CN101041677A - Producing raw material containing benzyl carbinol glycosides from Cistanche deserticola by using membrane separation technique and preparation method thereof - Google Patents
Producing raw material containing benzyl carbinol glycosides from Cistanche deserticola by using membrane separation technique and preparation method thereof Download PDFInfo
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- CN101041677A CN101041677A CN 200710102756 CN200710102756A CN101041677A CN 101041677 A CN101041677 A CN 101041677A CN 200710102756 CN200710102756 CN 200710102756 CN 200710102756 A CN200710102756 A CN 200710102756A CN 101041677 A CN101041677 A CN 101041677A
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- herba cistanches
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- benzyl carbinol
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- carbinol glycosides
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- 239000002994 raw material Substances 0.000 title claims abstract description 70
- 239000012528 membrane Substances 0.000 title claims description 89
- 229930182470 glycoside Natural products 0.000 title claims description 51
- -1 benzyl carbinol glycosides Chemical class 0.000 title claims description 47
- 238000000926 separation method Methods 0.000 title claims description 46
- 238000002360 preparation method Methods 0.000 title claims description 14
- 241000336291 Cistanche deserticola Species 0.000 title abstract description 3
- 238000000034 method Methods 0.000 claims abstract description 48
- 238000001035 drying Methods 0.000 claims abstract description 22
- 241000005787 Cistanche Species 0.000 claims description 103
- 239000007788 liquid Substances 0.000 claims description 57
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- 230000008569 process Effects 0.000 claims description 34
- 239000000126 substance Substances 0.000 claims description 30
- 238000005516 engineering process Methods 0.000 claims description 28
- 238000001728 nano-filtration Methods 0.000 claims description 26
- 238000000108 ultra-filtration Methods 0.000 claims description 24
- 239000000706 filtrate Substances 0.000 claims description 23
- 238000000605 extraction Methods 0.000 claims description 22
- 238000001471 micro-filtration Methods 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- 239000000284 extract Substances 0.000 claims description 15
- 239000006228 supernatant Substances 0.000 claims description 15
- QFRYQWYZSQDFOS-UHFFFAOYSA-N verbascoside Natural products CC1OC(COC2C(O)C(COC3OC(C(O)C(O)C3O)C(=O)O)OC(Oc4cc(O)cc5OC(=CC(=O)c45)c6ccc(O)c(O)c6)C2O)C(O)C(O)C1O QFRYQWYZSQDFOS-UHFFFAOYSA-N 0.000 claims description 14
- NJYVDFDTLLZVMG-UHFFFAOYSA-N echinacoside Natural products CC1OC(OC2C(O)C(OCCc3ccc(O)c(O)c3)OC(COC4OC(CO)C(O)C(O)C4O)C2OC(=O)C=Cc5cc(O)cc(O)c5)C(O)C(O)C1O NJYVDFDTLLZVMG-UHFFFAOYSA-N 0.000 claims description 9
- FSBUXLDOLNLABB-ISAKITKMSA-N echinacoside Chemical compound O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1O[C@H]1[C@H](OC(=O)\C=C\C=2C=C(O)C(O)=CC=2)[C@@H](CO[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O)O[C@@H](OCCC=2C=C(O)C(O)=CC=2)[C@@H]1O FSBUXLDOLNLABB-ISAKITKMSA-N 0.000 claims description 9
- KDSWDGKIENPKLB-QJDQKFITSA-N verbascoside Chemical compound O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1O[C@H]1[C@H](OC(=O)CCC=2C=C(O)C(O)=CC=2)[C@@H](CO)O[C@@H](OCCC=2C=C(O)C(O)=CC=2)[C@@H]1O KDSWDGKIENPKLB-QJDQKFITSA-N 0.000 claims description 9
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- 239000011780 sodium chloride Substances 0.000 claims description 7
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- ALERZNQPBWWLMW-UHFFFAOYSA-N 2''-acetylacteoside Natural products OC1C(O)C(O)C(C)OC1OC1C(OC(C)=O)C(OCCC=2C=C(O)C(O)=CC=2)OC(CO)C1OC(=O)C=CC1=CC=C(O)C(O)=C1 ALERZNQPBWWLMW-UHFFFAOYSA-N 0.000 claims description 2
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- FNMHEHXNBNCPCI-QEOJJFGVSA-N Isoacteoside Chemical compound O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1O[C@@H]1[C@@H](O)[C@H](OCCC=2C=C(O)C(O)=CC=2)O[C@H](COC(=O)\C=C\C=2C=C(O)C(O)=CC=2)[C@H]1O FNMHEHXNBNCPCI-QEOJJFGVSA-N 0.000 claims description 2
- HFJIGXAMJFDVFR-OMRKUVHCSA-N O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1O[C@@H]1[C@@H](OC(C)=O)[C@H](OCCC=2C=C(O)C(O)=CC=2)O[C@H](COC(=O)\C=C\C=2C=C(O)C(O)=CC=2)[C@H]1O Chemical compound O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1O[C@@H]1[C@@H](OC(C)=O)[C@H](OCCC=2C=C(O)C(O)=CC=2)O[C@H](COC(=O)\C=C\C=2C=C(O)C(O)=CC=2)[C@H]1O HFJIGXAMJFDVFR-OMRKUVHCSA-N 0.000 claims description 2
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- KJJKGAYHJMZKLA-DBDAIDROSA-N [(2r,3r,4s,5r,6r)-5-acetyloxy-6-[2-(3,4-dihydroxyphenyl)ethoxy]-2-(hydroxymethyl)-4-[[(2s,3r,4r,5r,6s)-3,4,5-trihydroxy-6-methyloxan-2-yl]methoxy]oxan-3-yl] (e)-3-(3,4-dihydroxyphenyl)prop-2-enoate Chemical compound O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1CO[C@@H]1[C@@H](OC(C)=O)[C@H](OCCC=2C=C(O)C(O)=CC=2)O[C@H](CO)[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 KJJKGAYHJMZKLA-DBDAIDROSA-N 0.000 claims description 2
- MRIFZKMKTDPBHR-UHFFFAOYSA-N boschnaloside Natural products CC1CCC(C(=CO2)C=O)C1C2OC1OC(CO)C(O)C(O)C1O MRIFZKMKTDPBHR-UHFFFAOYSA-N 0.000 claims description 2
- FNMHEHXNBNCPCI-RYEKTNFUSA-N isoacteoside Natural products C[C@@H]1O[C@H](O[C@H]2[C@H](O)[C@@H](COC(=O)C=Cc3ccc(O)c(O)c3)O[C@@H](OCCc4ccc(O)c(O)c4)[C@@H]2O)[C@H](O)[C@H](O)[C@H]1O FNMHEHXNBNCPCI-RYEKTNFUSA-N 0.000 claims description 2
- 150000002576 ketones Chemical class 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims description 2
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- 239000000047 product Substances 0.000 description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 7
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- 239000004615 ingredient Substances 0.000 description 6
- WRMNZCZEMHIOCP-UHFFFAOYSA-N 2-phenylethanol Chemical compound OCCC1=CC=CC=C1 WRMNZCZEMHIOCP-UHFFFAOYSA-N 0.000 description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 5
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
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- 150000004676 glycans Chemical class 0.000 description 4
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- 229940067107 phenylethyl alcohol Drugs 0.000 description 4
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- 108090000623 proteins and genes Proteins 0.000 description 4
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 description 3
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- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 description 1
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Landscapes
- Medicines Containing Plant Substances (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a manufacturing method of raw material with phenethylol from Cistanche deserticola through film separating technique, which comprises the following steps: selecting material; extracting; micro-filtering; hyperfiltering; nano-filtering; drying; obtaining the product with effective enriching; improving the extracting rate of effective component; saving manufacturing cost; shortening technical period.
Description
Technical field
The present invention relates to a kind of from Herba Cistanches, produce contain raw material of benzyl carbinol glycosides and preparation method thereof, especially a kind of using membrane separating technology is produced from Herba Cistanches contains raw material of benzyl carbinol glycosides and preparation method thereof.
Background technology
Chinese medicine Herba Cistanches Herba Cistanches is the chylocaulous of Orobanchaceae Orobanchaceae Cistanche Hoffmgg. et Link plants CistancheHoffmg.Et Link 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 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.At present pharmacy corporation is to being that the technological process of production of medicine, the healthcare products of main raw material also mainly concentrates on the extraction enrichment to benzyl carbinol glycosides with the Herba Cistanches.
Japanese document has been introduced a kind of method of extraction separation benzyl carbinol glycosides: adopt methanol eddy to extract, extract is successively with ethyl acetate, n-butanol extraction, macroporous adsorbent resin column chromatography is passed through at the n-butanol extraction position, with water, methanol-eluted fractions, again with the methanol-eluted fractions position through polyamide column chromatography, with water, methanol-eluted fractions, collect meoh eluate, concentrate, get the total glycosides enriched substance of phenylethyl alcohol.This method operation is loaded down with trivial details, solvent-oil ratio is big, energy consumption is high, and has used solvents such as ethyl acetate, propyl carbinol and methyl alcohol, has potential safety hazard, also causes the pollution of target compound simultaneously easily, only is applicable to prepared in laboratory.
Patent CN1268341C discloses a kind of method of suitability for industrialized production benzyl carbinol glycosides, mainly comprises three steps, the first step: solvent extraction (adopt the contour polarity solvent of water-pure system to extract, extracting solution is concentrated into certain weight proportion, and is standby); Second step: alcohol precipitation (extract concentrated solution is added high concentration ethanol, and fully vibration is left standstill, and filters, and filtrate concentrates, and must extract medicinal extract); The 3rd step: column chromatography purification (will extract medicinal extract and be dissolved in water, last macroporous adsorptive resins, with water-pure system gradient elution, collection contains the benzyl carbinol glycosides flow point).But this kind method solvent-oil ratio is big, cost is high, the production cycle is long, productive rate is relatively low, and has certain potential safety hazard.
Membrane separation technique (Membrane Separation Technique) j is an emerging high efficient separation technology, though the application in the field of Chinese medicines is just at the early-stage, has some and uses this technology successfully to extract the example of effective constituent in the enrichment Chinese medicine.Have not yet to see the research report of benzyl carbinol glycosides in the using membrane separating technology extraction separation Herba Cistanches.
Mainly contain chemical ingredientss such as phenylethyl alcohol glycoside, iridoid glycosides, lignanoids, alkaloids, glycitols, amino acids, polysaccharide and protein in the Herba Cistanches, wherein the higher compound of content has N.F,USP MANNITOL (Mw 182), trimethyl-glycine (Mw 117), phenylethyl alcohol glycoside (Mw 420～800), amino acids (Mw＜200), polysaccharide (Mw＞5000) and protein (Mw＞5000).Verbascoside (Acteoside, Mw 624) and echinacoside (Echinacoside, Mw 786) be the higher benzyl carbinol glycosides compound of content in the Herba Cistanches, domestic with the leading indicator of these 2 kinds of compositions as the evaluation quality of medicinal material, require the content of verbascoside in the Herba Cistanches extract high as far as possible in the international market, so they are major objective compositions of industrial production benzyl carbinol glycosides compound.From above data as can be seen, our desired target component molecular weight is between 600～800, and main impurity component can be divided into macromolecular substance (Mw＞5000) and small-molecule substance (Mw＜200) two big classes, the molecular weight boundary of target component and major impurity composition is obvious, shows that the benzyl carbinol glycosides composition in the Herba Cistanches is to be suitable for very much membrane separation technique to extract purifying.
Summary of the invention
The purpose of this invention is to provide a kind of raw material that contains benzyl carbinol glycosides that modern membrane separation technique is produced of using from Herba Cistanches; The present invention also provides a kind of using membrane separating technology to produce the method that contains the benzyl carbinol glycosides compounds simultaneously from Herba Cistanches.
The raw material that contains benzyl carbinol glycosides that using membrane separating technology of the present invention obtains from Herba Cistanches is characterized in containing in the described raw material verbascoside＞40%.
Also contain in the above-mentioned raw material that contains benzyl carbinol glycosides that from Herba Cistanches, obtains echinacoside (Echinacoside), different verbascoside (Isoacteoside), 2 '-ethanoyl verbascoside (2 '-Acetylacteoside), among pipe flower glycosides B (Tubuloside B), the boschnaloside A (Cistanoside A) one or more.
Above-mentioned Herba Cistanches is the plant that Herba Cistanches belongs to, comprise among Desert Herba Cistanches Cistanche deserticola Y.C.Ma, Cistanche Tubulosa Cistanche tubulosa (Schenk) Wight, the Saline Cistanche Herb Cistanche salsa G.Beck one or more, be preferably Cistanche Tubulosa or Saline Cistanche Herb; Material is selected the Herba Cistanches chylocaulous, preferably is not unearthed or the just unearthed part of not blooming.
The method of the raw material that contains benzyl carbinol glycosides that using membrane separating technology of the present invention is produced from Herba Cistanches is characterized in obtaining the benzyl carbinol glycosides enriched substance from the Herba Cistanches plant, and its step is as follows:
Step 1: choose clean Herba Cistanches chylocaulous and pulverizing as processing raw material;
Above-mentioned steps 1 selected Herba Cistanches is preferably is not unearthed or the just unearthed Herba Cistanches chylocaulous of not blooming;
In step 2: Yi Shui, water-low-carbon alcohol or water-low-carbon (LC) ketone one or more are as solvent, and get solvent and Herba Cistanches is processed raw material to dissolve extract and filter with Herba Cistanches 3～20 times of weight that process raw material, and collect to see through liquid and get filtrate;
Above-mentioned steps 2 is described be extracted as that decoction, refluxing extraction, diacolation are extracted, dipping extracts or supersound extraction in a kind of, be preferably supersound extraction.
Above-mentioned steps 2 preferably repeats 2～5 times, adds solvents by process raw material 3～10 times of weight of Herba Cistanches at every turn;
Step 3: step 2 gained filtrate is centrifugal or leave standstill and remove insolubles and get supernatant liquor;
Above-mentioned steps 3 is described centrifugally to be 500～20000 rev/mins and to get through liquid in centrifugal 2 minutes～1 hour, and described leaving standstill to leaving standstill got supernatant liquor after 1～48 hour;
Step 4: step 3 gained solution is got through liquid by the separation of microfiltration membrane separation system, remove submicron, particulate, flocks and most microorganism, described microfiltration membrane separation system is the microfiltration membrane of aperture 0.1～1 μ m, working pressure 0.01～0.5MPa, 20～70 ℃ of temperature;
The filter membrane of the microfiltration membrane separation system of above-mentioned steps 4 is preferably the inorganic ceramic film in 0.1～0.5 μ m aperture, and working pressure is 0.1～0.5MPa, 40～70 ℃ of solution temperatures;
Step 5, step 4 gained is seen through liquid to be got through liquid by the separation of ultra-filtration membrane separation system, remove soluble large molecule impurity such as polysaccharide, phlegmatic temperament, protein, described ultra-filtration membrane separation system is the ultra-filtration membrane of aperture 0.01～0.2 μ m, working pressure 0.2～2MPa, 20～70 ℃ of solution temperatures;
The ultra-filtration membrane molecular weight cut-off of the ultra-filtration membrane separation system of above-mentioned step 5 is greater than 5000, and working pressure is 1～2MPa, and solution temperature is 40～70 ℃;
Step 6; Above-mentioned steps 5 gained are seen through liquid carry out the nanofiltration purge process by the nanofiltration membrane separation system and get trapped substance, described nanofiltration membrane separation system is aperture 1～10nm nanofiltration membrane, and working pressure is 2～4MPa, 20～70 ℃ of solution temperatures;
It is 300～1000 that the nanofiltration membrane of the nanofiltration membrane separation system of above-mentioned steps 6 is preferably molecular weight cut-off, working pressure 3～4MPa, 40～70 ℃ of solution temperatures;
Step 7: drying.
The drying means of above-mentioned steps 7 can or vacuumize a kind of in the drying under reduced pressure for spraying drying, lyophilize, microwave vacuum cryodrying, dehydrates to moisture content≤9%.Described drying is preferably the microwave vacuum cryodrying.
Get and adopt the resulting Herba Cistanches extracting solution of the technology of the present invention route, with reference to " Chinese pharmacopoeia an appendix of version (VID) in 2005 test high performance liquid chromatography, with verbascoside and echinacoside (from Saline Cistanche Herb, separate making, UV, IR, EI-MS,
1HNMR,
13CNMR data fit bibliographical information value, content is measured purity greater than 97% through the HPLC area normalization method) carry out the external standard method quantitative analysis for reference substance, obtain the content of contained main effective constituent verbascoside and echinacoside in the Herba Cistanches, with measurement result and traditional technology method water extract-alcohol precipitation-macroporous adsorbent resin column chromatography method contrast.The result shows, verbascoside that adopts processing technology routine of the present invention to extract from Herba Cistanches to obtain and echinacoside are greatly improved than the rate of transform of traditional extraction technique, and dried cream productive rate has generally had to a certain degree reduction than traditional technology, the benzyl carbinol glycosides position that further specifies in the Herba Cistanches has obtained effective enrichment, prove the advance and the feasibility of present technique route, opened up new approach for the extraction of phenylethyl alcohol glycoside chemical ingredients in the Cistanche Hoffmgg. et Link plants is refining.
The benzyl carbinol glycosides of using in the inventive method extraction enrichment Herba Cistanches mainly has following superiority:
1, production process of the present invention mainly adopts membrane separating method to finish, and has improved target component benzyl carbinol glycosides retention rate, has removed most of invalid components, and the product activity composition has obtained effective enrichment;
2, microfiltration membrane separation system of the present invention has substituted traditional alcohol precipitation process, can save a large amount of ethanol, has reduced and has used increasing of security risk that ethanol causes and production cost, can also reduce ethanol simultaneously and reclaim required energy consumption, and then shorten the production cycle;
3, nanofiltration membrane separation of the present invention system also is the concentration process that a low temperature does not have phase transformation when holding back target substance, has reduced the concentrate drying time, has reduced energy consumption;
4, the present invention has higher selectivity to isolating target component, can change the specification and the operational condition of filter membrane according to the requirement of market to product, thereby the target substance of controlling products obtained therefrom is easily formed.
5, the mode of the present invention's preferred supersound extraction when extracting, utilize the special strong longitudinal vibration of ultrasonic wave, physicalies such as high speed impact fragmentation are destroyed the extract cellularstructure, make solvent can infiltrate cell interior, thereby quicken the dissolving of effective ingredient, under the prerequisite of the structure that does not change effective ingredient, improve the extraction rate of effective ingredient, also can shorten extraction time greatly.
6, the present invention is to the preferred microwave vacuum cryodrying of the drying mode of gained benzyl carbinol glycosides enriched substance, this technology is development and coming on the further investigation basis of water migration process under exchange of the physical change of material in to drying process, inside and outside caloic and the vacuum condition, belongs to the microwave heating category.Microwave and material are directly had an effect, its inside and outside is heated simultaneously, need not or transmit heat by convection current, have that rate of heating is fast, drying efficiency is high, dry mass is good, do not destroy advantages such as heat-sensitive materials, owing to all right kill vegetative forms of bacteria of microwave radiation, fungi, virus and bacterial spore pathogen etc., therefore played dual function dry and that sterilize simultaneously.
In sum, the rate of transform of the effective constituent of extracting from Herba Cistanches with method of the present invention is greatly improved, and dried cream productive rate has had to a certain degree reduction, activeconstituents in the Herba Cistanches has obtained effective enrichment, under the prerequisite of the structure that does not change effective ingredient, improved the extraction rate of effective ingredient greatly, and shortened process cycle, reduced energy consumption and production cost, quality product increases substantially.
Embodiment
Embodiment 1
1, gets the drying tube flower herba cistanches chylocaulous of removing impurity, be cut into small pieces, pulverized 840 μ m aperture sieve as processing raw material;
2, with the ethanol of concentration 70% as solvent, and get solvent to process raw material heating and refluxing extraction 2 hours of Herba Cistanches with the Herba Cistanches 18 times of weight that process raw material, then with 8 times of amount 70% alcohol reflux 2 times, each 1 hour;
3, merge said extracted liquid, be evaporated to relative density 1.08, insert in the whizzer centrifugal in 5000 rev/mins of following centrifugal treating 0.3 hour, collect supernatant liquor;
4, by the micro-filtration alumina-ceramic membrane filtration of aperture 0.25 μ m, 25 ℃ of working pressure 0.3MPa, temperature are removed submicron, particulate, flocks and most microorganism;
5, with the ultrafiltration alumina-ceramic membrane filtration that liquid passes through molecular weight cut-off 6000 that sees through of step 4 gained, 25 ℃ of working pressure 1.8MPa, temperature are removed soluble large molecule impurity such as polysaccharide, phlegmatic temperament, protein;
6, the liquid that sees through with step 5 gained is that 300 nanofiltration polysulfones organic hybrid films is handled by filter opening footpath molecular weight cut-off, 30 ℃ of working pressure 3MPa, temperature, and the gained film is held back part and is the benzyl carbinol glycosides enriched substance;
7, with step 6 gained benzyl carbinol glycosides enriched substance 60 ℃ of temperature, constantly reduce pressure to boiling point and be dried to moisture content less than 5%, get dry extract.
Embodiment 2
1, gets the dry Saline Cistanche Herb chylocaulous of removing impurity, pulverized 420 μ m aperture sieve;
2, with water be solvent, and get solvent to process raw material in ultrasonic frequency to Herba Cistanches be supersound extraction 40 minutes under the 20KHz with the Herba Cistanches 10 times of weight that process raw material, inclining supernatant liquor as extracting solution, repeats to extract 2 times each 30 minutes time then again with 6 times of amount solvents;
3, step 2 gained extracting solution is merged, be evaporated to relative density 1.05, put in the whizzer 3000 rev/mins, centrifugal treating 0.5 hour is collected and is seen through liquid;
4, get step 3 and see through the micro-filtration alumina-ceramic membrane filtration of liquid by aperture 0.10 μ m, working pressure 0.4MPa, 20 ℃ of temperature;
5, get step 4 and see through liquid, by the ultrafiltration alumina-ceramic membrane filtration of molecular weight cut-off 5000, working pressure 1.5MPa, 40 ℃ of temperature;
6, step 5 gained being seen through liquid is 400 nanofiltration polysulfones organic hybrid films by filter opening footpath molecular weight cut-off, working pressure 3.5MPa, and 40 ℃ of temperature, film is held back part and is the benzyl carbinol glycosides enriched substance;
7, with above-mentioned benzyl carbinol glycosides enriched substance under pressure 0.04Mpa, be lower than 6% with frequency 350MHz microwave vacuum cryodrying to moisture content, get dry extract.
Embodiment 3:
1, gets dry Desert Herba Cistanches chylocaulous 200 weight parts of removing impurity, pulverized the 1mm aperture sieve;
2, with water be solvent, and get solvent to process raw material in ultrasonic frequency to Herba Cistanches be supersound extraction 40 minutes under the 40KHz with the Herba Cistanches 12 times of weight that process raw material, inclining supernatant liquor as extracting solution, repeats to extract 3 times each 30 minutes time then again with 5 times of amount solvents;
3, step 2 gained extracting solution is merged, be evaporated to relative density 1.05, put in the whizzer, collect and see through liquid with 10000 rev/mins of centrifugal treating 0.2 hour;
4 see through liquid with step 3 gained passes through to be the micro-filtration weisspiessglanz ceramic membrane filter of aperture 0.10 μ m, working pressure 0.5MPa;
5, step 4 gained seen through the ultrafiltration weisspiessglanz ceramic membrane filter of liquid by molecular weight cut-off 5500, working pressure 2.0MPa;
6, the liquid that sees through with step 5 gained is that 600 nanofiltration polysulfones organic hybrid films is handled by filter opening footpath molecular weight cut-off, and working pressure 4.0MPa holds back part and is the benzyl carbinol glycosides enriched substance;
7, benzyl carbinol glycosides enriched substance spraying drying to water content is lower than 7%, gets dry extract.
Embodiment 4:
1, gets and remove the drying tube flower herba cistanches chylocaulous that impurity is not bloomed, be crushed to particulate state less than 5mm as raw material;
2, Herba Cistanches is processed raw material as solvent with the process raw material water of 20 times of weight of the described Herba Cistanches of step 1, decoct extraction 1 hour down for 100 ℃ in temperature, filter with 840 μ m aperture sieve, collect filtrate, the water that filter residue is added again 10 times of weight decocted 30 minutes again, filtered and collect filtrate with 840 μ m aperture sieve;
3, step 2 gained filtrate is merged leave standstill after 10 hours and get supernatant liquor;
4, step 3 gained supernatant liquor is got through liquid with the separation of microfiltration membrane separation system, described microfiltration membrane separation system is the microfiltration membrane of aperture 0.15 μ m, working pressure 0.4MPa, 50 ℃ of temperature;
5, step 4 gained is seen through liquid and get through liquid by the separation of ultra-filtration membrane separation system, described ultra-filtration membrane separation system is the ultra-filtration membrane of aperture 0.1 μ m, working pressure 0.7MPa, 50 ℃ of solution temperatures;
6, will state step 5 gained and see through liquid and carry out the nanofiltration purge process by the nanofiltration membrane separation system and get trapped substance, described nanofiltration membrane separation system is that molecular weight cut-off is 550 nanofiltration membrane, and working pressure is 2.5MPa, 50 ℃ of solution temperatures;
7, spraying drying is to moisture content≤4%.
Embodiment 5:
1, choosing the Desert Herba Cistanches chylocaulous dry product of totally not blooming also pulverizes as raw material; Be crushed to particle diameter and also cross the 2mm aperture sieve as raw material less than 2mm;
2, with the ethanol of concentration 85% as solvent, and get solvent and Herba Cistanches is processed raw material flood extraction in 12 hours with the Herba Cistanches 12 times of weight that process raw material, collect supernatant liquor and get filtrate, repeat above-mentioned steps 2 times, add the solvents dipping 12 hours by process raw material 5 times of weight of Herba Cistanches at every turn, filter the removal insolubles with 300 μ m aperture sieve for the last time;
3, with step 2 gained filtrate, be evaporated to relative density 1.07, got through liquid in centrifugal 5 minutes at 1400 rev/mins;
4, step 3 gained solution is got through liquid with the separation of microfiltration membrane separation system, described microfiltration membrane separation system is the microfiltration membrane of aperture 1 μ m, working pressure 0.2MPa, 20 ℃ of temperature;
5, step 4 gained is seen through liquid and get through liquid by the separation of ultra-filtration membrane separation system, described ultra-filtration membrane separation system is the ultrafiltration weisspiessglanz ceramic membrane of aperture 0.15 μ m, working pressure 0.6MPa, 70 ℃ of solution temperatures;
6, above-mentioned steps 5 gained being seen through liquid is 2MPa with 5nm nanofiltration membrane, working pressure, and 20 ℃ of conditions of solution temperature are carried out the nanofiltration purge process and got trapped substance, get trapped substance;
7, with step 7 gained trapped substance under the 0.07MPa negative pressure, with frequency 300MHz microwave drying to moisture content≤5%.
Embodiment 6;
1, chooses the just unearthed part dry meat stem of not blooming of clean Cistanche Tubulosa, and pulverized 500 μ m aperture sieve as raw material;
2, with water as solvent, and get solvent Herba Cistanches processed raw material with 50KHz ultrasonication 20 minutes with the Herba Cistanches 14 times of weight that process raw material, collect supernatant liquor and get filtrate;
Repeat above-mentioned steps 3 times, add solvents by the Herba Cistanches 5 times of weight that process raw material at every turn, repeat the back for the last time with 250 μ m aperture sieve elimination insolubless;
3, step 2 gained filtrate decompression is concentrated into relative density 1.06, under 5000 rev/mins of rotating speeds, got through liquid in centrifugal 5 minutes;
4, step 3 gained is seen through the inorganic ceramic film of liquid 0.8 μ m in the aperture, working pressure 0.2MPa, temperature descended leaching to see through liquid for 30 ℃;
5, step 4 gained is seen through liquid at retaining molecular weight greater than 5000 ultra-filtration membrane, working pressure 2MPa filters under 60 ℃ of conditions of solution temperature, gets through liquid;
6, step 5 gained is seen through liquid by aperture 3nm nanofiltration membrane, working pressure is 2.5MPa, and 70 ℃ of solution temperatures are got trapped substance;
7, insert step 6 gained trapped substance under the 0.03Mpa pressure, be warmed up to boiling point and be dried to moisture content≤4%.
Embodiment 7:
1, chooses clean Saline Cistanche Herb dry meat stem and be crushed to the following particle of 2mm as raw material;
2, with water as solvent, and get solvent and Herba Cistanches is processed raw material handled 10 minutes with frequency 100KHz ultrasonic wave with the Herba Cistanches 5 times of weight that process raw material, filter with 300 μ m sieve, collect through liquid and get filtrate, repeat above-mentioned steps 5 times, add the solvent aftertreatment by the Herba Cistanches 5 times of weight that process raw material at every turn;
3, step 2 gained filtrate is merged, be evaporated to relative density 1.05, insert whizzer and got through liquid in centrifugal 3 minutes at 10000 rev/mins;
4, step 3 gained is seen through liquid 40 ℃ of filtrations of inorganic ceramic film, working pressure 0.1MPa, temperature with aperture 0.5 μ m;
5, step 4 gained is seen through liquid and cross leaching through liquid for 20 ℃ with ultra-filtration membrane, working pressure 1MPa, the solution temperature of aperture 0.1 μ m;
6, step 5 gained is seen through liquid by molecular weight cut-off be 450, working pressure 3MPa, solution temperature handle down for 50 ℃ and get trapped substance;
7, step 6 trapped substance is placed under the 0.08Mpa pressure be dried to moisture content≤3% by 500MHz frequency microwave dehydration.
Embodiment 8:
1, chooses clean Desert Herba Cistanches chylocaulous dry product, be crushed to the following particle of 800 μ m as raw material;
2, with water as solvent, and with Herba Cistanches process raw material 15 times of weight get solvent to Herba Cistanches process raw material decoct cross after 2 hours 180 μ m sieve filtrate, the insolubles that leaches adds solvents and continues to decoct and crossed 180 μ m sieve in 1 hour by process raw material 10 times of weight of Herba Cistanches again, filtrate;
3, leave standstill after 48 hours after step 2 gained filtrate is merged and get supernatant liquor;
4, with the microfiltration membrane of step 3 gained supernatant liquor with aperture 0.25 μ m, working pressure 0.5MPa, temperature is crossed leaching for 70 ℃ and is seen through liquid;
5, step 4 gained is seen through the ultra-filtration membrane of liquid by aperture 0.08 μ m, working pressure 1.2MPa, solution temperature is crossed leaching for 70 ℃ and is seen through liquid;
6, above-mentioned steps 5 gained being seen through liquid is 350 nanofiltration membrane by molecular weight cut-off, working pressure 3.5MPa, and solution temperature is crossed the leaching trapped substance for 70 ℃;
7, with step 6 gained trapped substance under 0.07Mpa pressure, be dried to moisture content≤3% with 400MHz frequency microwave dehydration.
Embodiment 9:
1, chooses clean Saline Cistanche Herb chylocaulous and to be crushed to particle diameter 4mm following as raw material;
2, with water as solvent, and get solvent Herba Cistanches processed raw material down with frequency 100KHz ultrasonication 20 minutes with the Herba Cistanches 8 times of weight that process raw material, filter with the 1mm sieve, collect and see through liquid and get filtrate;
Repeat above-mentioned steps 4 times, add solvents by the Herba Cistanches 3 times of weight that process raw material at every turn;
3, step 2 gained filtrate decompression is concentrated into relative density 1.10, insert whizzer with 4000 rev/mins centrifugal 5 minutes filtrate;
4, with the microfiltration membrane of filtrate on step 3 gained with aperture 1 μ m, working pressure 0.1MPa, temperature is filtered down for 25 ℃, gets through liquid;
5, step 4 gained being seen through liquid is 8000 ultra-filtration membrane by molecular weight cut-off, and working pressure is 1MPa, and solution temperature is 45 ℃ and filters down, gets through liquid;
6, above-mentioned steps 5 gained being seen through liquid is 500 nanofiltration membrane by molecular weight cut-off, and at working pressure 4MPa, solution temperature filters down for 45 ℃, gets trapped substance;
7, vacuumize drying under reduced pressure to moisture content≤5%.
Embodiment 10:
1, chooses the clean Cistanche Tubulosa chylocaulous dry product that is not unearthed, be crushed to granularity 0.5mm as raw material;
2, with water as solvent, and get solvent with the Herba Cistanches 8 times of weight that process raw material, be that 120KHz processes raw material to Herba Cistanches and handled 15 minutes in ultrasonic frequency, filter with 150 μ m sieve, get and see through liquid and get filtrate, repeat above-mentioned steps 4 times, add solvents by the Herba Cistanches 8 times of weight that process raw material at every turn;
3, step 2 gained filtrate is left standstill removed insolubles in 24 hours and get supernatant liquor;
4, with the microfiltration membrane of step 3 gained supernatant liquor with aperture 0.15 μ m, working pressure 0.3MPa, temperature is filtered down for 55 ℃, gets through liquid;
5, step 4 gained is seen through the ultra-filtration membrane of liquid by molecular weight cut-off 6000, working pressure is 2MPa, and solution temperature is 55 ℃ and filters down, gets through liquid;
6, above-mentioned steps 5 gained are seen through the nanofiltration membrane of liquid by molecular weight cut-off 300, working pressure 4MPa, trapped substance is got in 55 ℃ of filtrations of solution temperature;
7, step 6 trapped substance is lower than 3% by frequency 450MHz microwave drying to moisture content under 20 ℃ of temperature.
Claims (14)
1, the raw material that contains benzyl carbinol glycosides that a kind of using membrane separating technology is produced from Herba Cistanches is characterized in that containing in the described raw material verbascoside＞40%.
2, the raw material that contains benzyl carbinol glycosides that using membrane separating technology as claimed in claim 1 is produced from Herba Cistanches, it is characterized in that also containing in the described raw material that contains benzyl carbinol glycosides that from Herba Cistanches, obtains echinacoside (Echinacoside), different verbascoside (Isoacteoside), 2 '-ethanoyl verbascoside (2 '-Acetylacteoside), among pipe flower glycosides B (Tubuloside B), the boschnaloside A (Cistanoside A) one or more.
3, the raw material of from Herba Cistanches, producing as claim 1 or 2 described using membrane separating technologies that contains benzyl carbinol glycosides, it is characterized in that described Herba Cistanches is the plant that Herba Cistanches belongs to, comprise among Desert Herba Cistanches Cistanche deserticolaY.C.Ma, Cistanche Tubulosa Cistanche tubulosa (Schenk) Wight, the Saline Cistanche Herb Cistanche salsa G.Beck one or more.
The preparation method of the raw material that contains benzyl carbinol glycosides that 4, a kind of using membrane separating technology is produced from Herba Cistanches is characterized in that obtaining the benzyl carbinol glycosides enriched substance from the Herba Cistanches plant, and its step is as follows:
Step 1: choose clean Herba Cistanches chylocaulous and pulverizing as processing raw material;
In step 2: Yi Shui, water-low-carbon alcohol or water-low-carbon (LC) ketone one or more are as solvent, and get solvent and Herba Cistanches is processed raw material to dissolve extract and filter with Herba Cistanches 3～20 times of weight that process raw material, and collect to see through liquid and get filtrate;
Step 3: step 2 gained filtrate is centrifugal or leave standstill and remove insolubles and get supernatant liquor;
Step 4: step 3 gained solution is got through liquid by the separation of microfiltration membrane separation system, and described microfiltration membrane separation system is the microfiltration membrane of aperture 0.1～1 μ m, working pressure 0.01～0.5MPa, 20～70 ℃ of temperature;
Step 5: step 4 gained is seen through liquid get through liquid by the separation of ultra-filtration membrane separation system, described ultra-filtration membrane separation system is the ultra-filtration membrane of aperture 0.01～0.2 μ m, working pressure 0.2～2MPa, 20～70 ℃ of solution temperatures;
Step 6: above-mentioned steps 5 gained are seen through liquid carry out the nanofiltration purge process by the nanofiltration membrane separation system and get trapped substance, described nanofiltration membrane separation system is aperture 1～10nm nanofiltration membrane, and working pressure is 2～4MPa, 20～70 ℃ of solution temperatures;
Step 7: drying.
The preparation method of the raw material that contains benzyl carbinol glycosides that 5, using membrane separating technology as claimed in claim 4 is produced from Herba Cistanches is characterized in that the selected Herba Cistanches of step 1 is not for being unearthed or just being unearthed the Herba Cistanches chylocaulous of not blooming.
6, using membrane separating technology as claimed in claim 4 is produced the preparation method of the raw material that contains benzyl carbinol glycosides from Herba Cistanches, it is characterized in that described being extracted as of step 2 decoction, refluxing extraction, diacolation extracted, dipping extracts or supersound extraction in a kind of.
The preparation method of the raw material that contains benzyl carbinol glycosides that 7, using membrane separating technology as claimed in claim 4 is produced from Herba Cistanches is characterized in that described step 2 repeats 2～5 times, adds solvents by Herba Cistanches 3～10 times of weight that process raw material at every turn.
The preparation method of the raw material that contains benzyl carbinol glycosides that 8, using membrane separating technology as claimed in claim 4 is produced from Herba Cistanches, it is characterized in that step 3 described centrifugal be 500～20000 rev/mins centrifugal 2 minutes～1 hour.
9, using membrane separating technology as claimed in claim 4 is produced the preparation method of the raw material that contains benzyl carbinol glycosides from Herba Cistanches, it is characterized in that described the leaving standstill to leaving standstill of step 3 get supernatant liquor after 1～48 hour.
The preparation method of the raw material that contains benzyl carbinol glycosides that 10, using membrane separating technology as claimed in claim 4 is produced from Herba Cistanches, the filter membrane that it is characterized in that the microfiltration membrane separation system of step 4 is the inorganic ceramic film in 0.1～0.5 μ m aperture, working pressure is 0.1～0.5MPa, 40～70 ℃ of solution temperatures.
The preparation method of the raw material that contains benzyl carbinol glycosides that 11, using membrane separating technology as claimed in claim 4 is produced from Herba Cistanches, the ultra-filtration membrane molecular weight cut-off of ultra-filtration membrane separation system that it is characterized in that step 5 is greater than 5000, working pressure is 1～2MPa, and solution temperature is 40～70 ℃.
The preparation method of the raw material that contains benzyl carbinol glycosides that 12, using membrane separating technology as claimed in claim 4 is produced from Herba Cistanches, the nanofiltration membrane that it is characterized in that the described nanofiltration membrane separation of step 6 system is that molecular weight cut-off is 300～1000, working pressure 3～4MPa, 40～70 ℃ of solution temperatures.
The method of the raw material that contains benzyl carbinol glycosides that 13, using membrane separating technology as claimed in claim 4 is produced from Herba Cistanches, it is characterized in that the described drying means of step 7 is spraying drying, lyophilize, microwave vacuum cryodrying or vacuumizes a kind of in the drying under reduced pressure, dehydrates to moisture content≤9%.
14, the preparation method of the raw material of producing from Herba Cistanches as claim 4 or 13 described using membrane separating technologies that contains benzyl carbinol glycosides is characterized in that the described drying of step 7 is the microwave vacuum cryodrying.
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2007
- 2007-04-23 CN CNB2007101027567A patent/CN100503626C/en not_active Expired - Fee Related
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