CN101214282A - Method for extracting active component from cistanche salsa - Google Patents
Method for extracting active component from cistanche salsa Download PDFInfo
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- CN101214282A CN101214282A CNA2007100328073A CN200710032807A CN101214282A CN 101214282 A CN101214282 A CN 101214282A CN A2007100328073 A CNA2007100328073 A CN A2007100328073A CN 200710032807 A CN200710032807 A CN 200710032807A CN 101214282 A CN101214282 A CN 101214282A
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- herba cistanches
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- cistanche
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- 238000000034 method Methods 0.000 title claims abstract description 72
- 241000336315 Cistanche salsa Species 0.000 title claims description 83
- 239000000284 extract Substances 0.000 claims abstract description 96
- 239000012528 membrane Substances 0.000 claims abstract description 90
- 238000005516 engineering process Methods 0.000 claims abstract description 63
- 238000001035 drying Methods 0.000 claims abstract description 55
- 102000004190 Enzymes Human genes 0.000 claims abstract description 36
- 108090000790 Enzymes Proteins 0.000 claims abstract description 36
- 150000001875 compounds Chemical class 0.000 claims abstract description 32
- 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 31
- 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 31
- 229930182478 glucoside Natural products 0.000 claims abstract description 30
- 150000008131 glucosides Chemical class 0.000 claims abstract description 30
- 239000000463 material Substances 0.000 claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 claims abstract description 10
- 230000001954 sterilising effect Effects 0.000 claims abstract description 7
- 238000004659 sterilization and disinfection Methods 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 241000005787 Cistanche Species 0.000 claims description 172
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 54
- 239000002994 raw material Substances 0.000 claims description 42
- 239000000203 mixture Substances 0.000 claims description 41
- 239000012141 concentrate Substances 0.000 claims description 40
- 238000003801 milling Methods 0.000 claims description 36
- 229930182470 glycoside Natural products 0.000 claims description 35
- 239000012535 impurity Substances 0.000 claims description 35
- -1 phenethyl alcohol glycoside compounds Chemical class 0.000 claims description 35
- WRMNZCZEMHIOCP-UHFFFAOYSA-N 2-Phenylethanol Natural products OCCC1=CC=CC=C1 WRMNZCZEMHIOCP-UHFFFAOYSA-N 0.000 claims description 33
- 230000000694 effects Effects 0.000 claims description 29
- 241001530097 Verbascum Species 0.000 claims description 27
- 235000010599 Verbascum thapsus Nutrition 0.000 claims description 27
- 150000008145 iridoid glycosides Chemical class 0.000 claims description 27
- 238000004140 cleaning Methods 0.000 claims description 25
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 24
- 239000002002 slurry Substances 0.000 claims description 23
- 238000000746 purification Methods 0.000 claims description 21
- 238000012216 screening Methods 0.000 claims description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 238000003825 pressing Methods 0.000 claims description 17
- 238000012545 processing Methods 0.000 claims description 17
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 16
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 16
- 230000010354 integration Effects 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 14
- 238000004458 analytical method Methods 0.000 claims description 13
- 238000001914 filtration Methods 0.000 claims description 13
- 239000007787 solid Substances 0.000 claims description 13
- 150000003384 small molecules Chemical class 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 12
- 229920002521 macromolecule Polymers 0.000 claims description 11
- 238000004321 preservation Methods 0.000 claims description 10
- 238000001694 spray drying Methods 0.000 claims description 10
- 241000336316 Cistanche tubulosa Species 0.000 claims description 9
- 238000001704 evaporation Methods 0.000 claims description 9
- 235000010323 ascorbic acid Nutrition 0.000 claims description 8
- 229960005070 ascorbic acid Drugs 0.000 claims description 8
- 239000011668 ascorbic acid Substances 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 235000010265 sodium sulphite Nutrition 0.000 claims description 8
- 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 claims description 7
- 238000005054 agglomeration Methods 0.000 claims description 7
- 230000002776 aggregation Effects 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 235000015165 citric acid Nutrition 0.000 claims description 6
- 235000013305 food Nutrition 0.000 claims description 6
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 claims description 6
- 239000000919 ceramic Substances 0.000 claims description 5
- 238000007710 freezing Methods 0.000 claims description 5
- 241000985690 Cistanche sinensis Species 0.000 claims description 4
- 241000308150 Orobanchaceae Species 0.000 claims description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 239000011780 sodium chloride Substances 0.000 claims description 4
- 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 description 2
- 238000013467 fragmentation Methods 0.000 claims description 2
- 238000006062 fragmentation reaction Methods 0.000 claims description 2
- ZINJLDJMHCUBIP-UHFFFAOYSA-N ethametsulfuron-methyl Chemical compound CCOC1=NC(NC)=NC(NC(=O)NS(=O)(=O)C=2C(=CC=CC=2)C(=O)OC)=N1 ZINJLDJMHCUBIP-UHFFFAOYSA-N 0.000 claims 1
- 238000006555 catalytic reaction Methods 0.000 abstract description 6
- 230000015556 catabolic process Effects 0.000 abstract description 2
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- 239000004480 active ingredient Substances 0.000 abstract 2
- 238000006243 chemical reaction Methods 0.000 abstract 1
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- 230000009897 systematic effect Effects 0.000 abstract 1
- 150000004676 glycans Chemical class 0.000 description 11
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- 239000005017 polysaccharide Substances 0.000 description 11
- 102000004169 proteins and genes Human genes 0.000 description 11
- 108090000623 proteins and genes Proteins 0.000 description 11
- 150000005846 sugar alcohols Polymers 0.000 description 10
- 238000005303 weighing Methods 0.000 description 10
- 239000006199 nebulizer Substances 0.000 description 9
- 239000007921 spray Substances 0.000 description 7
- 239000010408 film Substances 0.000 description 6
- 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
- 241000530105 Clerodendrum minahassae Species 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 238000001291 vacuum drying Methods 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
- 239000008280 blood Substances 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 150000002338 glycosides Chemical class 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 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
- 206010007247 Carbuncle Diseases 0.000 description 1
- 102000030523 Catechol oxidase Human genes 0.000 description 1
- 108010031396 Catechol oxidase Proteins 0.000 description 1
- 102000016559 DNA Primase Human genes 0.000 description 1
- 108010092681 DNA Primase Proteins 0.000 description 1
- 208000010228 Erectile Dysfunction Diseases 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
- 206010046543 Urinary incontinence Diseases 0.000 description 1
- 201000004810 Vascular dementia Diseases 0.000 description 1
- 125000002777 acetyl group Chemical group [H]C([H])([H])C(*)=O 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 210000004369 blood Anatomy 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
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- 238000004108 freeze drying Methods 0.000 description 1
- 239000007789 gas Substances 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
- 201000001881 impotence Diseases 0.000 description 1
- 208000021267 infertility disease Diseases 0.000 description 1
- 210000000936 intestine Anatomy 0.000 description 1
- 229930182489 iridoid glycoside Natural products 0.000 description 1
- 210000003127 knee Anatomy 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- KRTSDMXIXPKRQR-AATRIKPKSA-N monocrotophos Chemical compound CNC(=O)\C=C(/C)OP(=O)(OC)OC KRTSDMXIXPKRQR-AATRIKPKSA-N 0.000 description 1
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- Coloring Foods And Improving Nutritive Qualities (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The present invention provides a production method of cynamorlum extract full of active ingredients as echinacoside and veroascose glucoside monomeric compounds with high yield extracted from fresh cynamorlum succulent stem. The production method is implemented through systematic integrated technology of cytoclasis, serous extraction, membrane separation, high-temperature enzyme sterilization, spraying and drying, and other processes, so as to realize the manufacturing process from feeding the fresh cynamorlum to obtaining powdery or granular cynamorlum extract with high yield within 15 to 60 minutes. The present invention effectively inhibits, blocks and overcomes the technical defect of serious degradation and loss of active ingredients of echinacoside and veroascose glucoside monomeric compounds caused by enzyme catalysis reaction of poor drying method of cynamorlum. The major index ingredients of the obtained powdery or granular cynamorlum extract for measuring the cynamorlum quality are echinacoside and veroascose glucoside monomeric compounds, the productive rate of which is up to 15 to 23.4 percent (calculated in dry materials).
Description
Technical field
The present invention relates to a kind of from fresh chylocaulous extracting be rich in the production method of the cistanche salsa extract of active component echinacoside and mullein glucoside monomeric compound.
Background technology
Herba Cistanches (Herba Cistanches) is famous traditional traditional tonic medicine." Herba Cistanches that records of Chinese pharmacopoeia version in 2005 is the chylocaulous of orobanchaceae plant cistanche Cistanche deserticolaY.C.Ma and Cistanche Tubulosa Cistanche tubulosa (Schrenk) R.Wight dry zone scale leaf.The Shennong's Herbal cloud: Herba Cistanches " main five kinds of strain and seven kinds of impairment person is that fire declines can not the immature soil, non-in the dominator of QI void also.The treatment gynecopathy, salty can softening the hard mass and walk blood system also.The smart incontinence of urine of Herba Cistanches stopping leak removes hot carbuncle in the stem, can lead asthenic fire also down with it, old man's dryness accumulated in the stomach and intestine, the benefit food of cooking congee ".Successive dynasties Confucian classics record, the Herba Cistanches property of medicine is gentle, mends and not high, supports and not dry, has the effect of kidney-replenishing, benefiting essence-blood, loosening bowel to relieve constipation; Be used for the treatment of diseases such as sexual impotence, infertile, soreness of the waist and knees, muscles and bones are unable, constipation.In order to promote Herba Cistanches to belong to the development and use of medicinal plants, Chinese scholars belongs to medicinal plants to Herba Cistanches and has carried out extensive studies.The effective active matter phenethyl alcohol glycoside compounds of Cistanche Tubulosa has been developed two kind new medicines that become the treatment vascular dementia.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 (Phenylethanoid Glycosides, Ph Gs) comprise boschnaloside, echinacoside (echinacosid), verbascoside (acteoside or acteoside), 2 '-materials such as acetyl group verbascoside.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, 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, just echinacoside and mullein glucoside monomeric compound content are very abundant in the fresh herba cistanches chylocaulous of being unearthed, can be up to 24.3% (in dry), but different processing modes reaches from the place of production, kind, in the different desertliving cistanche sheet samples of collecting of host and collection season, echinacoside and mullein glucoside monomeric compound content only are 0.03%~1.0%, 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 extracting be rich in the production method of the cistanche salsa extract of active component echinacoside and mullein glucoside monomeric compound.
The present invention proposes a kind of passing through system integration technology, from the fresh herba cistanches chylocaulous, the production method of the cistanche salsa extract of active component echinacoside and mullein glucoside monomeric compound is rich in the high yield extracting, by cell breakage technology, the serosity extraction process, membrane separation process, high temperature enzyme denaturing technology, the enforcement of system integration technologies such as drying process with atomizing, technological process is short, make water few as solvent and consumption, meet the environmental requirement of energy-saving and emission-reduction, be implemented in and finish the technology manufacture process of the fresh herba cistanches raw material being obtained the cistanche salsa extract that is powdery or fine granularity that is rich in echinacoside and mullein glucoside monomeric compound isoreactivity material from the paramount productive rate that feeds intake in 15~60 minutes, effectively containment, blocking-up and overcome the echinacoside that enzymic catalytic reaction caused that the bad drying method of common Herba Cistanches causes and technological deficiency that mullein glucoside monomeric compound isoreactivity composition is lost by severely degrade is lifted at the economic worth that western desert is promoted the parasitic Herba Cistanches of sand-fixation plant significantly.
Method of the present invention is, select the fresh herba cistanches chylocaulous, or employing places 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, raw material is placed the rinsing bowl cold rinse, 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; The fragmentation and the technical process of milling, Material control also can adopt to charge into common food grade liquid nitrogen or CO at low temperature environment below 20 ℃
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 to 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 industrial centrifugal machine separates and obtains Herba Cistanches smudge cells cleaning mixture; 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 membrane separating technology device ultrafilter membrane, selectivity sieves and holds back macromole impurity such as removing polysaccharide, protein and impurity such as microgranule and submicron, or further by NF membrane, selectivity sieves and holds back small molecular weight impurities such as removing polyhydric alcohol, separates obtaining being rich in phenethyl alcohol glycoside compounds and iridoid glycoside compounds isoreactivity material extract; Adopt common industrial vacuum concentration technology, or thin film evaporation concentration technology, the acquisition solid content is 20%~75% cistanche salsa extract concentrate, by common industrial drying process with atomizing, or three sections drying process with atomizing dryings, and utilize high temperature drying steam that the instantaneous processing of concentrate superhigh temperature of atomizing is made the enzyme activity forfeiture and obtains the instantaneous exsiccant effect of superhigh temperature; Also can be through second section drying tower body dry section with the further dehydrate of powdered cistanche salsa extract; Also can further cool off and the agglomeration pelletize powdered cistanche salsa extract, to obtain to be the cistanche salsa extract of fine granularity through the 3rd section dry section.Above system integration technology flow process was finished in 15~60 minutes; Measure by analysis, phenethyl alcohol glycoside compounds and iridoid glycoside compounds isoreactivity content of material are abundant in the cistanche salsa extract that is powdery or fine granularity of results, wherein weigh the leading indicator composition echinacoside of Herba Cistanches quality and mullein glucoside monomeric compound productive rate up to 15%~23.4% (in dry), moisture is 0.5%~2.8%.
The cistanche salsa extract concentrate that the inventive method is extracted also can adopt usually the method for other industrially drying to obtain powder, as industrial cylinder dry, microwave vacuum drying, vacuum drying, microwave drying, lyophilization and 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 4C~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 ℃; The industrial membrane separating technology device that adopts, by ultrafilter membrane fenestra selectivity screening and hold back the ultrafilter membrane of macromolecular substances or the relative molecular mass of ceramic membrane or NF membrane is 1000~3000, best selectivity screening and hold back the ultrafilter membrane of macromolecular substances or the relative molecular mass of ceramic membrane or NF membrane is 1500~2500; Also can pass through common industrial membrane separating technology device again, the relative molecular mass that sieves and hold back the NF membrane of small-molecule substance by NF membrane fenestra selectivity is 200~300, and the relative molecular mass that best selectivity sieved and held back the NF membrane of small-molecule substance is 210~250; It is 125 ℃~285 ℃ that the industrial drying process with atomizing that adopts, or three sections drying process with atomizing, the instantaneous processing of drying tower superhigh temperature make the temperature of enzyme activity forfeiture and the instantaneous exsiccant effect of acquisition superhigh temperature, 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), spend salt Herba Cistanches (Cistanche salsa var.albiflora P.F.Tu et Z.C.Lou) in vain, the Herba Cistanches chylocaulous of the fresh band scale leaf of one or more in 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), 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, selected raw material is placed the rinsing bowl cold rinse, 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 mill the technical process Material control 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, obtain 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 membrane separating technology, sieve and hold back and remove macromole impurity by ultrafilter membrane fenestra selectivity, or further sieve and hold back and remove small molecular weight impurity by the NF membrane selectivity, separate obtaining being rich in Herba Cistanches active substance extracts such as phenethyl alcohol glycoside compounds and iridoid glycoside compounds.
6, adopt common industrial vacuum concentration technology, or the industrial film evaporating and concentrating process, the acquisition solid content is 20%~75% cistanche salsa extract concentrate.
7, with the cistanche salsa extract concentrate, adopt common industrial drying process with atomizing, or three sections drying process with atomizing carry out drying, and utilize high temperature drying steam that the instantaneous processing of concentrate superhigh temperature of atomizing is made the enzyme activity forfeiture and the temperature that obtains the instantaneous exsiccant effect of superhigh temperature is 125 ℃~285 ℃; Also can be through second section drying tower body dry section with the further dehydrate of powdered cistanche salsa extract; Also can cool off and the agglomeration pelletize powdered cistanche salsa extract through the 3rd section dry section again, obtain to be the cistanche salsa extract of fine granularity.
8, above system integration technology flow process was finished in 15~60 minutes; Measure by analysis, phenethyl alcohol glycoside compounds and iridoid glycoside compounds isoreactivity content of material are abundant in the cistanche salsa extract that is powdery or fine granularity of results, wherein weigh the leading indicator composition echinacoside of Herba Cistanches quality and mullein glucoside monomeric compound productive rate up to 15%~23.4% (in dry), moisture is 0.5%~2.8%.
The percentage ratio of the various amounts that relate among the present invention (%) all is weight percentage.
The leading indicator composition echinacoside of measurement Herba Cistanches quality and the productive rate of mullein glucoside monomeric compound are contained echinacoside and the amount of mullein glucoside monomeric compound and the percentage ratio (in dry) of raw material gross weight in the product in the product described in the present invention (cistanche salsa extracts that are powdery or fine granularity of results).
The specific embodiment
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment one:
1, selects fresh tube flower herba cistanches chylocaulous as raw material;
2, raw material is placed the rinsing bowl cold rinse, the cold water water temperature is 4 ℃; 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 nitrogen gas concn 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, Herba Cistanches cell serosity is adopted common industrial membrane separating technology, sieve and hold back and remove polysaccharide by ultrafilter membrane fenestra selectivity, macromole impurity and impurity such as microgranule and submicron such as protein, and further sieve and hold back small molecular weight impurities such as removing polyhydric alcohol by the NF membrane selectivity, separate the extract that obtains being rich in Herba Cistanches such as phenethyl alcohol glycoside compounds and iridoid glycoside compounds, industrial membrane separating technology device selectivity screening of selecting for use and the relative molecular mass of holding back the ultrafilter membrane of macromolecular substances are 2000, and selectivity screening of selecting for use and the relative molecular mass of holding back the NF membrane of small-molecule substance are 200; And through the industrial vacuum concentration technology, temperature is 45 ℃, and the acquisition solid content is 40% cistanche salsa extract concentrate;
5, the cistanche salsa extract concentrate is passed through three sections drying process with atomizing dryings, the dry tower body that connects at the spray drying tower nebulizer carries out drying by 280 ℃ of high temperature drying steam to the concentrate that atomizes, and utilizes the instantaneous processing of superhigh temperature to make enzyme activity forfeiture and the instantaneous exsiccant effect of acquisition superhigh temperature; Then through second section drying tower body dry section with the further dehydrate of powdered cistanche salsa extract, through the 3rd section dry section powdered cistanche salsa extract is cooled off and the agglomeration pelletize again, to obtain the cistanche salsa extract of fine granularity;
6, above system integration technology flow process was finished in 55 minutes; Measure by analysis, phenethyl alcohol glycoside compounds and iridoid glycoside compounds isoreactivity content of material are abundant in the cistanche salsa extract that is fine granularity of results, leading indicator composition echinacoside and the mullein glucoside monomeric compound productive rate of wherein weighing the Herba Cistanches quality are 17.8% (in dry), and moisture is 1.5%.
Embodiment two:
1, select place the storehouse temperature be the fresh-keeping fresh tube flower herba cistanches chylocaulous of 4 ℃ industrial freezer and Saline Cistanche Herb chylocaulous as raw material, ratio is 2: 1;
2, raw material is placed rinsing bowl 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
2, CO in the 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 16 ℃;
3, the Herba Cistanches cell slurry after will milling adopts industrial centrifugal machine to separate, and obtains Herba Cistanches cell serosity; Simultaneously repeat filtering residue added 200% the technical pure water purification (weight ratio) through pre-cooling through secondary, water temperature is 5 ℃; And further grind to form slurry through common industrial grinder, obtain Herba Cistanches smudge cells cleaning mixture through industrial pressure filter filter pressing again;
4, adopt common industrial instantaneous ultrahigh-temperature sterilization device technique, will carry 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, with the Herba Cistanches extracting solution behind the instantaneous enzyme denaturing of superhigh temperature, adopt common industrial membrane separating technology, sieve and hold back and remove polysaccharide by ultrafilter membrane fenestra selectivity, macromole impurity and impurity such as microgranule and submicron such as protein, and further sieve and hold back small molecular weight impurities such as removing polyhydric alcohol by the NF membrane selectivity, separate the extract that obtains being rich in Herba Cistanches such as phenethyl alcohol glycoside compounds and iridoid glycoside compounds, industrial membrane separating technology device selectivity screening of selecting for use and the relative molecular mass of holding back the ultrafilter membrane of macromolecular substances are 1000, and selectivity screening of selecting for use and the relative molecular mass of holding back the NF membrane of small-molecule substance are 250; And through the industrial film evaporating and concentrating process, temperature is 45 ℃, and the acquisition solid content is 75% cistanche salsa extract concentrate;
6, with the cistanche salsa extract concentrate, the dry tower body that connects at the spray drying tower nebulizer carries out drying by high temperature drying steam to the concentrate that atomizes, the instantaneous exsiccant temperature of superhigh temperature is 180 ℃, again through second section drying tower body dry section with the further dehydrate of powdered cistanche salsa extract, obtain to be powdered cistanche salsa extract;
7, above system integration technology flow process was finished in 34 minutes; Measure by analysis, results to be in the powdered cistanche salsa extract phenethyl alcohol glycoside compounds and iridoid glycoside compounds isoreactivity content of material abundant, leading indicator composition echinacoside and the mullein glucoside monomeric compound productive rate of wherein weighing the Herba Cistanches quality are 18.6% (in dry), and moisture is 2.0%.
Embodiment three:
1, adopt the quick-freezing Cistanche Tubulosa chylocaulous of industrial freezer-52 ℃ cold preservation as raw material;
2, raw material is placed rinsing bowl 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; Broken and the technical process of milling is added into 0.002% sodium sulfite (weight ratio) of raw material weight; Recording temperature of charge is 3 ℃;
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, with after Herba Cistanches cell serosity and the merging of smudge cells cleaning mixture, adopt common industrial membrane separating technology, sieve and hold back macromole impurity such as removing polysaccharide, protein and impurity such as microgranule and submicron by ultrafilter membrane fenestra selectivity, separate the extract that obtains being rich in Herba Cistanches such as phenethyl alcohol glycoside compounds and iridoid glycoside compounds, the relative molecular mass that the industrial membrane separating technology device selectivity of selecting for use sieved and held back the ultrafilter membrane of macromolecular substances is 3000; And through the industrial vacuum concentration technology, temperature is 65 ℃, and the acquisition solid content is 55% cistanche salsa extract concentrate;
5, with the cistanche salsa extract concentrate, the dry tower body that connects at the spray drying tower nebulizer carries out drying to the concentrate of spray process atomizing and utilizes the instantaneous processing of superhigh temperature to make the enzyme activity forfeiture and the temperature that obtains the instantaneous exsiccant effect of superhigh temperature is 225 ℃ by high temperature drying steam; Through second section drying, the tower body dry section is with the further dehydrate of powdered cistanche salsa extract then; Through the 3rd section dry section powdered cistanche salsa extract is cooled off and the agglomeration pelletize again, obtain to be the cistanche salsa extract of fine granularity;
6, above system integration technology flow process was finished in 48 minutes; Measure by analysis, phenethyl alcohol glycoside compounds and iridoid glycoside compounds isoreactivity content of material are abundant in the cistanche salsa extract that is fine granularity of results, leading indicator composition echinacoside and the mullein glucoside monomeric compound productive rate of wherein weighing the Herba Cistanches quality are 18.8% (in dry), and moisture is 0.9%.
Embodiment four:
1, select for use selected Herba Cistanches chylocaulous and particle as raw material;
2, the raw material of selecting for use is placed rinsing bowl with 6 ℃ of cold rinse, 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 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 12 ℃;
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 added 100% the technical pure water purification (weight ratio) through pre-cooling, 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 again;
4, after Herba Cistanches cell serosity and the merging of smudge cells cleaning mixture, adopt common industrial membrane separating technology, sieve and hold back and remove polysaccharide by ultrafilter membrane fenestra selectivity, macromole impurity and impurity such as microgranule and submicron such as protein, and further sieve and hold back small molecular weight impurities such as removing polyhydric alcohol by the NF membrane selectivity, separate the extract that obtains being rich in Herba Cistanches such as phenethyl alcohol glycoside compounds and iridoid glycoside compounds, industrial membrane separating technology device selectivity screening of selecting for use and the relative molecular mass of holding back the ultrafilter membrane of macromolecular substances are 2500, and selectivity screening of selecting for use and the relative molecular mass of holding back the NF membrane of small-molecule substance are 250; And through the industrial film evaporating and concentrating process, temperature is 55 ℃; The acquisition solid content is 30% cistanche salsa extract concentrate;
5, with the cistanche salsa extract concentrate, dry tower body in the connection of spray drying tower nebulizer, by high temperature drying steam the concentrate of spray process atomizing is carried out drying, and utilize the instantaneous processing of superhigh temperature to make the enzyme activity forfeiture and the temperature that obtains the instantaneous exsiccant effect of superhigh temperature is 225 ℃; Again through second section drying tower body dry section with the further dehydrate of powdered cistanche salsa extract, obtain to be powdered cistanche salsa extract;
6, above system integration technology flow process was finished in 45 minutes; Measure by analysis, results to be in the powdered cistanche salsa extract phenethyl alcohol glycoside compounds and iridoid glycoside compounds isoreactivity content of material abundant, leading indicator composition echinacoside and the mullein glucoside monomeric compound productive rate of wherein weighing the Herba Cistanches quality are 18.2% (in dry), and moisture is 0.9%.
Embodiment five:
1, adopt selected Herba Cistanches sinensis chylocaulous and particle as raw material;
2, the raw material of selecting for use is placed rinsing bowl with 3 ℃ of cold rinse, 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 8 ℃;
3, the Herba Cistanches cell slurry after will milling adopts common industrial pressure filter filter pressing, obtains Herba Cistanches cell serosity;
4, with Herba Cistanches cell serosity and the common industrial membrane separating technology of employing, sieve and hold back and remove polysaccharide by ultrafilter membrane fenestra selectivity, macromole impurity and impurity such as microgranule and submicron such as protein, and further sieve and hold back small molecular weight impurities such as removing polyhydric alcohol by the NF membrane selectivity, separate the extract that obtains being rich in Herba Cistanches such as phenethyl alcohol glycoside compounds and iridoid glycoside compounds, industrial membrane separating technology device selectivity screening of selecting for use and the relative molecular mass of holding back the ultrafilter membrane of macromolecular substances are 1500, and selectivity screening of selecting for use and the relative molecular mass of holding back the NF membrane of small-molecule substance are 210; And through the industrial vacuum concentration technology, temperature is 60 ℃; The acquisition solid content is 48% cistanche salsa extract concentrate;
5, with the cistanche salsa extract concentrate, dry tower body in the connection of spray drying tower nebulizer, by high temperature drying steam the concentrate of spray process atomizing is carried out drying, and utilize the instantaneous processing of superhigh temperature to make the enzyme activity forfeiture and the temperature that obtains the instantaneous exsiccant effect of superhigh temperature is 130 ℃;
6, above system integration technology flow process was finished in 46 minutes; Measure by analysis, results to be in the powdered cistanche salsa extract phenethyl alcohol glycoside compounds and iridoid glycoside compounds isoreactivity content of material abundant, leading indicator composition echinacoside and the mullein glucoside monomeric compound productive rate of wherein weighing the Herba Cistanches quality are 15% (in dry), and moisture is 2.8%.
Embodiment six:
1, selects the fresh salt Herba Cistanches chylocaulous of spending in vain as raw material;
2, raw material is placed the rinsing bowl cold rinse, the cold water water temperature is 3 ℃; 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 nitrogen, and nitrogen gas concn is 3.0% (weight ratio) in the Herba Cistanches raw material; Recording temperature of charge is 10 ℃;
3, the Herba Cistanches cell slurry after will milling adopts common industrial pressure filter filter pressing, obtains Herba Cistanches cell serosity, and secondary repeats filtering residue added 100% the technical pure water purification (weight ratio) through pre-cooling simultaneously, and water temperature is 5 ℃; And further grind to form slurry through common industrial grinder, obtain Herba Cistanches smudge cells cleaning mixture through industrial pressure filter filter pressing again;
4, adopt common industrial instantaneous ultrahigh-temperature sterilization device technique, will carry 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 135 ℃;
5, will be through the Herba Cistanches extracting solution behind the instantaneous enzyme denaturing of superhigh temperature, adopt common industrial membrane separating technology, sieve and hold back and remove polysaccharide by ultrafilter membrane fenestra selectivity, macromole impurity and impurity such as microgranule and submicron such as protein, and further sieve and hold back small molecular weight impurities such as removing polyhydric alcohol by the NF membrane selectivity, separate the extract that obtains being rich in Herba Cistanches such as phenethyl alcohol glycoside compounds and iridoid glycoside compounds, industrial membrane separating technology device selectivity screening of selecting for use and the relative molecular mass of holding back the ultrafilter membrane of macromolecular substances are 1500, and selectivity screening of selecting for use and the relative molecular mass of holding back the NF membrane of small-molecule substance are 280; And to obtain solid content through the industrial vacuum concentration technology be 40% cistanche salsa extract concentrate;
6, with the cistanche salsa extract concentrate, through the industrial vacuum drying, baking temperature is 62 ℃; Acquisition is powdered cistanche salsa extract;
7, in 30 minutes, finish above system integration technology flow process, measure by analysis, results to be in the powdered cistanche salsa extract phenethyl alcohol glycoside compounds and iridoid glycoside compounds isoreactivity content of material abundant, leading indicator composition echinacoside and the mullein glucoside monomeric compound productive rate of wherein weighing the Herba Cistanches quality are 16.9% (in dry), and moisture is 1.2%.
Embodiment seven:
1, select for use selected Cistanche Tubulosa chylocaulous and particle as raw material;
2, raw material is placed rinsing bowl with 2 ℃ of cold rinse; 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
2Gas concentration is 1.0% (weight ratio); Broken and the technical process of milling is added 0.002% citric acid of raw material weight and 0.001% sodium sulfite (weight ratio); Recording temperature of charge is 8 ℃;
3, the Herba Cistanches cell slurry after will milling adopts common industrial pressure filter filter pressing, obtains Herba Cistanches cell serosity, and through repeating filtering residue added 70% the technical pure water purification (weight ratio) through pre-cooling for three times, water temperature is 4 ℃ simultaneously; 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, after Herba Cistanches cell serosity and the merging of smudge cells cleaning mixture, adopt common industrial membrane separating technology, sieve and hold back and remove polysaccharide by ultrafilter membrane fenestra selectivity, macromole impurity and impurity such as microgranule and submicron such as protein, and further sieve and hold back small molecular weight impurities such as removing polyhydric alcohol by the NF membrane selectivity, separate the extract that obtains being rich in Herba Cistanches such as phenethyl alcohol glycoside compounds and iridoid glycoside compounds, industrial membrane separating technology device selectivity screening of selecting for use and the relative molecular mass of holding back the ultrafilter membrane of macromolecular substances are 2500, and selectivity screening of selecting for use and the relative molecular mass of holding back the NF membrane of small-molecule substance are 250; And through the industrial film evaporating and concentrating process, temperature is 55 ℃; The acquisition solid content is 30% cistanche salsa extract concentrate;
5, with the cistanche salsa extract concentrate, dry tower body in the connection of spray drying tower nebulizer, by high temperature drying steam the concentrate of spray process atomizing is carried out drying, and utilize the instantaneous processing of superhigh temperature to make the enzyme activity forfeiture and the temperature that obtains the instantaneous exsiccant effect of superhigh temperature is 220 ℃; Then through second section drying tower body dry section with the further dehydrate of powdered cistanche salsa extract; Through the 3rd section dry section powdered cistanche salsa extract is cooled off and the agglomeration pelletize again, obtain to be the cistanche salsa extract of fine granularity;
6, above system integration technology flow process was finished in 60 minutes; Measure by analysis, phenethyl alcohol glycoside compounds and iridoid glycoside compounds isoreactivity content of material are abundant in the cistanche salsa extract that is fine granularity of results, leading indicator composition echinacoside and the mullein glucoside monomeric compound productive rate of wherein weighing the Herba Cistanches quality are 20.8% (in dry), and moisture is 0.7%.
Embodiment eight:
1, employing places 2 ℃ of fresh-keeping fresh Saline Cistanche Herb chylocaulouss of industrial freezer as raw material;
2, selected raw material is placed rinsing bowl 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; 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, Herba Cistanches cell serosity is adopted common industrial membrane separating technology, sieve and hold back macromole impurity such as removing polysaccharide, protein and impurity such as microgranule and submicron by ultrafilter membrane fenestra selectivity, separate the extract that obtains being rich in Herba Cistanches such as phenethyl alcohol glycoside compounds and iridoid glycoside compounds, the relative molecular mass that the industrial membrane separating technology device selectivity of selecting for use sieved and held back the ultrafilter membrane of material is 1000; And through the industrial vacuum concentration technology, temperature is 65 ℃; The acquisition solid content is 40% cistanche salsa extract concentrate;
5, with the cistanche salsa extract concentrate, dry tower body in the connection of spray drying tower nebulizer, by high temperature drying steam the concentrate of spray process atomizing is carried out drying, and utilize the instantaneous processing of superhigh temperature to make the enzyme activity forfeiture and the temperature that obtains the instantaneous exsiccant effect of superhigh temperature is 135 ℃; Again through second section drying tower body dry section with the further dehydrate of powdered cistanche salsa extract, obtain to be powdered cistanche salsa extract;
6, above system integration technology flow process was finished in 50 minutes; Measure by analysis, results to be in the powdered cistanche salsa extract phenethyl alcohol glycoside compounds and iridoid glycoside compounds isoreactivity content of material abundant, leading indicator composition echinacoside and the mullein glucoside monomeric compound productive rate of wherein weighing the Herba Cistanches quality are 16.9% (in dry), and moisture is 1.5%.
Embodiment nine:
1, select for use selected Cistanche Tubulosa chylocaulous and particle as raw material;
2, raw material is placed rinsing bowl with 12 ℃ of cold rinse, 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 into 0.003% ascorbic acid (weight ratio) of raw material weight; Recording temperature of charge is 18 ℃;
3, the Herba Cistanches cell slurry after will milling adopts common industrial pressure filter filter pressing, obtains Herba Cistanches cell serosity, separates through industrial centrifugal machine and obtains Herba Cistanches smudge cells cleaning mixture;
4, after Herba Cistanches cell serosity and the merging of smudge cells cleaning mixture, adopt common industrial membrane separating technology, sieve and hold back and remove polysaccharide by ultrafilter membrane fenestra selectivity, macromole impurity and impurity such as microgranule and submicron such as protein, and further sieve and hold back small molecular weight impurities such as removing polyhydric alcohol by the NF membrane selectivity, separate the extract that obtains being rich in Herba Cistanches such as phenethyl alcohol glycoside compounds and iridoid glycoside compounds, the relative molecular mass of the ceramic membrane of the industrial membrane separating technology of selecting for use is 2500, and selectivity screening of selecting for use and the relative molecular mass of holding back the NF membrane of small-molecule substance are 210; And through the industrial film evaporating and concentrating process, temperature is 58 ℃; The acquisition solid content is 53% cistanche salsa extract concentrate;
5, with the cistanche salsa extract concentrate, dry tower body in the connection of spray drying tower nebulizer, by high temperature drying steam the concentrate that spray process atomizes is carried out drying, and utilize the instantaneous processing of superhigh temperature to make enzyme activity forfeiture and the temperature that obtains the instantaneous exsiccant effect of superhigh temperature is 215 ℃, obtain to be powdered cistanche salsa extract;
6, above system integration technology flow process was finished in 33 minutes; Measure by analysis, results to be in the powdered cistanche salsa extract phenethyl alcohol glycoside compounds and iridoid glycoside compounds isoreactivity content of material abundant, leading indicator composition echinacoside and the mullein glucoside monomeric compound productive rate of wherein weighing the Herba Cistanches quality are 21.7% (in dry), and moisture is 1.8%.
Embodiment ten:
1, selects fresh tube flower herba cistanches chylocaulous as raw material;
2, selected raw material is placed rinsing bowl with 2 ℃ of cold rinse, after picking up, place common industrial breaker and milling device, the Herba Cistanches chylocaulous is broken and mill, make cell cracked; The temperature of charge that records is 12 ℃;
3, the Herba Cistanches cell slurry after will milling adopts common industrial centrifugal machine to separate, and obtains Herba Cistanches cell serosity, and through repeating to add 150% the technical pure water purification (weight ratio) through pre-cooling for three times, water temperature is 3 ℃ with filtering residue; Three repetitions further grind to form slurry through common industrial grinder, separate through industrial centrifugal machine again, obtain Herba Cistanches smudge cells cleaning mixture;
4, after Herba Cistanches cell serosity and the merging of smudge cells cleaning mixture, adopt common industrial membrane separating technology, sieve and hold back and remove polysaccharide by ultrafilter membrane fenestra selectivity, macromole impurity and impurity such as microgranule and submicron such as protein, and further sieve and hold back small molecular weight impurities such as removing polyhydric alcohol by the NF membrane selectivity, separate the extract that obtains being rich in Herba Cistanches such as phenethyl alcohol glycoside compounds and iridoid glycoside compounds, selecting property of the NF membrane screening of the industrial membrane separating technology of selecting for use and the relative molecular mass of holding back material are 1000, and selectivity screening of selecting for use and the relative molecular mass of holding back the NF membrane of small-molecule substance are 250; And through the industrial vacuum concentration technology, temperature is 45 ℃; The acquisition solid content is 56% cistanche salsa extract concentrate;
5, with the cistanche salsa extract concentrate, dry tower body in the connection of spray drying tower nebulizer, by high temperature drying steam the concentrate of spray process atomizing is carried out drying, and utilize the instantaneous processing of superhigh temperature to make the enzyme activity forfeiture and the temperature that obtains the instantaneous exsiccant effect of superhigh temperature is 195 ℃; Then through second section drying tower body dry section with the further dehydrate of powdered cistanche salsa extract; Through the 3rd section dry section powdered cistanche salsa extract is cooled off and the agglomeration pelletize again, obtain to be the cistanche salsa extract of fine granularity;
6, above system integration technology flow process was finished in 25 minutes; Measure by analysis, phenethyl alcohol glycoside compounds and iridoid glycoside compounds isoreactivity content of material are abundant in the cistanche salsa extract that is fine granularity of results, leading indicator composition echinacoside and the mullein glucoside monomeric compound productive rate of wherein weighing the Herba Cistanches quality are 23.4% (in dry), and moisture is 0.7%.
Claims (12)
- One kind from Herba Cistanches extracting be rich in the production method of the cistanche salsa extract of active component echinacoside and mullein glucoside monomeric compound, it is characterized in that selecting the Herba Cistanches chylocaulous of fresh and cold preservation for use is raw material; After the raw material rinsing picked up, by industrial fragmentation and milling device that the Herba Cistanches chylocaulous is broken and mill, adopt filter pressing or separating technology to obtain Herba Cistanches cell serosity; Filtering residue is added the technical pure water purification, after grinding to form slurry, obtain Herba Cistanches smudge cells cleaning mixture through filter pressing or separation again; With Herba Cistanches cell serosity or merging smudge cells cleaning mixture, or adopt the instantaneous enzyme denaturing of superhigh temperature, separate the cistanche salsa extract that obtains being rich in active component echinacoside and mullein glucoside monomeric compound through the industrial membrane separating technology; Obtain the cistanche salsa extract concentrate through concentration technology, dry and utilize high temperature drying by drying process with atomizing or three sections drying process with atomizing, steam makes the enzyme activity forfeiture and obtains the instantaneous exsiccant effect of superhigh temperature the instantaneous processing of concentrate superhigh temperature of atomizing, and results are the cistanche salsa extract of powdery or fine granularity.
- 2. in accordance with the method for claim 1, the concrete steps that it is characterized in that this 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) selected raw material is placed the rinsing bowl cold rinse, 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, broken and mill the technical process Material control 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, obtain 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 membrane separating technology, sieve and hold back and remove macromole impurity by ultrafilter membrane fenestra selectivity, or further sieve and hold back and remove small molecular weight impurity by the NF membrane selectivity, separate obtaining being rich in Herba Cistanches active substance extracts such as phenethyl alcohol glycoside compounds and iridoid glycoside compounds;(6) adopt common industrial vacuum concentration technology, or the industrial film evaporating and concentrating process, temperature is 45 ℃~65 ℃, the acquisition solid content is 20%~75% cistanche salsa extract concentrate;(7) with the cistanche salsa extract concentrate, adopt common industrial drying process with atomizing, or three sections drying process with atomizing carry out drying, and utilize high temperature drying steam that the instantaneous processing of concentrate superhigh temperature of atomizing is made the enzyme activity forfeiture and the temperature that obtains the instantaneous exsiccant effect of superhigh temperature is 125 ℃~285 ℃; Also can be through second section drying tower body dry section with the further dehydrate of powdered cistanche salsa extract; Also can cool off and the agglomeration pelletize powdered cistanche salsa extract through the 3rd section dry section again, obtain to be the cistanche salsa extract of fine granularity;(8) above system integration technology flow process was finished in 15~60 minutes; Measure by analysis, phenethyl alcohol glycoside compounds and iridoid glycoside compounds isoreactivity content of material are abundant in the cistanche salsa extract that is powdery or fine granularity of results, wherein weigh the leading indicator composition echinacoside of Herba Cistanches quality and mullein glucoside monomeric compound productive rate up to 15%~23.4% (in dry), moisture is 0.5%~2.8%.
- 3. in accordance with the method for claim 2, 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), spend salt Herba Cistanches (Cistanche salsa var.albiflora P.F.Tu etZ.C.Lou) in vain, Saline Cistanche Herb (Cisttanche salsa (C.A.Mey) G.Beck) and Herba Cistanches sinensis or title C.sinensis G.Beck (Cistanche sinensis G.Beck) can be selected one or more for use.
- 4. in accordance with the method for claim 2, it is characterized in that the fresh-keeping storehouse temperature of the industrial freezer described in the step (2) is 1 ℃~13 ℃; The storehouse temperature of industry freezer cold preservation is-52 ℃~-10 ℃; Cold water water temperature in the tank is 1 ℃~20 ℃; In the Herba Cistanches raw material, charge into liquid nitrogen or CO 2Concentration be 0.1%~5.0% (weight ratio); In the Herba Cistanches raw material, add CO 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 ℃; Ascorbic acid, citric acid, gluconic acid lactone, the sodium sulfite of the interpolation trace that adopts are food grade, and addition is 0.001%~0.03% (weight ratio), can select one or more for use.
- 5. in accordance with the method for claim 2, 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 10%~200% (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 1 ℃~20 ℃.
- 6. in accordance with the method for claim 2, the technological temperature that it is characterized in that the instantaneous enzyme denaturing of the described industrial superhigh temperature of step (4) is 135 ℃~141 ℃.
- 7. in accordance with the method for claim 2, it is characterized in that the industrial membrane separating technology device selectivity screening described in the step (5) and hold back the ultrafilter membrane of macromolecular substances or the relative molecular mass of ceramic membrane or NF membrane is 1000~3000; The relative molecular mass that selectivity sieved and held back the NF membrane of small-molecule substance is 200~300.
- 8. in accordance with the method for claim 2, it is characterized in that the industrial vacuum concentration technology described in the step (6), or the industrial film evaporating and concentrating process, temperature is 45 ℃~65 ℃.
- 9. in accordance with the method for claim 4, 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 ℃; Cold water water temperature in the tank is 4 ℃~10 ℃; In the Herba Cistanches raw material, charge into liquid nitrogen or CO 2Concentration be 0.5%~1% (weight ratio); In the Herba Cistanches raw material, add CO 2The frozen water temperature is 4 ℃~6 ℃; CO 2CO in the frozen water 2Concentration is 1%~2% (weight ratio); Ascorbic acid, citric acid, gluconic acid lactone, the sodium sulfite addition of the interpolation trace that adopts are 0.002%~0.004% (weight ratio).
- 10. in accordance with the method for claim 5, it is characterized in that described in filtering residue through once 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 ℃.
- 11. in accordance with the method for claim 7, it is characterized in that the selectivity screening that described industrial membrane separating technology device selects for use and hold back the ultrafilter membrane of macromolecular substances or the relative molecular mass of ceramic membrane or NF membrane is 1500~2500; The relative molecular mass that selectivity sieved and held back the small-molecule substance NF membrane is 210~250.
- 12. in accordance with the method for claim 2, it is characterized in that it is 190 ℃~230 ℃ that the instantaneous superhigh temperature of the spray drying tower described in the step (7) is handled the temperature that makes the enzyme activity forfeiture and obtain the instantaneous exsiccant effect of superhigh temperature.
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