extract from cistanche or waste residue liquid of cistanche glycoside extraction and application of galactitol and galactitol extract Download PDFInfo
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- CN101857526A CN101857526A CN200910134703A CN200910134703A CN101857526A CN 101857526 A CN101857526 A CN 101857526A CN 200910134703 A CN200910134703 A CN 200910134703A CN 200910134703 A CN200910134703 A CN 200910134703A CN 101857526 A CN101857526 A CN 101857526A
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Abstract
The invention provides a method for extracting and preparing galactitol and a component containing the galactitol from a cistanche medicinal material or waste residue liquid of cistanche glycoside extraction. The galactitol is an active constituent of the cistanche for taking the effect of loosing the bowel to relieve constipation and can be used as an additive of a functional health-care food preparation. The invention solves the problem of sufficient utilization of cistanche water-soluble residue liquid, improves the utilization value of cistanche plant resources and has good market development prospect.
Description
Technical field
The present invention relates to put forward the method for extraction separation melampyrum and melampyrum extract the glycosides waste residue liquid, the invention still further relates to their application in function of relaxing bowel food, healthcare products from Herba Cistanches and Herba Cistanches.
Background technology
Chinese medicine Herba Cistanches Herba Cistanches is the chylocaulous of Orobanchaceae Orobanchaceae Cistanche Hoffmgg. et Link plants Cistanche Hoffmg.EtLink arid zones scale leaf, beginning is stated from Shennong's Herbal, classify as top grade, tool kidney-replenishing, benefiting essence-blood, effect such as relax bowel are famous traditional tonic medicines.Its occurrence frequency in successive dynasties kidney-replenishing prescription is the highest, and the probability in anti-senility class prescriptions of traditional Chinese medicine is only second to genseng and occupies the second, and the title of " desert genseng " is therefore arranged again.Gentle because of its determined curative effect, the property of medicine, mend not high, support not dryly, Herba Cistanches is widely used in Chinese patent medicine, food therapeutic health, the tcm clinical practice prescription.
Over nearly one, 20 year, along with worldwide development and use natural plant resource grows with each passing day, Herba Cistanches becomes the hot subject of medical educational circles research with the historical and unique pharmaceutical use of its long medication.The achievement in research of comprehensive each side, benzyl carbinol glycosides compounds are the maximum chemical ingredientss of report in the present Cistanche Hoffmgg. et Link plants, also are topmost activeconstituentss in the Herba Cistanches.Clear and definite substantially this compounds of modern study is the basic substance that Herba Cistanches has multiple pharmacologically actives such as establishing-Yang, anti-oxidant, anti-ageing, memory.The domestic and international at present utilization to the Herba Cistanches resource is only limited to the benzyl carbinol glycosides compounds substantially, drug manufacturing enterprise is to being that the flow process of the Chinese medicine preparation production of main raw material also mainly concentrates on the extraction purifying to the benzyl carbinol glycosides constituents with the Herba Cistanches, extracts preparation melampyrum few people research in a large number glycosides waste residue, the waste liquid and carry from Herba Cistanches and Herba Cistanches.Waste residue, waste liquid that Herba Cistanches is extracted after the phenylethanol compound go out of use, not only severe contamination environment, and caused the significant wastage of Herba Cistanches herb resource.
Composition Study shows that the Herba Cistanches medicinal material contains a large amount of melampyrums, and it extensively is present in the Cistanche Hoffmgg. et Link plants.Melampyrum can improve osmotic pressure in the intestines, promotes intestinal peristalsis, suppresses the absorption of large intestine to moisture, is the main active ingredient that relaxes bowel in the Herba Cistanches.There is the scholar to adopt methods such as different solvents extraction, separation and recrystallization that Herba Cistanches is divided into melampyrum group, ethyl acetate extract group, n-butanol extract group and 4 components of residue water solubles group, carried out influence experiment to the mouse defaecation time, the result shows that the melampyrum group has significant shortening defaecation time effect, and other 3 component effects are not remarkable, show that melampyrum is the essential substance basis of Herba Cistanches effect of relaxing bowel.Melampyrum is as water-soluble very high multicomponent alcoholics compound in the Herba Cistanches medicinal material, mainly is present in the residual waste liquid, waste residue of the total glycosides of macroporous adsorbent resin preparation of industrialization phenylethyl alcohol.Xinjiang is that the distribution of Herba Cistanches plant resources is the widest, the area that output is the highest, the industrialization of Herba Cistanches, the marketization have reached considerable scale, our the obligated methodology of melampyrum in the Herba Cistanches being carried out separation and purification that also is necessary of research staff as the Xinjiang natural drug is inquired into, sum up an effective preparation were established, the a large amount of water-soluble waste residue that the total glycosides of preparation of industrialization phenylethyl alcohol stays is utilized, turned waste into wealth.
Comprehensive previous finding, melampyrum is clear and definite substantially as the activeconstituents that Herba Cistanches relaxes bowel, but have not yet to see the report of carrying a large amount of extraction separation melampyrums glycosides waste residue, the waste liquid or its extract from Herba Cistanches or Herba Cistanches, do not see that also having with natural melampyrum reactive site in the Herba Cistanches is the report that feedstock production becomes function of relaxing bowel Sexual health promotion food.
Summary of the invention
The invention solves the problem that makes full use of of the water-soluble residue liquid of Herba Cistanches.The purpose of invention is to provide a kind of and puies forward a large amount of methods that prepare melampyrum or its extract of extracting glycosides waste residue, the waste liquid from Herba Cistanches medicinal material or Herba Cistanches, comprises that also with natural melampyrum in the Herba Cistanches or its extract be the preparation of the functional health-care food with functions of loosening bowel relieving constipation of raw material.
Technical scheme of the present invention is achieved like this:
The method for preparing the melampyrum efficient part of from the Herba Cistanches medicinal material, extracting provided by the invention, its step is as follows:
Step 1, get the chylocaulous of the clean raw medicinal material Herba Cistanches arid zones scale leaf of removing impurity, pulverize, water or/and organic solvent extract;
Step 2, the extracting solution of step 1 gained is merged, concentrate, add the water suspendible, add several times amount high concentration ethanol again, water/pure method precipitation is removed water-soluble impurities such as polysaccharide, protein, inorganic salt;
Step 3, the filtrate of step 2 gained is concentrated, last macroporous adsorptive resins is that elutriant carries out wash-out with water.In elution process, carry out the o-dihydroxy reaction monitoring, collect o-dihydroxy positive reaction stream part with redox titration;
Step 4, stream part of step 3 collection is concentrated, dry promptly gets the melampyrum extract, can get colourless crystallization shape melampyrum monomeric compound with the polar organic solvent recrystallization.
The chylocaulous that the described Herba Cistanches medicinal material of step 1 is a Cistanche Hoffmgg. et Link plants arid zones scale leaf, comprise by " Herba Cistanches Cistanche deserticola Y.C.Ma that Chinese pharmacopoeia (version in 2005) is recorded and Cistanche Tubulosa Cistanche tubulosa (Schenk) Wight also comprise not by " Chinese pharmacopoeia is recorded but the Saline Cistanche Herb Cistanche salsa G.Beck of circulation is extensively arranged on market;
The described organic solvent of step 1 is that carbonatomss such as methyl alcohol, ethanol, propyl alcohol, Virahol are 1~5 low-carbon alcohol; Carbonatomss such as acetone, methylethylketone, diethyl ketone are 3~6 low-carbon (LC) ketone;
The consumption of the described extraction solvent of step 1 is 3~10 times of medicinal material amount;
The described extraction time of step 1 is 2~4 times;
The described extracting method of step 1 is that heating and refluxing extraction, diacolation extract, dipping extracts or supersound extraction;
The described adding high concentration ethanol of step 2 amount should make the alcohol amount that contains of whole water-pure system reach 40~90%;
The described macroporous adsorptive resins of step 3 is low polarity or Semi-polarity polymeric adsorbent, is among AB-8, D-101, DA-201, CAD-40, HPD-400, HPD-500, PD-400A, PD-450, XAD-2, XAD-4 or the SP-825 etc. any;
The described concentrated solution drying means of step 4 is spraying drying, lyophilize, constant pressure and dry or vacuumizes drying under reduced pressure;
The described polarity solvent that is used for crystallization or recrystallization of step 4 can be the mixed solvent of any or they of methyl alcohol, ethanol, acetone.
Provided by the invention carry the glycosides waste residue liquid extracting from Herba Cistanches prepare the method at melampyrum position, its step is as follows:
1, get the water elution liquid waste residue of Herba Cistanches medicinal material through macroporous adsorbent resin extraction benzyl carbinol glycosides composition, water is or/and the organic solvent extraction;
2, the extracting solution with step 1 gained merges, and concentrates, and adds the water suspendible, and last granular active carbon post resin column is that elutriant carries out wash-out with water.In elution process, carry out the o-dihydroxy reaction monitoring, collect o-dihydroxy positive reaction stream part with redox titration;
3, stream part that step 2 is collected is concentrated, dry, promptly gets the melampyrum extract, can get colourless crystallization shape melampyrum monomeric compound with the polar organic solvent recrystallization.
The described waste residue of step 1 is Herba Cistanches Cistanche deserticola Y.C.Ma, Cistanche Tubulosa Cistanche tubulosa (Schenk) Wight or Saline Cistanche Herb Cistanche salsa G.Beck medicinal material extract the benzyl carbinol glycosides composition through macroporous adsorbent resin a water elution liquid waste residue;
The described organic solvent of step 1 is that carbonatomss such as methyl alcohol, ethanol, propyl alcohol, Virahol are 1~5 low-carbon alcohol; Carbonatomss such as acetone, methylethylketone, diethyl ketone are 3~6 low-carbon (LC) ketone;
The consumption of the described extraction solvent of step 1 is 3~20 times of medicinal material amount;
The described extraction time of step 1 is 2~4 times;
The described extracting method of step 1 is that heating and refluxing extraction, diacolation extract, dipping extracts or supersound extraction;
The described concentrated solution drying means of step 3 is spraying drying, lyophilize, constant pressure and dry or vacuumizes drying under reduced pressure;
The described polarity solvent that is used for crystallization or recrystallization of step 3 can be the mixed solvent of any or they of methyl alcohol, ethanol, acetone.
What the invention solves the water-soluble residue liquid of Herba Cistanches utilizes problem again, easy, the easy row of method, and the active constituent content height of gained bulk drug, color and luster is good.This preparation were established adopts conventional extraction equipment in addition, and does not use deleterious organic solvent, so cost is low, and is pollution-free, is applicable to suitability for industrialized production.
The inventive method is extracted the melampyrum position of preparation, requires can be made into the functional health-care food with effect of relaxing bowel according to the technology preparation process in modern times.Contain the above-mentioned melampyrum position of 1~99% weight part in the protective foods, preferably contain 10~70% weight parts.
Above-mentioned protective foods is according to market demand and formulation requirement, can add various auxiliary materials and/or other Chinese medical extract is formed various oral preparations.
Auxiliary material of the present invention is solvent, tackiness agent, disintegrating agent, weighting agent, wetting agent, correctives, sanitas etc.
Other Chinese medical extract of the present invention is good with phenylethyl alcohol total glycosides extractive in the Herba Cistanches.
Oral preparations of the present invention can be tablet, pill, electuary, capsule, oral liquid, suspension, granule, tea drink etc.
Along with improving constantly of standard of living, people also have higher requirement to quality of life, particularly self health care are more and more paid attention to.Herba Cistanches is the agent of flat benefits, " book on Chinese herbal medicine converge speech " cloud: " Herba Cistanches, temperature and not hot are mended and not high, warm and not dry, and be sliding and do not let out, so name is calmly arranged also ".This characteristic of base with the additive of Herba Cistanches as the tonic of building up one's health by taking tonic, is easier to be accepted by the popular crowd of common physical appearance.The present invention be exactly extract to carry the glycosides waste residue liquid from Herba Cistanches or Herba Cistanches, isolating melampyrum or melampyrum extract be the function of relaxing bowel Sexual health promotion food that main raw material is made, property of medicine gentleness, safety non-toxic, determined curative effect, when being added with Herba Cistanches phenylethyl alcohol total glycosides extractive in the preparation, product has been increased nourish anti-ageing effect, be suitable for taking for a long time, have good market development application prospect.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail, but does not limit the present invention with this.
Embodiment 1: be feedstock production melampyrum extract or melampyrum with the Herba Cistanches
1, gets the Herba Cistanches chylocaulous 200g of the arid zones scale leaf of removing impurity, be cut into small pieces, be ground into 20 order particles;
2, extracted 2 hours with 10 times of amount 70% alcohol heating reflux earlier, measure 70% alcohol reflux 2 times, each 1 hour with 8 times then;
3, united extraction liquid is evaporated to the medicinal extract shape, adds ethanol to containing alcohol amount 50%, and standing over night is filtered;
4, filtrate decompression concentrates, and is dissolved in water SP825 macroporous adsorptive resins on the water liquid.The water wash-out is collected the stream part (o-dihydroxy reacting positive) that wherein contains melampyrum, is evaporated to thick paste, gets the melampyrum extract through lyophilize again, can get colourless crystallization shape melampyrum with ethyl alcohol recrystallization.
Embodiment 2: carry from Herba Cistanches and extract preparation melampyrum or its extract the glycosides waste residue liquid
1, gets the water elution liquid waste residue (500g) of Herba Cistanches, add 10 times of amount 70% alcohol immersion diacolations earlier and extracted 72 hours, measure 70% alcohol immersion diacolations with 8 times then and extract each 48 hours 2 times through macroporous adsorbent resin extraction benzyl carbinol glycosides composition;
2, united extraction liquid, concentrating under reduced pressure is dissolved in water, granular active carbon post resin column on the water liquid.With water elution, collect the stream part (o-dihydroxy reacting positive) that wherein contains melampyrum, be evaporated to thick paste, the spray-dried again melampyrum extract that gets can get colourless crystallization shape melampyrum with ethyl alcohol recrystallization.
Embodiment 3: the relax bowel preparation of health tea of a kind of natural melampyrum
Get 1kg high-quality black tea and 80g cyclodextrin, soak 30min down with 80 ℃ of water-baths of 10kg double distilled water, filter residue soaks down with 80 ℃ of water-baths of 8kg double distilled water and extracts each 20min 2 times.3 gained filtrates are merged, and concentrating under reduced pressure becomes the thick paste shape, 95 ℃ of tower temperature internal spraying dryings, gets effective content of tea and extracts the about 200g of dry powder.Spray-dried 100g Herba Cistanches phenylethyl alcohol total glycosides extractive, the natural melampyrum of 100g and above-mentioned tealeaves are extracted dry powder merge, add the fragrant and sweet element of 50g dextrin and 20g,, spray 75% ethanol system softwood through the 80 mesh sieves mixing that sieves repeatedly.Softwood is crossed 12 mesh sieves and is granulated, and dries under 60 ℃ of conditions, again through the whole grain of 14 mesh sieves, as 1 repackaging unit, in the tea filter paper bag of packing into, after the shaping packing, uses the cobalt radiation sterilization, promptly with every 5g.
Claims (9)
1. one kind is extracted the method for preparing the melampyrum efficient part from the Herba Cistanches medicinal material, it is characterized in that this method and step are:
(1) get the chylocaulous of the clean Herba Cistanches arid zones scale leaf of removing impurity, pulverize, with refluxing extraction, diacolation extract, dipping extracts or ultrasonic extracting method, with 3~10 times of water that is equivalent to the medicinal material amount or/and organic solvent extract 2~4 times;
(2) extracting solution with step 1 gained merges, and concentrates, and adds the water suspendible, adds several times amount high concentration ethanol again, makes the alcohol amount that contains of whole water-pure system reach 40~90%, and water/pure method precipitation is removed water-soluble impurities such as polysaccharide, protein, inorganic salt;
(3) filtrate with step 2 gained concentrates, and last macroporous adsorptive resins is that elutriant carries out wash-out with water.In elution process, carry out the o-dihydroxy reaction monitoring, collect o-dihydroxy positive reaction stream part with redox titration;
(4) stream part that step 3 is collected is concentrated, dry, promptly gets the melampyrum extract, can get colourless crystallization shape melampyrum monomeric compound with the polar organic solvent recrystallization.
2. by the described method for preparing the melampyrum efficient part of from the Herba Cistanches medicinal material, extracting of claim 1, it is characterized in that, the chylocaulous that the described Herba Cistanches medicinal material of step (1) is a Cistanche Hoffmgg. et Link plants arid zones scale leaf, comprise by " Herba Cistanches Cistanche deserticola Y.C.Ma that Chinese pharmacopoeia (version in 2005) is recorded and Cistanche Tubulosa Cistanche tubulosa (Schenk) Wight, also comprise not by " Chinese pharmacopoeia is recorded but the Saline Cistanche Herb Cistanche salsa G.Beck of circulation is extensively arranged on market, described extraction solvent is a methyl alcohol, ethanol, propyl alcohol, carbonatomss such as Virahol are 1~5 low-carbon alcohol, acetone, methylethylketone, carbonatomss such as diethyl ketone are 3~6 low-carbon (LC) ketone.
3. by the described method for preparing the melampyrum efficient part of from the Herba Cistanches medicinal material, extracting of claim 1, it is characterized in that, the described macroporous adsorptive resins of step (3) is low polarity or Semi-polarity polymeric adsorbent, is among AB-8, D-101, DA-201, CAD-40, HPD-400, HPD-500, PD-400A, PD-450, XAD-2, XAD-4 or the SP-825 etc. any.
4. by the described method for preparing the melampyrum efficient part of from the Herba Cistanches medicinal material, extracting of claim 1, it is characterized in that, the described concentrated solution drying means of step (4) is spraying drying, lyophilize, constant pressure and dry or vacuumizes drying under reduced pressure, and the described polarity solvent that is used for crystallization or recrystallization can be the mixed solvent of any or they of methyl alcohol, ethanol, acetone.
5. carry the glycosides waste residue liquid extracting from Herba Cistanches and prepare the method at melampyrum position for one kind, it is characterized in that this method and step are:
(1) get the Herba Cistanches medicinal material and extract the water elution liquid waste residue of benzyl carbinol glycosides composition through macroporous adsorbent resin, with refluxing extraction, diacolation extract, dipping extracts or ultrasonic extracting method, with 3~10 times of water that is equivalent to the medicinal material amount or/and organic solvent extract 2~4 times;
(2) extracting solution with step 1 gained merges, and concentrates, and adds the water suspendible, and last granular active carbon post resin column is that elutriant carries out wash-out with water.In elution process, carry out the o-dihydroxy reaction monitoring, collect o-dihydroxy positive reaction stream part with redox titration;
(3) stream part that step 2 is collected is concentrated, dry, promptly gets the melampyrum extract, can get colourless crystallization shape melampyrum monomeric compound with the polar organic solvent recrystallization.
By claim 5 described carry the glycosides waste residue liquid extracting from Herba Cistanches prepare the method at melampyrum position, it is characterized in that, the described waste residue of step (1) is Herba Cistanches Cistanche deserticola Y.C.Ma, Cistanche Tubulosa Cistanche tubulosa (Schenk) Wight or Saline Cistanche Herb Cistanche salsa G.Beck medicinal material extract the water elution liquid waste residue of benzyl carbinol glycosides composition through macroporous adsorbent resin, described extraction solvent is a methyl alcohol, ethanol, propyl alcohol, carbonatomss such as Virahol are 1~5 low-carbon alcohol, acetone, methylethylketone, carbonatomss such as diethyl ketone are 3~6 low-carbon (LC) ketone.
By claim 5 described carry the glycosides waste residue liquid extracting from Herba Cistanches prepare the method at melampyrum position, it is characterized in that, the described concentrated solution drying means of step (3) is spraying drying, lyophilize, constant pressure and dry or vacuumizes drying under reduced pressure, and the described polarity solvent that is used for crystallization or recrystallization can be the mixed solvent of any or they of methyl alcohol, ethanol, acetone.
8. by the described extract that derives from the natural melampyrum of Herba Cistanches medicinal material or contain melampyrum of claim 1, use separately or and other relax bowel the composition combined utilization in functional foodstuff, health-care preparation.
9. derive from the extract that Herba Cistanches is carried the natural melampyrum in the glycosides waste residue liquid or contains melampyrum by claim 5 is described, use separately or and other relax bowel the composition combined utilization in functional foodstuff, health-care preparation.
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CN200910134703A CN101857526A (en) | 2009-04-13 | 2009-04-13 | Method for preparing galactitol or galactitol extract from cistanche or waste residue liquid of cistanche glycoside extraction and application of galactitol and galactitol extract |
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CN200910134703A CN101857526A (en) | 2009-04-13 | 2009-04-13 | Method for preparing galactitol or galactitol extract from cistanche or waste residue liquid of cistanche glycoside extraction and application of galactitol and galactitol extract |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102114079A (en) * | 2011-02-16 | 2011-07-06 | 中国农业大学 | Method for extracting desertliving cistanche extract and application thereof |
CN103191196A (en) * | 2013-04-03 | 2013-07-10 | 中国科学院过程工程研究所 | Integrated ultrasonic cyclic extracting and separating technology for cistanche functional ingredient |
CN105272919A (en) * | 2015-11-12 | 2016-01-27 | 中国科学院过程工程研究所 | Method of preparing allantoin from cistanche oligomerization syrup |
CN105648016A (en) * | 2016-03-30 | 2016-06-08 | 蔡庭守 | Herba cistanche small molecule peptide extract, preparation method and application thereof |
CN105796656A (en) * | 2016-05-17 | 2016-07-27 | 杏辉天力(杭州)药业有限公司 | Cistanche tubulosa extract and preparation method thereof |
CN109091430A (en) * | 2018-09-29 | 2018-12-28 | 广州今盛美精细化工有限公司 | A kind of Herba Cistanches extract and its preparing the application in cosmetics |
CN109173335A (en) * | 2018-10-18 | 2019-01-11 | 湖北民族学院 | A kind of extraction preparation method visualizing vine tea active constituent |
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2009
- 2009-04-13 CN CN200910134703A patent/CN101857526A/en active Pending
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102114079A (en) * | 2011-02-16 | 2011-07-06 | 中国农业大学 | Method for extracting desertliving cistanche extract and application thereof |
CN102114079B (en) * | 2011-02-16 | 2012-04-11 | 中国农业大学 | Method for extracting desertliving cistanche extract and application thereof |
CN103191196A (en) * | 2013-04-03 | 2013-07-10 | 中国科学院过程工程研究所 | Integrated ultrasonic cyclic extracting and separating technology for cistanche functional ingredient |
CN103191196B (en) * | 2013-04-03 | 2015-04-01 | 中国科学院过程工程研究所 | Integrated ultrasonic cyclic extracting and separating technology for cistanche functional ingredient |
CN105272919A (en) * | 2015-11-12 | 2016-01-27 | 中国科学院过程工程研究所 | Method of preparing allantoin from cistanche oligomerization syrup |
CN105648016A (en) * | 2016-03-30 | 2016-06-08 | 蔡庭守 | Herba cistanche small molecule peptide extract, preparation method and application thereof |
CN105796656A (en) * | 2016-05-17 | 2016-07-27 | 杏辉天力(杭州)药业有限公司 | Cistanche tubulosa extract and preparation method thereof |
CN109091430A (en) * | 2018-09-29 | 2018-12-28 | 广州今盛美精细化工有限公司 | A kind of Herba Cistanches extract and its preparing the application in cosmetics |
CN109173335A (en) * | 2018-10-18 | 2019-01-11 | 湖北民族学院 | A kind of extraction preparation method visualizing vine tea active constituent |
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Application publication date: 20101013 |