CN101214281B - Method for producing cistanche salsa extract - Google Patents
Method for producing cistanche salsa extract Download PDFInfo
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- CN101214281B CN101214281B CN2007100328069A CN200710032806A CN101214281B CN 101214281 B CN101214281 B CN 101214281B CN 2007100328069 A CN2007100328069 A CN 2007100328069A CN 200710032806 A CN200710032806 A CN 200710032806A CN 101214281 B CN101214281 B CN 101214281B
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- herba cistanches
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- echinacoside
- monomeric compound
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- 241000336315 Cistanche salsa Species 0.000 title claims description 5
- 150000001875 compounds Chemical class 0.000 claims abstract description 110
- 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 abstract description 94
- 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 abstract description 94
- 229930182478 glucoside Natural products 0.000 claims abstract description 92
- 150000008131 glucosides Chemical class 0.000 claims abstract description 92
- 238000000034 method Methods 0.000 claims abstract description 66
- 238000001035 drying Methods 0.000 claims abstract description 65
- 238000005516 engineering process Methods 0.000 claims abstract description 49
- 238000000746 purification Methods 0.000 claims abstract description 47
- 102000004190 Enzymes Human genes 0.000 claims abstract description 33
- 108090000790 Enzymes Proteins 0.000 claims abstract description 33
- 239000011347 resin Substances 0.000 claims abstract description 28
- 229920005989 resin Polymers 0.000 claims abstract description 28
- 239000000463 material Substances 0.000 claims abstract description 23
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 16
- 230000001954 sterilising effect Effects 0.000 claims abstract description 7
- 238000004659 sterilization and disinfection Methods 0.000 claims abstract description 7
- 238000010521 absorption reaction Methods 0.000 claims abstract description 6
- 241000005787 Cistanche Species 0.000 claims description 212
- 241001530097 Verbascum Species 0.000 claims description 89
- 235000010599 Verbascum thapsus Nutrition 0.000 claims description 89
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 50
- 238000003801 milling Methods 0.000 claims description 39
- 239000000203 mixture Substances 0.000 claims description 38
- 239000012141 concentrate Substances 0.000 claims description 36
- 239000002994 raw material Substances 0.000 claims description 35
- 230000000694 effects Effects 0.000 claims description 29
- 238000004140 cleaning Methods 0.000 claims description 24
- 239000002002 slurry Substances 0.000 claims description 24
- 238000001816 cooling Methods 0.000 claims description 16
- 238000003825 pressing Methods 0.000 claims description 16
- 230000010354 integration Effects 0.000 claims description 15
- 238000001179 sorption measurement Methods 0.000 claims description 15
- 238000001914 filtration Methods 0.000 claims description 14
- 238000003556 assay Methods 0.000 claims description 13
- 239000007787 solid Substances 0.000 claims description 13
- 238000004321 preservation Methods 0.000 claims description 10
- 238000001694 spray drying Methods 0.000 claims description 10
- 238000001704 evaporation Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 7
- 241000308150 Orobanchaceae Species 0.000 claims description 6
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 claims description 6
- 241000336316 Cistanche tubulosa Species 0.000 claims description 5
- 238000007710 freezing Methods 0.000 claims description 5
- 241000985690 Cistanche sinensis Species 0.000 claims description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- 239000011780 sodium chloride Substances 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 241000336291 Cistanche deserticola Species 0.000 claims description 2
- 239000013543 active substance Substances 0.000 claims 3
- 238000000926 separation method Methods 0.000 abstract description 13
- -1 phenethyl alcohol glucoside compound Chemical class 0.000 abstract description 10
- 238000006555 catalytic reaction Methods 0.000 abstract description 6
- 230000015556 catabolic process Effects 0.000 abstract description 2
- 238000006731 degradation reaction Methods 0.000 abstract description 2
- 238000000605 extraction Methods 0.000 abstract description 2
- 239000011149 active material Substances 0.000 abstract 2
- 239000004480 active ingredient Substances 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 abstract 1
- 230000007547 defect Effects 0.000 abstract 1
- 238000005507 spraying Methods 0.000 abstract 1
- 230000009897 systematic effect Effects 0.000 abstract 1
- 239000000126 substance Substances 0.000 description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 18
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 15
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 12
- 239000003463 adsorbent Substances 0.000 description 12
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 12
- 239000007788 liquid Substances 0.000 description 11
- 239000006199 nebulizer Substances 0.000 description 9
- 229910052757 nitrogen Inorganic materials 0.000 description 9
- 229930182470 glycoside Natural products 0.000 description 8
- WRMNZCZEMHIOCP-UHFFFAOYSA-N 2-Phenylethanol Natural products OCCC1=CC=CC=C1 WRMNZCZEMHIOCP-UHFFFAOYSA-N 0.000 description 7
- 239000007921 spray Substances 0.000 description 7
- PHOQVHQSTUBQQK-SQOUGZDYSA-N D-glucono-1,5-lactone Chemical compound OC[C@H]1OC(=O)[C@H](O)[C@@H](O)[C@@H]1O PHOQVHQSTUBQQK-SQOUGZDYSA-N 0.000 description 6
- 238000005054 agglomeration Methods 0.000 description 6
- 230000002776 aggregation Effects 0.000 description 6
- 235000010323 ascorbic acid Nutrition 0.000 description 6
- 229960005070 ascorbic acid Drugs 0.000 description 6
- 239000011668 ascorbic acid Substances 0.000 description 6
- 235000010265 sodium sulphite Nutrition 0.000 description 6
- 239000010408 film Substances 0.000 description 4
- 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 description 4
- 235000015165 citric acid Nutrition 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 206010010774 Constipation Diseases 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 2
- 229930185474 acteoside Natural products 0.000 description 2
- FBSKJMQYURKNSU-ZLSOWSIRSA-N acteoside 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)O[C@@H](OCCC=2C=C(O)C(O)=CC=2)[C@@H]1O FBSKJMQYURKNSU-ZLSOWSIRSA-N 0.000 description 2
- FBSKJMQYURKNSU-UKQWSTALSA-N acteoside I Natural products C[C@@H]1O[C@H](O[C@@H]2[C@@H](O)[C@H](OCCc3ccc(O)c(O)c3)O[C@H](CO)[C@H]2OC(=O)C=Cc4ccc(O)c(O)c4)[C@H](O)[C@H](O)[C@H]1O FBSKJMQYURKNSU-UKQWSTALSA-N 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 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 description 2
- MRIFZKMKTDPBHR-XLOWEYQUSA-N 8-Epiiridotrial glucoside Chemical compound O([C@H]1[C@H]2[C@@H](C(=CO1)C=O)CC[C@H]2C)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O MRIFZKMKTDPBHR-XLOWEYQUSA-N 0.000 description 1
- 102000030523 Catechol oxidase Human genes 0.000 description 1
- 108010031396 Catechol oxidase Proteins 0.000 description 1
- 241000530105 Clerodendrum minahassae Species 0.000 description 1
- 102000016559 DNA Primase Human genes 0.000 description 1
- 108010092681 DNA Primase Proteins 0.000 description 1
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 1
- 102000005744 Glycoside Hydrolases Human genes 0.000 description 1
- 108010031186 Glycoside Hydrolases Proteins 0.000 description 1
- 201000004810 Vascular dementia Diseases 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- MRIFZKMKTDPBHR-UHFFFAOYSA-N boschnaloside Natural products CC1CCC(C(=CO2)C=O)C1C2OC1OC(CO)C(O)C(O)C1O MRIFZKMKTDPBHR-UHFFFAOYSA-N 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 150000002338 glycosides Chemical class 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 210000001624 hip Anatomy 0.000 description 1
- 238000007602 hot air drying Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 201000001881 impotence Diseases 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 210000000936 intestine Anatomy 0.000 description 1
- 229930182489 iridoid glycoside Natural products 0.000 description 1
- 150000008145 iridoid glycosides Chemical class 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 210000003127 knee Anatomy 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
- 230000002107 myocardial effect Effects 0.000 description 1
- 230000000324 neuroprotective effect Effects 0.000 description 1
- 210000000607 neurosecretory system Anatomy 0.000 description 1
- 229920001542 oligosaccharide Polymers 0.000 description 1
- 230000003071 parasitic effect Effects 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 239000006187 pill Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000009938 salting Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 239000003826 tablet Substances 0.000 description 1
- 230000001256 tonic effect Effects 0.000 description 1
Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Medicines Containing Plant Substances (AREA)
- Saccharide Compounds (AREA)
Abstract
The present invention provides a production method of cynamorlum extract full of echinacoside and veroascose glucoside monomeric compounds and other active materials with high yield extracted from fresh cynamorlum succulent stem. The production method is implemented through systematic integrated technology of cytoclasis, serous extraction, macroporous resin absorption, chromatography, separation and purification, high-temperature enzyme sterilization, spraying and drying, and other processes, so as to realize the manufacturing process from feeding the fresh cynamorlum to obtaining cynamorlum extract full of echinacoside, veroascose glucoside monomeric compounds and other active materials with high yield within 20 to 60 minutes. The present invention effectively overcomes the technical defect of serious degradation and loss of active ingredients of phenethyl alcohol glucoside compound caused by enzyme catalysis reaction of poor drying method of cynamorlum. In the obtained cynamorlum extract (calculated in dry materials), the productive rate of echinacoside monomeric compounds up to 1.9 to 7.0 percent and the content of echinacoside and veroascose glucoside monomeric compounds up to 20 to 70 percent.
Description
Technical field
The present invention relates to a kind of from Herba Cistanches high yield extract the production method of the Herba Cistanches extract be rich in echinacoside and mullein glucoside monomeric compound isoreactivity material.
Background technology
Chinese medicine Herba Cistanches (Herba Cistanches) is the chylocaulous that Orobanchaceae (Orobanchaceae) Herba Cistanches belongs to (CistancheHoffmg.et Link) parasitic for many years herbal dry zone scale leaf, is the traditional traditional tonic medicine of China.Beginning is stated from Shennong's Herbal, classifies as top gradely, has kidney-replenishing, benefiting essence-blood, effects such as loosening bowel to relieve constipation; Be used to treat impotence in male, infertilitas feminis, soreness of the waist and knees, muscles and bones is unable, the dryness of the intestine constipation.Modern age, pharmaceutical research showed, Herba Cistanches has pharmacological action widely, to the human body immunity improving function, regulated neuroendocrine system, reinforcing the kidney and supporting YANG and hypermnesis function, and defying age, effect such as myocardial preservation and neuroprotective is obviously.Discover that echinacoside that Herba Cistanches is rich in and mullein glucoside monomeric compound have significant curative effect to the treatment vascular dementia.
The research that separates the Herba Cistanches active component in recent years is very active, and modern study shows that the main active of Herba Cistanches is phenethyl alcohol glycosides, iridoid glycosides, lignanoid's glycoside, oligosaccharide esters and polyhydric alcohol etc.The chemical compound of phenethyl alcohol glycosides (PhenylethanoidGlycosides, Ph Gs) comprise boschnaloside, echinacoside (echinacosid), verbascoside (acteoside or acteoside), 2 '-acetyl group verbascoside isoreactivity material.And echinacoside and mullein glucoside monomeric compound are the higher phenethyl alcohol glycoside compounds of content in the Herba Cistanches chylocaulous, and these two kinds of representative active component are as the leading indicator of estimating the Herba Cistanches quality at present.
Fresh herba cistanches chylocaulous moisture surpasses 80% usually, and the course of processing is difficult for dry.Traditional diamond-making technique adopts the fresh herba cistanches chylocaulous placed under the sunlight always and dries, or shady and cool place dries in the shade, or dries behind the salting, or dries after the stripping and slicing, section etc., and technology falls behind, and dry run is very slow, short then two weeks, long then one to two moon.Discover that containing a large amount of K, Na, Ca, Fe etc. in the Herba Cistanches has the metal ion of activation, wherein K to the enzyme catalysis vigor
+Concentration is up to 0.3%～2.3%, Na
+Concentration is up to 0.1%～1.7%, Ca
2+Concentration is up to 0.03%～0.36%, Fe
3+Concentration is up to 0.005%～0.14%; Particularly there is abundant enzymes such as hydrolytic enzyme, glycoside hydrolase and polyphenol oxidase system in the fresh herba cistanches chylocaulous; The dried process is because undried Herba Cistanches is in bad dried environment such as moistening, damp and hot for a long time; And in the course of processing because of reasons such as physical damnifications; The enzyme that is activated causes active enzymic catalytic reaction rapidly and produces enzymatic browning, and the phenethyl alcohol glycoside compounds isoreactivity composition that causes Herba Cistanches to be rich in is hydrolyzed, degrades, transforms or synthetic new product at enzyme-catalyzed reaction.Testing result shows; Echinacoside and mullein glucoside monomeric compound content are very abundant in the fresh herba cistanches chylocaulous of just being unearthed; Usually at 13%～24.3% (in dry); But different processing modes reaches from the different desertliving cistanche sheet samples of collecting of the place of production, kind, host and collection season; Echinacoside and mullein glucoside monomeric compound content are merely 0.03%～1.0%, and the active component phenethyl alcohol glycoside compounds that Herba Cistanches is rich in conventional processes is by severely degrade, and wherein representative active component echinacoside and mullein glucoside monomeric compound attenuation rate are up to 92.31%～99.87%.Discover; Bad processing technique and drying method are that the primase catalytic reaction causes the active component phenethyl alcohol glycosides degradation loss that Herba Cistanches is rich in, particularly the key factor of two kinds of representative active component echinacoside and the loss of mullein glucoside monomeric compound severely degrade.
Summary of the invention
The purpose of this invention is to provide a kind of from the fresh herba cistanches chylocaulous high yield extract the Herba Cistanches extract production method be rich in echinacoside and mullein glucoside monomeric compound isoreactivity material.
The present invention proposes a kind of system integration technology of passing through; From the fresh herba cistanches chylocaulous; Effectively extract the production method of the Herba Cistanches extract that is rich in echinacoside and mullein glucoside monomeric compound isoreactivity material; Enforcement through system integration technologies such as cell breakage technology, serosity extraction process, macroporous resin adsorption and chromatography purifying technique, high temperature enzyme denaturing technology, drying process with atomizing; Technological process is short; Make water few, meet the environmental requirement of energy-saving and emission-reduction, be implemented in to accomplish in 20～60 minutes the fresh herba cistanches raw material is obtained the technology manufacture process that is rich in echinacoside and mullein glucoside monomeric compound isoreactivity material from the paramount productive rate that feeds intake as solvent and consumption; The phenethyl alcohol glycoside compounds isoreactivity composition that enzymic catalytic reaction caused of effectively containing, blocking and overcome the bad drying method initiation of common Herba Cistanches is significantly promoted the medical value of Herba Cistanches by the technological deficiency of severely degrade loss.
Method of the present invention is, selects the fresh herba cistanches chylocaulous, or adopts and place the fresh-keeping fresh herba cistanches chylocaulous of industrial freezer, or adopts the quick-freezing Herba Cistanches chylocaulous of industrial freezer cold preservation, or selects for use selected Herba Cistanches chylocaulous and particle as raw material.Place rinsing bowl to use cold rinse raw material, or with industrial pure water rinsing; After picking up, place common industrial breaker and milling device that the Herba Cistanches chylocaulous is broken and mill, make cell cracked; Broken and the process material of milling is controlled at low temperature environment below 20 ℃, also can adopt to charge into common food grade liquid nitrogen or CO
2, or add CO
2Frozen water also can add micro-food grade ascorbic acid, citric acid, gluconic acid lactone, sodium sulfite etc.; Herba Cistanches cell slurry after milling is adopted common industrial pressure filter filter pressing, or the industrial centrifugal machine separation, Herba Cistanches cell serosity obtained; Also can be with filtering residue through once extremely adding for several times the technical pure water purification; Or through the technical pure water purification of pre-cooling; Once to further grinding to form slurry through common industrial grinder for several times, again through industrial pressure filter filter pressing, or Herba Cistanches smudge cells cleaning mixture is obtained in the industrial centrifugal machine separation; Adopt common industrial instantaneous ultrahigh-temperature sterilization device technique, with Herba Cistanches cell serosity, or merging smudge cells cleaning mixture carries out the instantaneous enzyme denaturing of superhigh temperature; With Herba Cistanches cell serosity; Or merging smudge cells cleaning mixture; Or the Herba Cistanches extracting solution behind the instantaneous enzyme denaturing of superhigh temperature; Adopt common industrial macroporous resin adsorption and chromatography technology that echinacoside in the Herba Cistanches extract and mullein glucoside monomeric compound isoreactivity material are adsorbed purification, and, obtain the echinacoside and the mullein glucoside monomeric compound isoreactivity composition extracting solution of high concentration through further absorption and purification; Adopt common industrial vacuum concentration technology, or the thin film evaporation concentration technology, obtain solid content and be 25%～65% be rich in echinacoside and mullein glucoside monomeric compound isoreactivity substance concentrate; Through common industrial drying process with atomizing, or three sections drying process with atomizing dryings, and utilize high temperature drying steam the concentrate superhigh temperature instantaneous processed of atomizing to be made the effect of enzyme activity forfeiture and acquisition superhigh temperature instantaneous drying; Also can be through second section drying tower body dry section with the further dehydrate of powdered Herba Cistanches extract; Also can further cool off and the agglomeration pelletize powdered Herba Cistanches extract, to obtain to be the Herba Cistanches extract of fine granularity through the 3rd section dry section.Above system integration technology flow process was accomplished in 20～60 minutes; Through assay determination; In the Herba Cistanches extract of being gathered in the crops that is powdery or fine granularity (in dry); Representative active component echinacoside monomeric compound productive rate is up to 9.0%～18.8%, and the mullein glucoside monomeric compound productive rate is up to 1.9%～9.2%; Representative active component echinacoside and mullein glucoside monomeric compound content reach 20%～76.6% in the Herba Cistanches extract; Moisture is 0.5%～2.8%.
The inventive method is extracted is rich in echinacoside and mullein glucoside monomeric compound isoreactivity substance concentrate; Also can adopt usually the method for other industrially drying to obtain powder, like industrial cylinder dry, microwave vacuum drying, vacuum drying, microwave drying, lyophilization or hot air drying etc.
The fresh-keeping storehouse temperature of employing industry freezer that the inventive method relates to is 1 ℃～13 ℃, and best freezer fresh-keeping warehouse temperature is 4 ℃～10 ℃; Adopting the storehouse temperature of industrial freezer cold preservation is-52 ℃～-10 ℃, and the storehouse temperature of best freezer cold preservation is-36 ℃～-18 ℃; The cold water water temperature that places tank that adopts is 1 ℃～20 ℃, and best cold water water temperature is 4 ℃～10 ℃; That adopts charges into liquid nitrogen or CO in the Herba Cistanches raw material
2Concentration be 0.1%～5.0% (weight ratio), optium concentration is 0.5%～1% (weight ratio); That adopts adds CO in the Herba Cistanches raw material
2The frozen water amount is 1%～20% (weight ratio), CO
2CO in the frozen water
2Concentration is 0.1%～5.0% (weight ratio), CO
2The frozen water temperature is 1 ℃～20 ℃, CO
2The frozen water optimum temperature is 4 ℃～6 ℃, CO
2CO in the frozen water
2Optium concentration is 1%～2% (weight ratio); Ascorbic acid, citric acid, gluconic acid lactone, the sodium sulfite of the interpolation trace that adopts are food grade; Addition is 0.001%～0.03% (weight ratio); Optimum addition is 0.002%～0.004% (weight ratio), can select one or more for use; Adopt in filtering residue through once to adding for several times the technical pure water purification or being 10%～200% (weight ratio) through the addition of the technical pure water purification of pre-cooling; Optimum addition is 50%～100% (weight ratio); Technical pure water purification water temperature through pre-cooling is 1 ℃～20 ℃, and optimum water temperature is 4 ℃～10 ℃; The temperature that the industrial instantaneous ultrahigh-temperature sterilization device technique that adopts carries out the instantaneous enzyme denaturing of superhigh temperature is 135 ℃～141 ℃; The industrial vacuum concentration technology that adopts and the temperature of industrial film evaporating and concentrating process are 45 ℃～65 ℃; Macroporous adsorbent resin can be selected usually external commodity XAD for use; Diaion; SP; Posapak and Chromosorb and homemade commodity nonionic polymeric sorbent AB-8; CHA-III; CAD-40; D101; D301; D296; D396R; D4006; D4020; D3520; DA201; DM301; D130; GDX104; HPD100; HPD450; HPD500; HPD600; HPD8; H107; JD-KW; LD601; LD605; ME-1; ME-2; ME-3; NKA-2; NKA-9; R-A; S8; SIP; Commodity macroporous adsorbent resins such as WLD and X-5 type; It is 125 ℃～285 ℃ that the industrial drying process with atomizing that adopts, or three sections drying process with atomizing, drying tower superhigh temperature instantaneous processed make the temperature of the effect of enzyme activity forfeiture and acquisition superhigh temperature instantaneous drying, and best temperature is 190 ℃～230 ℃.
The Herba Cistanches that the present invention relates to is Orobanchaceae plant (Orobanchaceae) Herba Cistanches or claims Desert Herba Cistanches (Cistanchedeserticola Y.C.Ma), Cistanche Tubulosa (Cistanche tubulosa (Schrenk) R.Wight), spends one or more the Herba Cistanches chylocaulous of fresh band scale leaf in salt Herba Cistanches (Cistanche salsa var.albiflora P.F.Tu et Z.C.Lou), Saline Cistanche Herb (Cistanche salsa (C.A.Mey) G.Beck) and Herba Cistanches sinensis or the title C.sinensis G.Beck (Cistanche sinensis G.Beck) in vain; Or through the fresh-keeping fresh herba cistanches chylocaulous of freezer; Or the quick-freezing Herba Cistanches chylocaulous of freezer cold preservation, or select selected Herba Cistanches chylocaulous and particle for use.
The cistanche salsa extract that is powdery or fine granularity that the inventive method is produced; Can be directly as products such as raw material production capsule, tablet, granule, electuary, pill or teabag; Also can provide as medical material, or through further many kinds of extract and separate monomeric compound or extract.
The concrete steps of the inventive method comprise:
1, selects the fresh herba cistanches chylocaulous, or adopt and to place the fresh-keeping fresh herba cistanches chylocaulous of industrial freezer, or adopt the quick-freezing Herba Cistanches chylocaulous of industrial freezer cold preservation, or select for use selected Herba Cistanches chylocaulous and particle as raw material.
2, place rinsing bowl to use cold rinse the raw material of being selected for use, or, after picking up, place common industrial breaker and milling device with industrial pure water rinsing, the Herba Cistanches chylocaulous is broken and mill, make cell cracked; Broken and the process material of milling is controlled at low temperature environment below 20 ℃, also can adopt to charge into common food grade liquid nitrogen or CO
2, or add CO
2Frozen water also can add micro-food grade ascorbic acid, citric acid, gluconic acid lactone, sodium sulfite etc.
3, the Herba Cistanches cell slurry after will milling adopts common industrial pressure filter filter pressing, or industrial centrifugal machine separates, and obtains Herba Cistanches cell serosity; Also can be with filtering residue through once extremely adding for several times the technical pure water purification; Or through the technical pure water purification of pre-cooling, once to further grinding to form slurry through common industrial grinder for several times, again through industrial pressure filter filter pressing; Or the industrial centrifugal machine separation, obtain Herba Cistanches smudge cells cleaning mixture.
4, adopt common industrial instantaneous ultrahigh-temperature sterilization device technique, with Herba Cistanches cell serosity, or merging smudge cells cleaning mixture carries out the instantaneous enzyme denaturing of superhigh temperature;
5, with Herba Cistanches cell serosity; Or merging smudge cells cleaning mixture; Or the Herba Cistanches extracting solution behind the instantaneous enzyme denaturing of superhigh temperature; Adopt common industrial macroporous resin adsorption and chromatography technology that echinacoside in the Herba Cistanches extract liquid and mullein glucoside monomeric compound isoreactivity material are adsorbed purification, and obtain the echinacoside and the mullein glucoside monomeric compound isoreactivity composition extracting solution of high concentration through further absorption and purification.
6, adopt common industrial vacuum concentration technology, or the industrial film evaporating and concentrating process, obtain solid content and be 30%～60% be rich in echinacoside and mullein glucoside monomeric compound isoreactivity substance concentrate;
7, will be rich in echinacoside and mullein glucoside monomeric compound isoreactivity material extracting solution or concentrate; Adopt common industrial drying process with atomizing; Or three sections drying process with atomizing of industry carry out drying, and utilize high temperature drying steam that the concentrate superhigh temperature instantaneous processed of atomizing is made enzyme activity forfeiture and the temperature that obtains the effect of superhigh temperature instantaneous drying is 125 ℃～285 ℃; Also can be through second section drying tower body dry section with the further dehydrate of powdered Herba Cistanches extract; Also can cool off and the agglomeration pelletize through the 3rd section dry section, results are the Herba Cistanches extract of fine granularity again.
8, above system integration technology flow process was accomplished in 20～60 minutes; Through assay determination; In the Herba Cistanches extract of being gathered in the crops that is powdery or fine granularity (in dry); Representative active component echinacoside monomeric compound productive rate is up to 9.0%～18.8%, and the mullein glucoside monomeric compound productive rate is up to 1.9%～7.0%; Representative active component echinacoside and mullein glucoside monomeric compound content reach 20%～70% in the Herba Cistanches extract of results; Moisture is 0.5%～2.8%.
Also can adopt industrial macroporous resin adsorption and chromatography technology as required, further purify and improve the degree of echinacoside and mullein glucoside monomeric compound in the Herba Cistanches extract.
The percentage ratio of the various amounts that relate among the present invention (%) all is weight percentage.
The productive rate of representative active component echinacoside monomeric compound is the percentage ratio (in dry) of the amount and the raw material gross weight of contained echinacoside monomeric compound in the product in the product described in the present invention (Herba Cistanches extract of being gathered in the crops that is powdery or fine granularity).The productive rate of representative active component mullein glucoside monomeric compound is the percentage ratio (in dry) of the amount and the raw material gross weight of contained mullein glucoside monomeric compound in the product in the product.
The specific embodiment
Below in conjunction with embodiment the present invention is done further explain.
Embodiment one:
1, selects fresh Saline Cistanche Herb chylocaulous as raw material;
2, place rinsing bowl to use cold rinse raw material, the cold water water temperature is 2 ℃; After picking up, place common industrial breaker and milling device that the Herba Cistanches chylocaulous is broken and mill, make cell cracked; Broken and the technical process of milling charges into liquid nitrogen, and liquid nitrogen concentration is 0.5% (weight ratio) in the material; Recording temperature of charge is 15 ℃;
3, the Herba Cistanches cell slurry after will milling adopts common industrial centrifugal machine to separate, and obtains Herba Cistanches cell serosity;
4, adopt common industrial macroporous resin adsorption and chromatography technology that echinacoside in the Herba Cistanches extracting solution and mullein glucoside monomeric compound isoreactivity material are adsorbed purification in Herba Cistanches cell serosity, obtain the echinacoside and the mullein glucoside monomeric compound isoreactivity composition extracting solution of high concentration through further absorption and purification; And through the industrial vacuum concentration technology, temperature is 60 ℃, obtain solid content and be 40% be rich in echinacoside and mullein glucoside monomeric compound isoreactivity substance concentrate; The industrial macroporous adsorbent resin of selecting for use is the AB-8 type;
5, will be rich in echinacoside and mullein glucoside monomeric compound isoreactivity substance concentrate through three sections drying process with atomizing dryings; The dry tower body that connects at industrial spray drying tower nebulizer carries out drying through 280 ℃ of high temperature drying steam to the extract that atomizes, and utilizes the superhigh temperature instantaneous processed to make the effect of enzyme activity forfeiture and acquisition superhigh temperature instantaneous drying; Second section drying tower body dry section of warp cools off the further dehydrate of powdered Herba Cistanches extract and the agglomeration pelletize through the 3rd section dry section more then, to obtain to be the Herba Cistanches extract of fine granularity.
6, above system integration technology flow process was accomplished in 45 minutes; Through assay determination, in the Herba Cistanches extract of being gathered in the crops that is fine granularity (in dry), representative active component echinacoside monomeric compound productive rate is 15.9%, and the mullein glucoside monomeric compound productive rate is 4.1%; Representative active component echinacoside and mullein glucoside monomeric compound content are 50.1% in the Herba Cistanches extract; Moisture is 0.5%.
Embodiment two:
1, selects that to place the storehouse temperature be that the fresh-keeping fresh herba cistanches chylocaulous of 4 ℃ industrial freezer is as raw material;
2, with the fresh herba cistanches chylocaulous with industrial pure water rinsing, after picking up, place common industrial breaker and milling device that the Herba Cistanches chylocaulous is broken and mill, make cell cracked; Broken and the technical process of milling charges into CO
2Gas, CO in the Herba Cistanches raw material
2Concentration is 0.8% (weight ratio), and is added into 0.002% ascorbic acid of raw material weight, 0.002% gluconic acid lactone and 0.003% citric acid (weight ratio); Recording temperature of charge is 12 ℃;
3, the Herba Cistanches cell slurry after will milling adopts industrial centrifugal machine to separate, and obtains Herba Cistanches cell serosity, simultaneously with filtering residue through repeating to add 200% technical pure water purification (weight ratio) for three times through pre-cooling, water temperature is 4 ℃; Three repetitions further grind to form slurry through common industrial grinder, obtain Herba Cistanches smudge cells cleaning mixture through industrial pressure filter filter pressing again;
4, with after Herba Cistanches cell serosity and the merging of smudge cells cleaning mixture; Adopt common industrial macroporous resin adsorption and chromatography technology that echinacoside in the Herba Cistanches extracting solution and mullein glucoside monomeric compound isoreactivity material are adsorbed purification, obtain the echinacoside and the mullein glucoside monomeric compound isoreactivity composition extracting solution of high concentration through further absorption and purification; Through the industrial film evaporating and concentrating process, temperature is 50 ℃, obtain solid content and be 50% be rich in echinacoside and mullein glucoside monomeric compound isoreactivity substance concentrate; The industrial macroporous adsorbent resin of selecting for use is the D101 type;
5, will be rich in echinacoside and mullein glucoside monomeric compound isoreactivity substance concentrate; The dry tower body that connects at industrial spray drying tower nebulizer carries out drying through high temperature drying steam to the concentrate that atomizes; And utilize the superhigh temperature instantaneous processed to make enzyme activity forfeiture and the temperature that obtains the effect of superhigh temperature instantaneous drying is 180 ℃; Second section drying tower body dry section of warp obtains to be powdered Herba Cistanches extract with the further dehydrate of powdered Herba Cistanches extract again;
6, above system integration technology flow process was accomplished in 34 minutes; Through assay determination, that is gathered in the crops is (in dry) in the powdered Herba Cistanches extract, and representative active component echinacoside monomeric compound productive rate is 16.1%, and the mullein glucoside monomeric compound productive rate is 4.4%; Representative active component echinacoside and mullein glucoside monomeric compound content are 53.4% in the Herba Cistanches extract; Moisture is 1.3%.
Embodiment three:
1, adopt the quick-freezing of industrial freezer-52 ℃ cold preservation to spend salt Herba Cistanches chylocaulous in vain as raw material;
2, place rinsing bowl with industrial pure water rinsing raw material, after picking up, place common industrial breaker and milling device, the Herba Cistanches chylocaulous is broken and mill, make cell cracked; Broken and the technical process of milling is added 0.003% sodium sulfite (weight ratio); Recording temperature of charge is 5 ℃;
3, the Herba Cistanches cell slurry after will milling adopts common industrial pressure filter filter pressing, obtains Herba Cistanches cell serosity; Filtering residue is added 60% pure water (weight ratio), further grind to form slurry, separate through industrial centrifugal machine again and obtain Herba Cistanches smudge cells cleaning mixture through common industrial grinder;
4, adopt common industrial instantaneous ultrahigh-temperature sterilization device technique, with carrying out the instantaneous enzyme denaturing of superhigh temperature after Herba Cistanches cell serosity and the merging of smudge cells cleaning mixture, the temperature of the instantaneous enzyme denaturing of superhigh temperature is 190 ℃;
5, with the Herba Cistanches extracting solution behind the instantaneous enzyme denaturing of superhigh temperature; Adopt common industrial macroporous resin adsorption and chromatography technology that echinacoside in the Herba Cistanches extracting solution and mullein glucoside monomeric compound isoreactivity material are adsorbed purification, and further separation and purification obtain the echinacoside and the mullein glucoside monomeric compound isoreactivity composition extracting solution of high concentration; Through the industrial vacuum concentration technology, temperature is 65 ℃, obtain solid content and be 55% be rich in echinacoside and mullein glucoside monomeric compound isoreactivity substance concentrate; The industrial macroporous adsorbent resin of selecting for use is the D301 type;
6, will be rich in echinacoside and mullein glucoside monomeric compound isoreactivity substance concentrate; Dry tower body in industrial spray drying tower nebulizer connection; Through high temperature drying steam the concentrate that spray process atomizes is carried out drying, the temperature of superhigh temperature instantaneous drying is 225 ℃; Second section drying tower body dry section of warp is with the further dehydrate of powdered Herba Cistanches extract then; Through the 3rd section dry section powdered Herba Cistanches extract is cooled off and the agglomeration pelletize again, obtain to be the Herba Cistanches extract of fine granularity;
7, above system integration technology flow process was accomplished in 58 minutes; Through assay determination, in the Herba Cistanches extract of being gathered in the crops that is fine granularity (in dry), representative active component echinacoside monomeric compound productive rate is 17.2%, and the mullein glucoside monomeric compound productive rate is 3.9%; Representative active component echinacoside and mullein glucoside monomeric compound content are 59.2% in the Herba Cistanches extract; Moisture is 0.7%.
Embodiment four:
1, select for use selected Herba Cistanches chylocaulous and particle and Cistanche Tubulosa chylocaulous as raw material, ratio is 1: 2;
2, place rinsing bowl to use cold rinse the raw material of selecting for use, the cold water water temperature is 6 ℃, after picking up, places common industrial breaker and milling device, and the Herba Cistanches chylocaulous is broken and mill, and makes cell cracked; Broken and the technical process of milling adds the CO of 13% (weight ratio)
2Frozen water, CO
2CO in the frozen water
2Concentration is 2% (weight ratio), CO
2The frozen water temperature is 4 ℃; Recording temperature of charge is 18 ℃;
3, the Herba Cistanches cell slurry after will milling adopts industrial centrifugal machine to separate, and obtains Herba Cistanches cell serosity, simultaneously filtering residue is repeated to add 100% the technical pure water purification (weight ratio) through pre-cooling through secondary, and water temperature is 4 ℃; Secondary repeats further to grind to form slurry through common industrial grinder, obtains Herba Cistanches smudge cells cleaning mixture through industrial pressure filter filter pressing again;
4, with after Herba Cistanches cell serosity and the merging of smudge cells cleaning mixture; Adopt common industrial macroporous resin adsorption and chromatography technology that echinacoside in the Herba Cistanches extracting solution and mullein glucoside monomeric compound isoreactivity material are adsorbed purification, and further separation and purification obtain the echinacoside and the mullein glucoside monomeric compound isoreactivity composition extracting solution of high concentration; Through the industrial film evaporating and concentrating process, temperature is 55 ℃, obtain solid content and be 30% be rich in echinacoside and mullein glucoside monomeric compound isoreactivity substance concentrate; The industrial macroporous adsorbent resin of selecting for use is the AB-8 type;
5, will be rich in echinacoside and mullein glucoside monomeric compound isoreactivity substance concentrate; Dry tower body in industrial spray drying tower nebulizer connection; Through high temperature drying steam the concentrate of spray process atomizing is carried out drying, and utilize the superhigh temperature instantaneous processed to make the enzyme activity forfeiture and the temperature that obtains the effect of superhigh temperature instantaneous drying is 225 ℃; Second section drying tower body dry section of warp obtains to be powdered Herba Cistanches extract with the further dehydrate of powdered Herba Cistanches extract again.
6, above system integration technology flow process was accomplished in 60 minutes; Through assay determination, that is gathered in the crops is (in dry) in the powdered Herba Cistanches extract, and representative active component echinacoside monomeric compound productive rate is 15.9%, and the mullein glucoside monomeric compound productive rate is 1.92%; Representative active component echinacoside and mullein glucoside monomeric compound content are 49.3% in the Herba Cistanches extract; Moisture is 0.8%.
Embodiment five:
1, employing places the fresh-keeping fresh Saline Cistanche Herb chylocaulous of 10 ℃ of storehouse temperature of industrial freezer as raw material;
2, place rinsing bowl with 2 ℃ of cold rinse the raw material of selecting for use, after picking up, place common industrial breaker and milling device, the Herba Cistanches chylocaulous is broken and mill, make cell cracked; Broken and the technical process of milling is added 0.001% ascorbic acid and 0.003% gluconic acid lactone (weight ratio); Recording temperature of charge is 17 ℃;
3, the Herba Cistanches cell slurry after will milling adopts common industrial pressure filter filter pressing, obtains Herba Cistanches cell serosity, simultaneously filtering residue is added 80% the technical pure water purification (weight ratio) through pre-cooling, and water temperature is 5 ℃; Further grind to form slurry through common industrial grinder, separate through industrial centrifugal machine again and obtain Herba Cistanches smudge cells cleaning mixture;
4, adopt common industrial instantaneous ultrahigh-temperature sterilization device technique, with carrying out the instantaneous enzyme denaturing of superhigh temperature after Herba Cistanches cell serosity and the merging of smudge cells cleaning mixture, the temperature of the instantaneous enzyme denaturing of superhigh temperature is 139 ℃;
5, will be through the Herba Cistanches extracting solution liquid behind the instantaneous enzyme denaturing of superhigh temperature; Adopt common industrial macroporous resin adsorption and chromatography technology that echinacoside in the Herba Cistanches extracting solution and mullein glucoside monomeric compound isoreactivity material are adsorbed purification, and further separation and purification obtain the echinacoside and the mullein glucoside monomeric compound isoreactivity composition extracting solution of high concentration; Through the industrial vacuum concentration technology, temperature is 60 ℃, obtain solid content and be 48% be rich in echinacoside and mullein glucoside monomeric compound isoreactivity substance concentrate; The industrial macroporous adsorbent resin of selecting for use is the HPD100 type;
6, will be rich in echinacoside and mullein glucoside monomeric compound isoreactivity substance concentrate, dry through industrial vacuum, baking temperature is 55 ℃, obtains to be powdered Herba Cistanches extract.
7, above system integration technology flow process was accomplished in 40 minutes; Through assay determination, that is gathered in the crops is (in dry) in the powdered Herba Cistanches extract, and representative active component echinacoside monomeric compound productive rate is 18.2%, and the mullein glucoside monomeric compound productive rate is 7.0%; Representative active component echinacoside and mullein glucoside monomeric compound content are 70% in the Herba Cistanches extract; Moisture is 0.5%.
Embodiment six:
1, selects fresh Herba Cistanches sinensis chylocaulous as raw material;
2, place rinsing bowl with 3 ℃ of cold rinse raw material, after picking up, place common industrial breaker and milling device that the Herba Cistanches chylocaulous is broken and mill, make cell cracked; Broken and the technical process of milling charges into liquid nitrogen, and liquid nitrogen concentration is 3.0% (weight ratio) in the Herba Cistanches raw material; Recording temperature of charge is 15 ℃;
3, the Herba Cistanches cell slurry after will milling adopts common industrial pressure filter filter pressing; Obtain Herba Cistanches cell serosity; Simultaneously filtering residue is added 100% technical pure water purification (weight ratio) through pre-cooling; Water temperature is 5 ℃, further grinds to form slurry through common industrial grinder, obtains Herba Cistanches smudge cells cleaning mixture through industrial pressure filter filter pressing again;
4, with after Herba Cistanches cell serosity and the merging of smudge cells cleaning mixture; Adopt common industrial macroporous resin adsorption and chromatography technology that echinacoside in the Herba Cistanches extracting solution and mullein glucoside monomeric compound isoreactivity material are adsorbed purification, and further separation and purification obtain the echinacoside and the mullein glucoside monomeric compound isoreactivity composition extracting solution of high concentration; Through the industrial vacuum concentration technology, temperature is 45 ℃, obtain solid content and be 30% be rich in echinacoside and mullein glucoside monomeric compound isoreactivity substance concentrate; The industrial macroporous adsorbent resin of selecting for use is the HPD450 type;
5, will being rich in Herba Cistanches cell serosity, to adopt the thin film evaporation concentration technology to obtain solid content be 65% Herba Cistanches extract concentrate; Dry tower body in industrial spray drying tower nebulizer connection; Through high temperature drying steam the concentrate of spray process atomizing is carried out drying, and utilize the superhigh temperature instantaneous processed to make the enzyme activity forfeiture and the effect temperature that obtains the superhigh temperature instantaneous drying is 225 ℃; Acquisition is powdered Herba Cistanches extract.
6, above system integration technology flow process was accomplished in 20 minutes; Through assay determination, that is gathered in the crops is (in dry) in the powdered Herba Cistanches extract, and representative active component echinacoside monomeric compound productive rate is 18.1%, and the mullein glucoside monomeric compound productive rate is 4.1%; Representative active component echinacoside and mullein glucoside monomeric compound content are 59.3% in the Herba Cistanches extract; Moisture is 2.8%.
Embodiment seven:
1, select for use selected Herba Cistanches chylocaulous and particle as raw material;
2, place rinsing bowl with 2 ℃ of cold rinse raw material, after picking up, place common industrial breaker and milling device that the Herba Cistanches chylocaulous is broken and mill, make cell cracked; Broken and the technical process of milling charges into CO
2, CO
2Concentration is 4.0% (weight ratio); Broken and the technical process of milling is added into the citric acid of raw material weight 0.002% and 0.001% sodium sulfite (weight ratio); Recording temperature of charge is 15 ℃;
3; Herba Cistanches cell slurry after milling is adopted common industrial pressure filter filter pressing; Obtain Herba Cistanches cell serosity; Simultaneously with filtering residue through repeating to add 90% technical pure water purification (weight ratio) for three times through pre-cooling; Water temperature is 6 ℃, and three repetitions further grind to form slurry through common industrial grinder, obtain Herba Cistanches smudge cells cleaning mixture through industrial pressure filter filter pressing again;
4, with after Herba Cistanches cell serosity and the merging of smudge cells cleaning mixture; Adopt common industrial macroporous resin adsorption and chromatography technology that echinacoside in the Herba Cistanches extracting solution and mullein glucoside monomeric compound isoreactivity material are adsorbed purification, and further separation and purification obtain the echinacoside and the mullein glucoside monomeric compound isoreactivity composition extracting solution of high concentration; Through the industrial vacuum concentration technology, temperature is 55 ℃, obtain solid content and be 30% be rich in echinacoside and mullein glucoside monomeric compound isoreactivity substance concentrate; The industrial macroporous adsorbent resin of selecting for use is the HPD500 type;
5, will be rich in echinacoside and mullein glucoside monomeric compound isoreactivity substance concentrate; Dry tower body in industrial spray drying tower nebulizer connection; Through high temperature drying steam the concentrate of spray process atomizing is carried out drying, and utilize the superhigh temperature instantaneous processed to make the enzyme activity forfeiture and the temperature that obtains the effect of superhigh temperature instantaneous drying is 220 ℃; Second section drying tower body dry section of warp is with the further dehydrate of powdered Herba Cistanches extract then; Through the 3rd section dry section powdered Herba Cistanches extract is cooled off and the agglomeration pelletize again, obtain to be the Herba Cistanches extract of fine granularity;
6, above system integration technology flow process was accomplished in 60 minutes; Through assay determination, in the Herba Cistanches extract of being gathered in the crops that is fine granularity (in dry), representative active component echinacoside monomeric compound productive rate is 17.5%, and the mullein glucoside monomeric compound productive rate is 0.8%; Representative active component echinacoside and mullein glucoside monomeric compound content are 38.2% in the Herba Cistanches extract; Moisture is 0.6%.
Embodiment eight:
1, employing places 8 ℃ of fresh-keeping fresh herba cistanches chylocaulouss of industrial freezer as raw material;
2, place rinsing bowl with 5 ℃ of cold rinse the raw material of being selected for use, after picking up, place common industrial breaker and milling device, the Herba Cistanches chylocaulous is broken and mill, make cell cracked; Broken and the technical process of milling charges into liquid nitrogen, and liquid nitrogen concentration is 2.50% (weight ratio); Broken and the technical process of milling are added the sodium sulfite (weight ratio) of 0.002% ascorbic acid, 0.001% gluconic acid lactone and 0.002%; Recording temperature of charge is 18 ℃;
3, the Herba Cistanches cell slurry after will milling adopts common industrial centrifugal machine to separate, and obtains Herba Cistanches cell serosity, and filtering residue is added 80% the pure water through pre-cooling (weight ratio), and water temperature is 4 ℃; Further grind to form slurry through common industrial grinder, obtain Herba Cistanches smudge cells cleaning mixture through industrial pressure filter filter pressing or industrial centrifugal machine separation again;
4, with after Herba Cistanches cell serosity and the merging of smudge cells cleaning mixture; Adopt common industrial macroporous resin adsorption and chromatography technology that echinacoside in the Herba Cistanches extracting solution and mullein glucoside monomeric compound isoreactivity material are adsorbed purification, and further separation and purification obtain the echinacoside and the mullein glucoside monomeric compound isoreactivity composition extracting solution of high concentration; Through the industrial vacuum concentration technology, temperature is 60 ℃, obtain solid content and be 40% be rich in echinacoside and mullein glucoside monomeric compound isoreactivity substance concentrate; The industrial macroporous adsorbent resin of selecting for use is the HPD600 type;
5, will be rich in echinacoside and mullein glucoside monomeric compound isoreactivity substance concentrate; Dry tower body in industrial spray drying tower nebulizer connection; Through high temperature drying steam the concentrate of spray process atomizing is carried out drying, and utilize the superhigh temperature instantaneous processed to make the enzyme activity forfeiture and the temperature that obtains the effect of superhigh temperature instantaneous drying is 150 ℃; Second section drying tower body dry section of warp obtains to be powdered Herba Cistanches extract with the further dehydrate of powdered Herba Cistanches extract again;
6, above system integration technology flow process was accomplished in 35 minutes; Through assay determination, that is gathered in the crops is (in dry) in the powdered Herba Cistanches extract, and representative active component echinacoside monomeric compound productive rate is 16.8%, and the mullein glucoside monomeric compound productive rate is 3.2%; Representative active component echinacoside and mullein glucoside monomeric compound content are 36.2% in the Herba Cistanches extract; Moisture is 0.95%.
Embodiment nine:
1, selected Herba Cistanches chylocaulous and particle are as raw material;
2, place rinsing bowl with 3 ℃ of cold rinse raw material, after picking up, place common industrial breaker and milling device, the Herba Cistanches chylocaulous is broken and mill, make cell cracked; Recording temperature is 16 ℃;
3, the Herba Cistanches cell slurry after will milling adopts common industrial pressure filter filter pressing, obtains Herba Cistanches cell serosity;
4, adopt common industrial macroporous resin adsorption and chromatography technology that echinacoside in the Herba Cistanches extracting solution and mullein glucoside monomeric compound isoreactivity material are adsorbed purification in Herba Cistanches cell serosity; And the echinacoside and the mullein glucoside monomeric compound isoreactivity composition extracting solution of further separation and purification acquisition high concentration, the industrial macroporous adsorbent resin of selecting for use is the HPD8 type;
5, will be rich in echinacoside and mullein glucoside monomeric compound isoreactivity substance concentrate; Dry tower body in industrial spray drying tower nebulizer connection; Through high temperature drying steam the concentrate that spray process atomizes is carried out drying; And utilize the superhigh temperature instantaneous processed to make enzyme activity forfeiture and the temperature that obtains the effect of superhigh temperature instantaneous drying is 125 ℃, obtain to be powdered Herba Cistanches extract.
6, above system integration technology flow process was accomplished in 20 minutes; Through assay determination, in the Herba Cistanches extract of being gathered in the crops that is fine granularity (in dry), representative active component echinacoside monomeric compound productive rate is 9.0%, and the mullein glucoside monomeric compound productive rate is 3.1%; Representative active component echinacoside and mullein glucoside monomeric compound content are 20% in the Herba Cistanches extract; Moisture is 2.8%.
Embodiment ten:
1, selects fresh tube flower herba cistanches chylocaulous as raw material;
2, place rinsing bowl with 4 ℃ of cold rinse the raw material of being selected for use, after picking up, place common industrial breaker and milling device, the Herba Cistanches chylocaulous is broken and mill, make cell cracked; Recording temperature of charge is 18 ℃;
3, the Herba Cistanches cell slurry after will milling adopts common industrial centrifugal machine to separate, and obtains Herba Cistanches cell serosity, and filtering residue is added 40% the pure water through pre-cooling (weight ratio), and water temperature is 5 ℃; Further grind to form slurry through common industrial grinder, separate through industrial centrifugal machine again, obtain Herba Cistanches smudge cells cleaning mixture;
4, with after Herba Cistanches cell serosity and the merging of smudge cells cleaning mixture; Adopt common industrial macroporous resin adsorption and chromatography technology that echinacoside in the Herba Cistanches extracting solution and mullein glucoside monomeric compound isoreactivity material are adsorbed purification; And further separation and purification obtains the echinacoside and the mullein glucoside monomeric compound isoreactivity composition extracting solution of high concentration; Through the industrial vacuum concentration technology; Temperature is 45 ℃, obtain solid content and be 56% be rich in echinacoside and mullein glucoside monomeric compound isoreactivity substance concentrate; The industrial macroporous adsorbent resin of selecting for use is the HPDD101 type;
5, will be rich in echinacoside and mullein glucoside monomeric compound isoreactivity substance concentrate; The dry tower body that connects at industrial spray drying tower nebulizer carries out drying to the concentrate of spray process atomizing and utilizes the superhigh temperature instantaneous processed to make the enzyme activity forfeiture and the temperature that obtains the effect of superhigh temperature instantaneous drying is 175 ℃ through high temperature drying steam; Second section drying tower body dry section of warp is with the further dehydrate of powdered Herba Cistanches extract then; Through the 3rd section dry section powdered Herba Cistanches extract is cooled off and the agglomeration pelletize again, obtain to be the Herba Cistanches extract of fine granularity.
6, above system integration technology flow process was accomplished in 46 minutes; Through assay determination, in the Herba Cistanches extract of being gathered in the crops that is fine granularity (in dry), representative active component echinacoside monomeric compound productive rate is 18.8%, and the mullein glucoside monomeric compound productive rate is 6.1%; Representative active component echinacoside and mullein glucoside monomeric compound content are 58.3% in the Herba Cistanches extract; Moisture is 0.55%.
Claims (7)
1. the production method of a Herba Cistanches extract is characterized in that the concrete steps of this method comprise:
(1) selects fresh herba cistanches chylocaulous, the quick-freezing Herba Cistanches chylocaulous that places the fresh-keeping fresh herba cistanches chylocaulous of industrial freezer, industrial freezer cold preservation or selected Herba Cistanches chylocaulous and particle as raw material;
(2) place rinsing bowl to use cold rinse the raw material of being selected for use; The cold water water temperature is 1 ℃～20 ℃, or with industrial pure water rinsing, after picking up; Place common industrial breaker and milling device; The Herba Cistanches chylocaulous is broken and mill, make cell cracked, brokenly be controlled at low temperature environment below 20 ℃ with the process material of milling;
(3) the Herba Cistanches cell slurry after will milling adopts common industrial pressure filter filter pressing, or industrial centrifugal machine separates, and obtains Herba Cistanches cell serosity; Perhaps with filtering residue through once to adding for several times the technical pure water purification or through the technical pure water purification of pre-cooling; Water temperature through the technical pure water purification of pre-cooling is 1 ℃～20 ℃; Once to further grinding to form slurry through common industrial grinder for several times; Again through industrial pressure filter filter pressing, or industrial centrifugal machine separates, and obtains Herba Cistanches smudge cells cleaning mixture;
(4) adopt common industrial instantaneous ultrahigh-temperature sterilization device technique, with Herba Cistanches cell serosity, or merge the smudge cells cleaning mixture and carry out the instantaneous enzyme denaturing of superhigh temperature, temperature is 135 ℃～141 ℃;
(5) will be through the Herba Cistanches extracting solution behind the instantaneous enzyme denaturing of superhigh temperature; Adopt common industrial macroporous resin adsorption and chromatography technology that echinacoside in the Herba Cistanches extracting solution and mullein glucoside monomeric compound active substance are adsorbed purification, and obtain to contain echinacoside and mullein glucoside monomeric compound active component extracting solution through further absorption and purification;
(6) adopt common industrial vacuum concentration technology, or the industrial film evaporating and concentrating process, obtain solid content and be 30%～60% contain echinacoside and mullein glucoside monomeric compound active substance concentrate; Described industrial vacuum concentration technology or industrial film evaporating and concentrating process temperature are 45 ℃～65 ℃;
(7) will contain echinacoside and mullein glucoside monomeric compound active substance concentrate; Adopt common industrial drying process with atomizing; Or three sections drying process with atomizing of industry carry out drying; And utilize high temperature drying steam to make enzyme activity lose and obtain the effect of superhigh temperature instantaneous drying to the concentrate superhigh temperature instantaneous processed of atomizing, temperature is 125 ℃～285 ℃;
(8) above system integration technology flow process was accomplished in 20～60 minutes; Through assay determination, in the Herba Cistanches extract of being gathered in the crops that is powdery or fine granularity, in dry, representative active component echinacoside monomeric compound productive rate reaches 9.0%～18.8%, and the mullein glucoside monomeric compound productive rate reaches 1.9%～7.0%; Representative active component echinacoside and mullein glucoside monomeric compound content reach 20%～70% in the Herba Cistanches extract; Moisture is 0.5%～2.8%.
2. according to the described method of claim 1; It is characterized in that the Herba Cistanches described in the step (1) is Orobanchaceae plant (Orobanchaceae) Herba Cistanches or claims Desert Herba Cistanches (Cistanche deserticola Y.C.Ma), Cistanche Tubulosa (Cistanche tubulosa (Schrenk) R.Wight), spends salt Herba Cistanches (Cistanche salsavar.albiflora P.F.Tu etZ.C.Lou), Saline Cistanche Herb (Cistanche salsa var.albiflora P.F.Tu etZ.C.Lou) and Herba Cistanches sinensis in vain or claim C.sinensis G.Beck (Cistanche sinensis G.Beck), selects one or more for use.
3. according to the described method of claim 1, it is characterized in that the fresh-keeping storehouse temperature of the industrial freezer described in the step (1) is 1 ℃～13 ℃; Adopting the storehouse temperature of industrial freezer cold preservation is-52 ℃～-10 ℃.
4. according to the described method of claim 1, it is characterized in that described in the step (3) in filtering residue through once to adding for several times the technical pure water purification or being 10%～200% weight ratio through the addition of the technical pure water purification of pre-cooling.
5. according to the described method of claim 1, it is characterized in that the fresh-keeping storehouse temperature of described industrial freezer is 4 ℃～10 ℃; The storehouse temperature of industry freezer cold preservation is-36 ℃～-18 ℃; The cold water water temperature that places tank is 4 ℃～10 ℃.
6. according to the described method of claim 1, it is characterized in that described in the step (3) in filtering residue through one to adding for several times the technical pure water purification or being 50%～100% weight ratio through the addition of the technical pure water purification of pre-cooling; Water temperature through the technical pure water purification of pre-cooling is 4 ℃～10 ℃.
7. according to the described method of claim 1, it is characterized in that it is 190 ℃～230 ℃ that the spray drying superhigh temperature instantaneous processed described in the step (7) makes the temperature of the effect of enzyme activity forfeiture and acquisition superhigh temperature instantaneous drying.
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| CN101629200B (en) * | 2009-08-04 | 2012-01-11 | 中山大学 | Method for producing acteoside by fresh herba cistanches |
| CN101654692B (en) * | 2009-08-04 | 2011-12-21 | 中山大学 | Method for producing mullein glucoside monomeric compound |
| CN101629198B (en) * | 2009-08-04 | 2011-12-21 | 中山大学 | Method for producing monomeric compounds of acteoside |
| CN101629197B (en) * | 2009-08-04 | 2011-11-16 | 中山大学 | Method for increasing content of acteoside in herba cistanches |
| CN103896997B (en) * | 2014-04-14 | 2016-07-06 | 青海伊纳维康生物科技有限公司 | The isolation and purification method of verbascoside in a kind of Herba Cistanches |
| CN104189099A (en) * | 2014-06-17 | 2014-12-10 | 新疆医科大学 | Application of cistanche phenylethanoid glycoside extractive to control altitude sickness |
| CN105272919B (en) * | 2015-11-12 | 2018-01-05 | 中国科学院过程工程研究所 | A kind of method that allantoin is prepared in the oligosaccharide syrup from saline cistanche |
| CN106692311A (en) * | 2016-12-23 | 2017-05-24 | 庆阳敦博科技发展有限公司 | Processing method of herba cistanche tablet |
| CN112826925B (en) * | 2021-04-12 | 2022-09-06 | 仕医堂(吉林)生物药业有限公司 | Traditional Chinese medicine liquid for treating osteoarticular diseases and preparation method thereof |
| CN114886944A (en) * | 2022-03-30 | 2022-08-12 | 内蒙古宏魁苁蓉产业股份有限公司 | Cistanche extraction method, product and application thereof |
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| CN1823914A (en) * | 2005-02-23 | 2006-08-30 | 阿瓦提县人民政府 | Processing technology of cistanche decocting pieces |
| CN101041677A (en) * | 2007-04-23 | 2007-09-26 | 和田帝辰医药生物科技有限公司 | Producing raw material containing benzyl carbinol glycosides from Cistanche deserticola by using membrane separation technique and preparation method thereof |
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