CN101214283B - Method for producing cistanche salsa extract - Google Patents

Method for producing cistanche salsa extract Download PDF

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Publication number
CN101214283B
CN101214283B CN2007100328105A CN200710032810A CN101214283B CN 101214283 B CN101214283 B CN 101214283B CN 2007100328105 A CN2007100328105 A CN 2007100328105A CN 200710032810 A CN200710032810 A CN 200710032810A CN 101214283 B CN101214283 B CN 101214283B
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herba cistanches
temperature
industrial
cistanche
drying
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CN101214283A (en
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刘昕
季青
贾宝国
陈海
彭青云
钟倩莉
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SHENZHEN XUEZI BIOLOGY CO Ltd
Sun Yat Sen University
National Sun Yat Sen University
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SHENZHEN XUEZI BIOLOGY CO Ltd
National Sun Yat Sen University
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Abstract

The present invention provides a production method of effectively extracting active ingredients as echinacoside and veroascose glucoside monomeric compound from fresh cynamorlum succulent stem through systematic integrated technology. The production method is implemented through systematic integrated technology of cytoclasis, serous extraction, 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 within 15 to 45 minutes. The present invention effectively overcomes the technical defect of serious degradation and loss of active ingredients of phenethyl alcohol glucoside compounds caused by enzyme catalysis reaction of poor drying method of cynamorlum. Through analysis and determination, the content of phenethyl alcohol glucoside compound and iridoid glucoside compound in the obtained powdery or granular cynamorlum extract is abundant; wherein, the productive rate of the major index ingredients for measuring the cynamorlum quality as echinacoside and veroascose glucoside monomeric compounds is up to 15 to 23.8 percent (calculated in dry materials), and the water content is 0.5 to 3 percent.

Description

A kind of production method of cistanche salsa extract
Technical field
The present invention relates to a kind of production method of cistanche salsa extract.
Background technology
Herba Cistanches (Herba Cistanches) is famous traditional tonic medicine, is the highest kidney-replenishing medicine of successive dynasties traditional Chinese medical science usage frequency." Herba Cistanches that records of Chinese pharmacopoeia version in 2005 is the chylocaulous of Orobanchaceae plant Cistanche deserticola Y.C.Ma and Cistanche Tubulosa Cistanchetubulosa (Schrenk) Wight dry zone scale leaf.The Compendium of Material Medica record " Herba Cistanches cures mainly five kinds of strain and seven kinds of impairment, and invigorating middle warmer removes cold and heat carbuncle in the stem, supports the five internal organs, reinforcing YIN-essence, and tonifying YANG, beneficial vital essence, how sub.Fu Ren mass in the abdomen, clothes are made light of one's life by commiting suicide for a long time.Remove bladder pathogen lumbago, dysentery relieving.The benefit marrow, improving healthy complexion is prolonged life, and mends tonifying YANG greatly, and day was driven letter, controlled woman's metrorrhagia.The man is exhausted, and sun is out of fashion, and the woman is exhausted, and the moon does not produce.Moistening five ZANG-organs, longue meat, warm waist knee joint.The man lets out smart urine, and blood is lost drop, the cloudy carbuncle of woman's leukorrhagia.The mutually fiery not enough person of the gate of vitality mends it with this, be kidney channel blood system medicine also ... ".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.Modern study shows that the main active ingredient of Herba Cistanches is phenethyl alcohol glycosides, iridoid glycosides, lignanoid's glycoside, oligosaccharide esters and polyhydric alcohol etc.Phenethyl alcohol glycosides (PhenylethanoidGlycosides, Ph Gs) chemical compound 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, 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 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 through system integration technology, from the fresh herba cistanches chylocaulous, effectively the production method of active component echinacoside and mullein glucoside monomeric compound is rich in extracting.The system integration technology of the present invention through technologies such as cell breakage technology, serosity extraction process, high temperature enzyme denaturing technology, spray drying are carried out continuously; Be implemented in 15~45 minutes and accomplish the fresh herba cistanches raw material, effectively contain, block and overcome the phenethyl alcohol glycoside compounds isoreactivity composition that enzymic catalytic reaction caused that the bad drying method of common Herba Cistanches causes by the technological deficiency of severely degrade loss from being dosed to the technical process of obtaining cistanche salsa extract.The inventive method can be 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, 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; Or with Herba Cistanches cell serosity, or merge the smudge cells cleaning mixture, adopt common industrial vacuum concentration technology, or the thin film evaporation concentration technology, the acquisition solid content is 20%~75% Herba Cistanches extract concentrate; Adopt common industrial drying process with atomizing, or three sections drying process with atomizing dryings of industry, and utilize high temperature drying steam to make enzyme activity lose and obtain the effect of superhigh temperature instantaneous drying to the cell serosity or the extract concentrate superhigh temperature instantaneous processed of atomizing; 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 accomplished in 15~45 minutes; Through assay determination; 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; Leading indicator composition echinacoside and the mullein glucoside monomeric compound productive rate of wherein weighing the Herba Cistanches quality are up to 15%~23.8% (in dry), and moisture is 0.5%~3.0%.
The Herba Cistanches extract concentrate that the inventive method is extracted 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 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-48 ℃~-10 ℃, and the storehouse temperature of best freezer cold preservation is-36 ℃~-18 ℃; The cold water water temperature that places the tank rinsing 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 2Optimum temperature is 4 ℃~6 ℃ in the frozen water, 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%~0.02% (weight ratio); Optimum addition is 0.002%~0.005% (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%~150% (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 ℃; It is 120 ℃~280 ℃ that the industrial drying process with atomizing that adopts, or three sections drying process with atomizing of industry, 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 180 ℃~210 ℃.
The Herba Cistanches that the present invention relates to is Orobanchaceae plant (Orobanchaceae) Herba Cistanches or claims Desert Herba Cistanches (Cistanche deserticolaY.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.albifloraR.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 (Cistanchesinensis 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, select 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 selected Herba Cistanches chylocaulous and particle is 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, adopt common industrial vacuum concentration technology; Or industrial film evaporating and concentrating process; With Herba Cistanches cell serosity; Or merge the smudge cells cleaning mixture, or the Herba Cistanches extracting solution behind the instantaneous enzyme denaturing of superhigh temperature concentrates, and obtains solid content and be 20%~75% Herba Cistanches extract concentrate.
6, with the cell serosity; Or merging smudge cells cleaning mixture; Or the Herba Cistanches extracting solution behind the instantaneous enzyme denaturing of superhigh temperature, or spissated Herba Cistanches extract concentrate, adopt common industrial drying process with atomizing; Or three sections drying process with atomizing dryings of industry, and utilize high temperature drying steam that cell serosity or the concentrate superhigh temperature instantaneous processed of atomizing made the enzyme activity forfeiture and the temperature that obtains the effect of superhigh temperature instantaneous drying is 120 ℃~280 ℃; 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.
7, above system integration technology flow process was accomplished in 15~45 minutes; Through assay determination; 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; Leading indicator composition echinacoside and the mullein glucoside monomeric compound productive rate of wherein weighing the Herba Cistanches quality are up to 15%~23.8% (in dry), and moisture is 0.5%~3.0%.
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 done further explain.
Embodiment one:
1, selects fresh tube flower herba cistanches chylocaulous as raw material;
2, place rinsing bowl to use cold rinse raw material, the cold water water temperature is 10 ℃; After picking up, place common industrial breaker and milling device that the Herba Cistanches chylocaulous is broken and mill, make cell cracked; It is 18 ℃ that the broken and technical process of milling records temperature of charge, charges into liquid nitrogen, and liquid nitrogen concentration is 1.0% (weight ratio) in the material;
3, the Herba Cistanches cell slurry after will milling adopts common industrial pressure filter filter pressing, obtains Herba Cistanches cell serosity;
4, Herba Cistanches cell serosity is passed through three sections drying process with atomizing dryings of industry; The dry tower body that connects at the spray drying tower nebulizer carries out drying through 280 ℃ of high temperature drying steam to the Herba Cistanches cell serosity 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 cistanche salsa extract and the agglomeration pelletize to powdered cistanche salsa extract through the 3rd section dry section more then, to obtain to be the cistanche salsa extract of fine granularity;
5, above system integration technology flow process was accomplished in 42 minutes; Through assay determination; 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 17.3% (in dry), and moisture is 1.2%.
Embodiment two:
1, selects that to place the storehouse temperature be that the fresh-keeping fresh tube flower herba cistanches chylocaulous of 4 ℃ industrial freezer is as raw material;
2, with raw material 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; It is 10 ℃ that the broken and technical process of milling records temperature of charge, charges into CO 2, CO in the material 2Concentration is 0.5% (weight ratio), and is added into 0.002% ascorbic acid of raw material weight and 0.001% gluconic acid lactone (weight ratio);
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 85% technical pure water purification (weight ratio) for three times through pre-cooling, water temperature is 4 ℃; And further grind to form slurry through common industrial grinder, separate through industrial centrifugal machine again and obtain Herba Cistanches smudge cells cleaning mixture;
4, with after Herba Cistanches cell serosity and the merging of smudge cells cleaning mixture; Adopt the industrial film evaporating and concentrating process; Temperature is 65 ℃; The acquisition solid content is 60% Herba Cistanches extracting solution concentrate; The dry tower body that connects at industrial spray drying tower nebulizer carries out drying through high temperature drying steam to the concentrate of 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 200 ℃, 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;
5, above system integration technology flow process was accomplished in 45 minutes; Through assay determination; 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 23.8% (in dry), and moisture is 0.5%.
Embodiment three:
1, select for use selected Herba Cistanches chylocaulous and particle as raw material;
2, place rinsing bowl to use cold rinse raw material, the cold water water temperature is 4 ℃, 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 CO 2Frozen water; Add CO 2The frozen water amount is 20% (weight ratio) of inventory, CO 2CO in the frozen water 2Concentration is 1% (weight ratio), and the frozen water temperature is 4 ℃, and recording temperature of charge is 10 ℃;
3, the Herba Cistanches cell slurry after will milling adopts common industrial pressure filter filter pressing; Obtain Herba Cistanches cell serosity; Filtering residue is added 45% technical pure water purification (weight ratio); 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, 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 adopt common industrial film evaporating and concentrating process through the Herba Cistanches extracting solution behind the instantaneous enzyme denaturing of superhigh temperature; Temperature is 60 ℃; The acquisition solid content is 50% Herba Cistanches extracting solution concentrate; Carry out spray drying through industrial spray drying tower then, the temperature of superhigh temperature instantaneous drying is 210 ℃; Second section drying tower body dry section of warp obtains to be powdered cistanche salsa extract with the further dehydrate of powdered cistanche salsa extract then;
6, above system integration technology flow process was accomplished in 30 minutes; Through assay determination; 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 18.1% (in dry), and moisture is 1.7%.
Embodiment four:
1, the quick-freezing Saline Cistanche Herb chylocaulous that adopts industrial freezer-10 ℃ cold preservation is 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; Recording temperature of charge after milling is 18 ℃;
3, the Herba Cistanches cell slurry after will milling adopts common industrial pressure filter filter pressing, further separates through industrial centrifugal machine again, obtains Herba Cistanches cell serosity;
4, Herba Cistanches cell serosity is adopted the industrial vacuum concentration technology; Temperature is 45 ℃; The acquisition solid content is 40% Herba Cistanches extracting solution concentrate; The dry tower body that connects at industrial spray drying tower nebulizer carries out drying through high temperature drying steam to the concentrate of 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 120 ℃;
5, above system integration technology flow process was accomplished in 45 minutes; Through assay determination; 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 2.4%.
Embodiment five:
1, employing places the fresh-keeping fresh herba cistanches chylocaulous of 4 ℃ of storehouse temperature of industrial freezer 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; Recording temperature of charge is 19 ℃; Broken and the technical process of milling is added the food grade sodium sulfite of trace, and addition is 0.002% of a raw material weight;
3, the Herba Cistanches cell slurry after will milling adopts common industrial pressure filter filter pressing, obtains Herba Cistanches cell serosity, and filtering residue is added 150% 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, with after Herba Cistanches cell serosity and the merging of smudge cells cleaning mixture; Adopt the industrial film evaporating and concentrating process; Temperature is 50 ℃; Obtain solid content and be 50% Herba Cistanches extracting solution concentrate, the dry tower body that connects at industrial spray drying tower nebulizer carries out drying through high temperature drying steam to the concentrate of 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 200 ℃; With the further dehydrate of powdered cistanche salsa extract, obtain to be powdered cistanche salsa extract through second section drying tower body dry section;
5, above system integration technology flow process was accomplished in 38 minutes; Through assay determination; 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 18.8% (in dry), and moisture is 1.8%.
Embodiment six:
1, selects fresh Herba Cistanches sinensis chylocaulous and fresh tube flower herba cistanches chylocaulous as raw material, ratio 1: 2;
2, place rinsing bowl with 2 ℃ 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; Broken and the technical process of milling can add 20%CO 2Frozen water (weight ratio), CO 2CO in the frozen water 2Concentration is 1% (weight ratio), CO 2The frozen water temperature is 4 ℃, and adds the food grade ascorbic acid of trace, and addition is 0.003% of a raw material weight; 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;
4, Herba Cistanches cell serosity is adopted the industrial film evaporating and concentrating process; Temperature is 55 ℃; The acquisition solid content is 65% Herba Cistanches extract thing concentrate; The dry tower body that connects at industrial spray drying tower nebulizer carries out drying through high temperature drying steam to the concentrate of 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 185 ℃, obtains to be powdered cistanche salsa extract;
5, above system integration technology flow process was accomplished in 24 minutes; Through assay determination; 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 20.2% (in dry), and moisture is 1.9%.
Embodiment seven:
1, selects the fresh herba cistanches chylocaulous as raw material;
2, place rinsing bowl with 4 ℃ 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; Fragmentation and the food grade ascorbic acid of technical process interpolation 0.001% and 0.001% the sodium sulfite (weight ratio) of milling; Recording temperature of charge is 17 ℃;
3, the Herba Cistanches cell slurry after will milling adopts common industrial centrifugal machine to separate; Obtain Herba Cistanches cell serosity; Technical pure water purification (weight ratio) with filtering residue adding 80% 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 the industrial film evaporating and concentrating process; Temperature is 50 ℃; Obtain solid content and be 50% Herba Cistanches extracting solution concentrate, the dry tower body that connects at industrial spray drying tower nebulizer carries out drying through high temperature drying steam to the concentrate of atomizing, and utilizes the superhigh temperature instantaneous processed to make the enzyme activity forfeiture and the effect temperature that obtains the superhigh temperature instantaneous drying is 270 ℃; Second section drying tower body dry section of warp obtains to be powdered cistanche salsa extract with the further dehydrate of powdered cistanche salsa extract then;
5, above system integration technology flow process was accomplished in 28 minutes; Through assay determination; 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 21.3% (in dry), and moisture is 1.3%.
Embodiment eight:
1, employing places the fresh-keeping fresh Herba Cistanches sinensis chylocaulous of 2 ℃ of storehouse temperature of industrial freezer 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; Recording temperature of charge is 19 ℃;
3, the Herba Cistanches cell slurry after will milling adopts common industrial pressure filter filter pressing, obtains Herba Cistanches cell serosity, and filtering residue is repeated to add 200% the technical pure water purification (weight ratio) through pre-cooling through secondary, and water temperature is 4 ℃; 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, with after Herba Cistanches cell serosity and the merging of smudge cells cleaning mixture, adopt the industrial film evaporating and concentrating process, temperature is 45 ℃, and the acquisition solid content is 48% Herba Cistanches extracting solution 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 235 ℃; Second section drying tower body dry section of warp obtains to be powdered cistanche salsa extract with the further dehydrate of Herba Cistanches extracting solution concentrate then;
5, above system integration technology flow process was accomplished in 32 minutes; Through assay determination; 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 20.4% (in dry), and moisture is 1.9%.
Embodiment nine:
1, employing places the quick-freezing of industrial freezer-36 ℃ cold preservation to spend salt Herba Cistanches, Herba Cistanches and Cistanche Tubulosa chylocaulous in vain as raw material, and ratio is 1: 2: 1;
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; Recording temperature of charge is 3 ℃;
3, the saline cistanche cell slurry after will milling adopts common industrial filter press press filtration; Obtain saline cistanche cell slurries; Simultaneously through repeating filter residue added 100% technical pure water purification (weight ratio) for four times; Repetition further grinds to form slurry through common industrial grinder, obtains saline cistanche smudge cells cleaning solution through industrial filter press press filtration again;
4, with after Herba Cistanches cell serosity and the merging of smudge cells cleaning mixture, adopt the industrial film evaporating and concentrating process, temperature is 55 ℃, and the acquisition solid content is 40% Herba Cistanches extracting solution concentrate; Through industrial spray drying tower high temperature drying steam the concentrate of atomizing 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 210 ℃, obtain to be powdered cistanche salsa extract;
5, above system integration technology flow process was accomplished in 28 minutes; Through assay determination; 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 22.1% (in dry), and moisture is 2.3%.
Embodiment ten:
1, select for use selected Herba Cistanches and Cistanche Tubulosa chylocaulous and particle as raw material, ratio is 1: 1;
2, place rinsing bowl with 8 ℃ 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 of charge is 20 ℃;
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 instantaneous ultrahigh-temperature sterilization device technique, Herba Cistanches cell serosity is carried out the instantaneous enzyme denaturing of superhigh temperature, the temperature of the instantaneous enzyme denaturing of superhigh temperature is 141 ℃;
5, will adopt common industrial vacuum concentration technology through the Herba Cistanches cell serosity behind the instantaneous enzyme denaturing of superhigh temperature, temperature is 45 ℃, and the acquisition solid content is 55% Herba Cistanches extracting solution concentrate; Through the industrial microwave vacuum drying, baking temperature is 60 ℃, obtains to be powdered cistanche salsa extract;
6, above system integration technology flow process was accomplished in 15 minutes; Through assay determination; 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 15.2% (in dry), and moisture is 3.0%.

Claims (7)

1. the production method of a cistanche salsa extract is characterized in that the concrete steps of this method comprise:
(1) selects the fresh-keeping fresh herba cistanches chylocaulous of fresh herba cistanches chylocaulous, industrial freezer or 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, the cold water water temperature is 1 ℃~20 ℃, or with industrial pure water rinsing, 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 process material of milling is controlled at low temperature environment below 20 ℃;
(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 again 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; Separate through industrial pressure filter filter pressing or industrial centrifugal machine again, obtain 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), adopt common industrial vacuum concentration technology, or industrial film evaporating and concentrating process will concentrate through the Herba Cistanches extracting solution behind the instantaneous enzyme denaturing of superhigh temperature, obtains solid content and be 20%~75% Herba Cistanches extract concentrate; Described industrial vacuum concentration technology or industrial film evaporating and concentrating process temperature are 45 ℃~65 ℃;
The Herba Cistanches extract concentrate that (6) will obtain through concentration technology; Adopt common industrial drying process with atomizing; Or three sections drying process with atomizing dryings of industry; 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 120 ℃~280 ℃;
(7) above system integration technology flow process was accomplished in 15~45 minutes; Through assay determination; Phenethyl alcohol glycoside compounds and iridoid glycosides compound activity content of material are abundant in the cistanche salsa extract that is powdery or fine granularity of results; Leading indicator composition echinacoside and the mullein glucoside monomeric compound productive rate of wherein weighing the Herba Cistanches quality reach 15%~23.8% in dry, and moisture is 0.5%~3%.
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 salsa var.albiflora P.F.Tu et Z.C.Lou), Saline Cistanche Herb (Cistanche salsa (C.A.Mey) G.Beck) 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 ℃; The storehouse temperature of industry freezer cold preservation is-48 ℃~-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%~150% 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 ℃; Cold water water temperature in the 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 once to adding for several times the technical pure water purification, or be 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 180 ℃~210 ℃ that the spray drying superhigh temperature instantaneous processed described in the step (6) makes the temperature of the effect of enzyme activity forfeiture and acquisition superhigh temperature instantaneous drying.
CN2007100328105A 2007-12-28 2007-12-28 Method for producing cistanche salsa extract Expired - Fee Related CN101214283B (en)

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CN101654692B (en) * 2009-08-04 2011-12-21 中山大学 Method for producing mullein glucoside monomeric compound
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
CN114588201B (en) * 2022-03-30 2024-01-02 北京中科健宇生物科技有限公司 Preparation method of cistanche extract and anti-alcohol liver-protecting product containing cistanche extract

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