CN101214282B - Method for extracting active component from cistanche salsa - Google Patents
Method for extracting active component from cistanche salsa Download PDFInfo
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- CN101214282B CN101214282B CN2007100328073A CN200710032807A CN101214282B CN 101214282 B CN101214282 B CN 101214282B CN 2007100328073 A CN2007100328073 A CN 2007100328073A CN 200710032807 A CN200710032807 A CN 200710032807A CN 101214282 B CN101214282 B CN 101214282B
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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 succulent stem extracting be rich in the production method of the cistanche salsa extract of active component echinacoside and mullein glucoside monomeric compound.
Background technology
Saline cistanche (Herba Cistanches) is famous traditional traditional tonic medicine." saline cistanche recorded of Chinese pharmacopoeia version in 2005 is the succulent stem 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: saline cistanche " main general debility person is that fire declines can not the immature soil, non-in the dominator of QI void also.The treatment gynecopathy, the soft heavily fortified point of salty energy and walk blood system also.The smart something lost of desert cistanche stopping leak drowned, and removes hot carbuncle in the stem, can lead the fire of deficiency type also down with it, old man's constipation, the benefit food of cooking congee ".Successive dynasties Confucian classics record, the saline cistanche property of medicine is gentle, mends and not high, supports and not dry, the effect that have kidney-replenishing, benefiting essence-blood, relaxes bowel; Be used for the treatment of diseases such as impotence, infertile, soreness and weakness of waist and knees, muscles and bones are unable, constipation.In order to promote saline cistanche to belong to the development and use of medicinal plant, Chinese scholars belongs to medicinal plant to saline cistanche and has carried out extensive studies.The effective active matter benzyl carbinol glycosides compounds of Cistanche tubulosa has been developed two kind new medicines that become the treatment blood vessel nature feeble-mindedness.Modern study shows that the main active of saline cistanche is benzyl carbinol glycoside, iridoid glycosides, lignanoid's glycoside, few sugar esters and polyalcohol etc.The compound of benzyl carbinol glycoside (Phenylethanoid Glycosides, Ph Gs) comprise boschnaloside, echinacoside (echinacosid), acteoside (acteoside or acteoside), 2 '-materials such as acetyl group acteoside.And echinacoside and mullein glucoside monomeric compound are the higher benzyl carbinol glycosides compounds of content in the saline cistanche succulent stem, and these two kinds of representative active components are as the leading indicator of estimating the saline cistanche quality at present.
Fresh herba cistanches succulent stem moisture surpasses 80% usually, and process is difficult for dry.Traditional diamond-making technique adopts the fresh herba cistanches succulent stem placed under the sunlight always and dries, or shady and cool place dries in the shade, or dries behind the salt marsh, 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 saline cistanche has the metal ion of activation, wherein K to the enzymatic 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 hydrolase, glycoside hydrolase and polyphenol oxidase system in the fresh herba cistanches succulent stem, dry processing procedure is because undried saline cistanche is in bad dry processing environments such as moistening, damp and hot for a long time, and in the process because of reasons such as physical damnifications, the enzyme that is activated causes active enzymic catalytic reaction rapidly and produces enzymatic browning, the benzyl carbinol glycosides compounds isoreactivity composition that causes saline cistanche 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 succulent stem that is 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 benzyl carbinol glycosides compounds that saline cistanche 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 technology and drying method are that the primase catalytic reaction causes the active component benzyl carbinol glycosides compounds degraded loss that saline cistanche is rich in, particularly the key factor of two kinds of representative active component echinacosides 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 succulent stem 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 succulent stem, 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 clasmatosis technology, the slurries extraction process, membrane separation process, the high temperature enzymatic process that goes out, 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 saline cistanche 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 saline cistanche of sand-fixation plant significantly.
Method of the present invention is, select the fresh herba cistanches succulent stem, or employing places the fresh-keeping fresh herba cistanches succulent stem of industrial freezer, or the quick-frozen saline cistanche succulent stem that adopts industrial freezer to refrigerate, or select for use selected saline cistanche succulent stem 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 saline cistanche succulent stem 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, glucolactone, sodium sulfite etc.; Saline cistanche cell slurry after milling is adopted common industrial filter press press filtration, or the industrial centrifugal machine separation, saline cistanche cell slurries obtained; Also can be with filter residue through once to adding for several times the technical pure water purification or through the technical pure water purification of precooling, once to further grinding to form slurry through common industrial grinder for several times, again through industrial filter press press filtration, or industrial centrifugal machine separates and obtains saline cistanche smudge cells cleaning solution; Adopt common industrial ultra high temperature short time sterilization device technique, with saline cistanche cell slurries, or merging smudge cells cleaning solution carries out the instantaneous enzyme that goes out of superhigh temperature; With saline cistanche cell slurries, or merging smudge cells cleaning solution, or the saline cistanche extract behind the instantaneous enzyme that goes out of superhigh temperature, adopt common industrial membrane separating technology device milipore filter, selectivity screening and hold back and remove big molecular impurity such as polysaccharide, protein and impurity such as particulate and submicron, or further by NF membrane, small molecular weight impurities such as removing polyalcohol is sieved and held back to selectivity, separates obtaining being rich in benzyl carbinol glycosides 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 hot gas the instantaneous processing of concentrate superhigh temperature of atomizing to be made the effect of enzyme activity forfeiture and the instantaneous drying of acquisition superhigh temperature; Also can further dehydrate through the cistanche salsa extract of second section drying tower body dry section with powdery; Also can further cool off and the agglomeration granulation, to obtain to be the cistanche salsa extract of fine granularity through the cistanche salsa extract of the 3rd section dry section to powdery.Above system integration technology flow process was finished in 15～60 minutes; Measure by analysis, benzyl carbinol glycosides 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 saline cistanche 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 roller drying, micro-wave vacuum, vacuum drying, microwave drying, freeze drying and heated-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 refrigeration is-52 ℃～-10 ℃, and the storehouse temperature of best freezer refrigeration 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 saline cistanche raw material
2Concentration be 0.1%～5.0% (weight ratio), optium concentration is 0.5%～1% (weight ratio); That adopts adds CO in the saline cistanche 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, glucolactone, 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 filter 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 precooling, optimum addition is 50%～100% (weight ratio), technical pure water purification water temperature through precooling is 1 ℃～20 ℃, and optimum water temperature is 4 ℃～10 ℃; The temperature that the industrial ultra high temperature short time sterilization device technique that adopts carries out the instantaneous enzyme that goes out 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 milipore filter fenestra selectivity screening and hold back the milipore filter of macromolecular substances or the relative molecular mass of ceramic membrane or NF membrane is 1000～3000, best selectivity screening and hold back the milipore filter 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 the NF membrane of small-molecule substance was sieved and held back to best selectivity 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 the effect of enzyme activity forfeiture and the instantaneous drying of acquisition superhigh temperature, and best temperature is 190 ℃～230 ℃.
The saline cistanche that the present invention relates to is Orobanchaceae plant (Orobanchaceae) saline cistanche or claims Desert Herba Cistanches (Cistanchedeserticola Y.C.Ma), Cistanche tubulosa (Cistanche tubulosa (Schrenk) R.Wight), spend salt desert cistanche (Cistanche salsa var.albiflora P.F.Tu et Z.C.Lou) in vain, the saline cistanche succulent stem of the fresh band scale leaf of one or more in the husky raw meat desert cistanche of salt raw meat desert cistanche (Cistanche salsa (C.A.Mey) G.Beck) and husky desert cistanche or title (Cistanche sinensis G.Beck), or through the fresh-keeping fresh herba cistanches succulent stem of freezer, or the quick-frozen saline cistanche succulent stem of freezer refrigeration, or select selected saline cistanche succulent stem and particle for use.
The cistanche salsa extract that is powdery or fine granularity that the inventive method is produced, can directly produce products such as capsule, tablet, granule, electuary, pill or tea in bag as raw material, 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 succulent stem, or adopt and to place the fresh-keeping fresh herba cistanches succulent stem of industrial freezer, or adopt the quick-frozen saline cistanche succulent stem of industrial freezer refrigeration, or select for use selected saline cistanche succulent stem 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 saline cistanche succulent stem 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, glucolactone, sodium sulfite etc.
3, the saline cistanche cell slurry after will milling adopts common industrial filter press press filtration, or industrial centrifugal machine separates, obtain saline cistanche cell slurries, also can be with filter residue through once extremely adding for several times the technical pure water purification, or through the technical pure water purification of precooling, once to further grinding to form slurry through common industrial grinder for several times, again through industrial filter press press filtration, or the industrial centrifugal machine separation, obtain saline cistanche smudge cells cleaning solution.
4, adopt common industrial ultra high temperature short time sterilization device technique, with saline cistanche cell slurries, or merging smudge cells cleaning solution carries out the instantaneous enzyme that goes out of superhigh temperature.
5, with saline cistanche cell slurries, or merging smudge cells cleaning solution, or the saline cistanche extract behind the instantaneous enzyme that goes out of superhigh temperature, adopt common industrial membrane separating technology, sieve and hold back and remove big molecular impurity by milipore filter fenestra selectivity, or further sieve and hold back and remove small molecular weight impurity by the NF membrane selectivity, separate obtaining being rich in saline cistanche active material extracts such as benzyl carbinol glycosides 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 hot gas that the instantaneous processing of concentrate superhigh temperature of atomizing is made the enzyme activity forfeiture and the temperature that obtains the effect of the instantaneous drying of superhigh temperature is 125 ℃～285 ℃; Also can further dehydrate through the cistanche salsa extract of second section drying tower body dry section with powdery; Also can cool off and the agglomeration granulation through the cistanche salsa extract of the 3rd section dry section again, obtain to be the cistanche salsa extract of fine granularity powdery.
8, above system integration technology flow process was finished in 15～60 minutes; Measure by analysis, benzyl carbinol glycosides 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 saline cistanche quality and mullein glucoside monomeric compound productive rate up to 15%～23.4% (in dry), moisture is 0.5%～2.8%.
The percentage of the various amounts that relate among the present invention (%) all is weight percentage.
The leading indicator composition echinacoside of measurement saline cistanche quality and the productive rate of mullein glucoside monomeric compound are contained echinacoside and the amount of mullein glucoside monomeric compound and the percentage (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 succulent stem 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 saline cistanche succulent stem 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 saline cistanche cell slurry after will milling adopts common industrial centrifugal machine to separate, and obtains saline cistanche cell slurries;
4, saline cistanche cell slurries are adopted common industrial membrane separating technology, sieve and hold back and remove polysaccharide by milipore filter fenestra selectivity, big molecular impurity such as protein and impurity such as particulate and submicron, and further sieve and hold back small molecular weight impurities such as removing polyalcohol by the NF membrane selectivity, separate and obtain being rich in the extract of saline cistanches such as benzyl carbinol glycosides 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 milipore filter 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 atomizer carries out drying by 280 ℃ of high temperature drying hot gas to the concentrate that atomizes, and utilizes the instantaneous processing of superhigh temperature to make the effect of enzyme activity forfeiture and the instantaneous drying of acquisition superhigh temperature; Further dehydrate through the cistanche salsa extract of second section drying tower body dry section then, cool off and the agglomeration granulation through the cistanche salsa extract of the 3rd section dry section again, to obtain the cistanche salsa extract of fine granularity powdery with powdery;
6, above system integration technology flow process was finished in 55 minutes; Measure by analysis, benzyl carbinol glycosides 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 saline cistanche 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 succulent stem of 4 ℃ industrial freezer and salt raw meat desert cistanche succulent stem 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 saline cistanche succulent stem 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% glucolactone and 0.003% citric acid (weight ratio); Recording temperature of charge is 16 ℃;
3, the saline cistanche cell slurry after will milling adopts industrial centrifugal machine to separate, and obtains saline cistanche cell slurries; Simultaneously repeat filter residue added 200% the technical pure water purification (weight ratio) through precooling through secondary, water temperature is 5 ℃; And further grind to form slurry through common industrial grinder, obtain saline cistanche smudge cells cleaning solution through industrial filter press press filtration again;
4, adopt common industrial ultra high temperature short time sterilization device technique, will carry out the instantaneous enzyme that goes out of superhigh temperature after saline cistanche cell slurries and the merging of smudge cells cleaning solution, the temperature of the instantaneous enzyme that goes out of superhigh temperature is 139 ℃;
5, with the saline cistanche extract behind the instantaneous enzyme that goes out of superhigh temperature, adopt common industrial membrane separating technology, sieve and hold back and remove polysaccharide by milipore filter fenestra selectivity, big molecular impurity such as protein and impurity such as particulate and submicron, and further sieve and hold back small molecular weight impurities such as removing polyalcohol by the NF membrane selectivity, separate and obtain being rich in the extract of saline cistanches such as benzyl carbinol glycosides 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 milipore filter 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 atomizer carries out drying by high temperature drying hot gas to the concentrate that atomizes, the temperature of the instantaneous drying of superhigh temperature is 180 ℃, further dehydrate through the cistanche salsa extract of second section drying tower body dry section again, obtain to be the cistanche salsa extract of powdery powdery;
7, above system integration technology flow process was finished in 34 minutes; Measure by analysis, benzyl carbinol glycosides compounds and iridoid glycoside compounds isoreactivity content of material are abundant in the cistanche salsa extract that is powdery of results, leading indicator composition echinacoside and the mullein glucoside monomeric compound productive rate of wherein weighing the saline cistanche quality are 18.6% (in dry), and moisture is 2.0%.
Embodiment three:
1, adopt the quick-frozen Cistanche tubulosa succulent stem of industrial freezer-52 ℃ refrigeration 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 saline cistanche succulent stem 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 saline cistanche cell slurry after will milling adopts common industrial filter press press filtration, obtains saline cistanche cell slurries; Filter residue is added 60% pure water (weight ratio), further grind to form slurry, separate through industrial centrifugal machine again and obtain saline cistanche smudge cells cleaning solution through common industrial grinder;
4, with after saline cistanche cell slurries and the merging of smudge cells cleaning solution, adopt common industrial membrane separating technology, by milipore filter fenestra selectivity screening and hold back and remove big molecular impurity such as polysaccharide, protein and impurity such as particulate and submicron, separate obtaining being rich in the extract of saline cistanches such as benzyl carbinol glycosides compounds and iridoid glycoside compounds, the relative molecular mass that the milipore filter of macromolecular substances was sieved and held back to the industrial membrane separating technology device selectivity of selecting for use 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 atomizer 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 effect of the instantaneous drying of superhigh temperature is 225 ℃ by high temperature drying hot gas; Through second section drying, the tower body dry section further dehydrates the cistanche salsa extract of powdery then; Cool off and the agglomeration granulation through the cistanche salsa extract of the 3rd section dry section again, obtain to be the cistanche salsa extract of fine granularity powdery;
6, above system integration technology flow process was finished in 48 minutes; Measure by analysis, benzyl carbinol glycosides 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 saline cistanche quality are 18.8% (in dry), and moisture is 0.9%.
Embodiment four:
1, select for use selected saline cistanche succulent stem 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 saline cistanche succulent stem 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 saline cistanche cell slurry after will milling adopts industrial centrifugal machine to separate, and obtains saline cistanche cell slurries, simultaneously filter residue is added 100% the technical pure water purification (weight ratio) through precooling, and water temperature is 4 ℃; Further grind to form slurry through common industrial grinder, obtain saline cistanche smudge cells cleaning solution through industrial filter press press filtration again;
4, after saline cistanche cell slurries and the merging of smudge cells cleaning solution, adopt common industrial membrane separating technology, sieve and hold back and remove polysaccharide by milipore filter fenestra selectivity, big molecular impurity such as protein and impurity such as particulate and submicron, and further sieve and hold back small molecular weight impurities such as removing polyalcohol by the NF membrane selectivity, separate and obtain being rich in the extract of saline cistanches such as benzyl carbinol glycosides 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 milipore filter 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 atomizer, by high temperature drying hot gas 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 effect of the instantaneous drying of superhigh temperature is 225 ℃; Further dehydrate through the cistanche salsa extract of second section drying tower body dry section again, obtain to be the cistanche salsa extract of powdery powdery;
6, above system integration technology flow process was finished in 45 minutes; Measure by analysis, benzyl carbinol glycosides compounds and iridoid glycoside compounds isoreactivity content of material are abundant in the cistanche salsa extract that is powdery of results, leading indicator composition echinacoside and the mullein glucoside monomeric compound productive rate of wherein weighing the saline cistanche quality are 18.2% (in dry), and moisture is 0.9%.
Embodiment five:
1, adopt selected husky desert cistanche succulent stem 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 saline cistanche succulent stem is broken and mill, make cell cracked; Recording temperature of charge is 8 ℃;
3, the saline cistanche cell slurry after will milling adopts common industrial filter press press filtration, obtains saline cistanche cell slurries;
4, with saline cistanche cell slurries and the common industrial membrane separating technology of employing, sieve and hold back and remove polysaccharide by milipore filter fenestra selectivity, big molecular impurity such as protein and impurity such as particulate and submicron, and further sieve and hold back small molecular weight impurities such as removing polyalcohol by the NF membrane selectivity, separate and obtain being rich in the extract of saline cistanches such as benzyl carbinol glycosides 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 milipore filter 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 atomizer, by high temperature drying hot gas 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 effect of the instantaneous drying of superhigh temperature is 130 ℃;
6, above system integration technology flow process was finished in 46 minutes; Measure by analysis, benzyl carbinol glycosides compounds and iridoid glycoside compounds isoreactivity content of material are abundant in the cistanche salsa extract that is powdery of results, leading indicator composition echinacoside and the mullein glucoside monomeric compound productive rate of wherein weighing the saline cistanche quality are 15% (in dry), and moisture is 2.8%.
Embodiment six:
1, selects the fresh salt desert cistanche succulent stem 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 saline cistanche succulent stem 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 saline cistanche raw material; Recording temperature of charge is 10 ℃;
3, the saline cistanche cell slurry after will milling adopts common industrial filter press press filtration, obtains saline cistanche cell slurries, and secondary repeats filter residue added 100% the technical pure water purification (weight ratio) through precooling simultaneously, and water temperature is 5 ℃; And further grind to form slurry through common industrial grinder, obtain saline cistanche smudge cells cleaning solution through industrial filter press press filtration again;
4, adopt common industrial ultra high temperature short time sterilization device technique, will carry out the instantaneous enzyme that goes out of superhigh temperature after saline cistanche cell slurries and the merging of smudge cells cleaning solution, the temperature of the instantaneous enzyme that goes out of superhigh temperature is 135 ℃;
5, will be through the saline cistanche extract behind the instantaneous enzyme that goes out of superhigh temperature, adopt common industrial membrane separating technology, sieve and hold back and remove polysaccharide by milipore filter fenestra selectivity, big molecular impurity such as protein and impurity such as particulate and submicron, and further sieve and hold back small molecular weight impurities such as removing polyalcohol by the NF membrane selectivity, separate and obtain being rich in the extract of saline cistanches such as benzyl carbinol glycosides 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 milipore filter 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 the cistanche salsa extract of powdery;
7, in 30 minutes, finish above system integration technology flow process, measure by analysis, benzyl carbinol glycosides compounds and iridoid glycoside compounds isoreactivity content of material are abundant in the cistanche salsa extract that is powdery of results, leading indicator composition echinacoside and the mullein glucoside monomeric compound productive rate of wherein weighing the saline cistanche quality are 16.9% (in dry), and moisture is 1.2%.
Embodiment seven:
1, select for use selected Cistanche tubulosa succulent stem 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 saline cistanche succulent stem 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 saline cistanche cell slurry after will milling adopts common industrial filter press press filtration, obtains saline cistanche cell slurries, and through repeating filter residue added 70% the technical pure water purification (weight ratio) through precooling for three times, water temperature is 4 ℃ simultaneously; Three repetitions further grind to form slurry through common industrial grinder, obtain saline cistanche smudge cells cleaning solution through industrial filter press press filtration again;
4, after saline cistanche cell slurries and the merging of smudge cells cleaning solution, adopt common industrial membrane separating technology, sieve and hold back and remove polysaccharide by milipore filter fenestra selectivity, big molecular impurity such as protein and impurity such as particulate and submicron, and further sieve and hold back small molecular weight impurities such as removing polyalcohol by the NF membrane selectivity, separate and obtain being rich in the extract of saline cistanches such as benzyl carbinol glycosides 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 milipore filter 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 atomizer, by high temperature drying hot gas 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 effect of the instantaneous drying of superhigh temperature is 220 ℃; Further dehydrate through the cistanche salsa extract of second section drying tower body dry section then powdery; Cool off and the agglomeration granulation through the cistanche salsa extract of the 3rd section dry section again, obtain to be the cistanche salsa extract of fine granularity powdery;
6, above system integration technology flow process was finished in 60 minutes; Measure by analysis, benzyl carbinol glycosides 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 saline cistanche quality are 20.8% (in dry), and moisture is 0.7%.
Embodiment eight:
1, employing places 2 ℃ of fresh-keeping fresh salt raw meat desert cistanche succulent stems 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 saline cistanche succulent stem is broken and mill, make cell cracked; Recording temperature of charge is 15 ℃;
3, the saline cistanche cell slurry after will milling adopts common industrial centrifugal machine to separate, and obtains saline cistanche cell slurries;
4, saline cistanche cell slurries are adopted common industrial membrane separating technology, by milipore filter fenestra selectivity screening and hold back and remove big molecular impurity such as polysaccharide, protein and impurity such as particulate and submicron, separate obtaining being rich in the extract of saline cistanches such as benzyl carbinol glycosides compounds and iridoid glycoside compounds, the relative molecular mass that the milipore filter of material was sieved and held back to the industrial membrane separating technology device selectivity of selecting for use 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 atomizer, by high temperature drying hot gas 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 effect of the instantaneous drying of superhigh temperature is 135 ℃; Further dehydrate through the cistanche salsa extract of second section drying tower body dry section again, obtain to be the cistanche salsa extract of powdery powdery;
6, above system integration technology flow process was finished in 50 minutes; Measure by analysis, benzyl carbinol glycosides compounds and iridoid glycoside compounds isoreactivity content of material are abundant in the cistanche salsa extract that is powdery of results, leading indicator composition echinacoside and the mullein glucoside monomeric compound productive rate of wherein weighing the saline cistanche quality are 16.9% (in dry), and moisture is 1.5%.
Embodiment nine:
1, select for use selected Cistanche tubulosa succulent stem 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 saline cistanche succulent stem 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 saline cistanche cell slurry after will milling adopts common industrial filter press press filtration, obtains saline cistanche cell slurries, separates through industrial centrifugal machine and obtains saline cistanche smudge cells cleaning solution;
4, after saline cistanche cell slurries and the merging of smudge cells cleaning solution, adopt common industrial membrane separating technology, sieve and hold back and remove polysaccharide by milipore filter fenestra selectivity, big molecular impurity such as protein and impurity such as particulate and submicron, and further sieve and hold back small molecular weight impurities such as removing polyalcohol by the NF membrane selectivity, separate and obtain being rich in the extract of saline cistanches such as benzyl carbinol glycosides 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 atomizer, by high temperature drying hot gas 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 effect of the instantaneous drying of superhigh temperature is 215 ℃, obtain to be the cistanche salsa extract of powdery;
6, above system integration technology flow process was finished in 33 minutes; Measure by analysis, benzyl carbinol glycosides compounds and iridoid glycoside compounds isoreactivity content of material are abundant in the cistanche salsa extract that is powdery of results, leading indicator composition echinacoside and the mullein glucoside monomeric compound productive rate of wherein weighing the saline cistanche quality are 21.7% (in dry), and moisture is 1.8%.
Embodiment ten:
1, selects fresh tube flower herba cistanches succulent stem 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 saline cistanche succulent stem is broken and mill, make cell cracked; The temperature of charge that records is 12 ℃;
3, the saline cistanche cell slurry after will milling adopts common industrial centrifugal machine to separate, and obtains saline cistanche cell slurries, and through repeating to add 150% the technical pure water purification (weight ratio) through precooling for three times, water temperature is 3 ℃ with filter residue; Three repetitions further grind to form slurry through common industrial grinder, separate through industrial centrifugal machine again, obtain saline cistanche smudge cells cleaning solution;
4, after saline cistanche cell slurries and the merging of smudge cells cleaning solution, adopt common industrial membrane separating technology, sieve and hold back and remove polysaccharide by milipore filter fenestra selectivity, big molecular impurity such as protein and impurity such as particulate and submicron, and further sieve and hold back small molecular weight impurities such as removing polyalcohol by the NF membrane selectivity, separate and obtain being rich in the extract of saline cistanches such as benzyl carbinol glycosides 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 atomizer, by high temperature drying hot gas 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 effect of the instantaneous drying of superhigh temperature is 195 ℃; Further dehydrate through the cistanche salsa extract of second section drying tower body dry section then powdery; Cool off and the agglomeration granulation through the cistanche salsa extract of the 3rd section dry section again, obtain to be the cistanche salsa extract of fine granularity powdery;
6, above system integration technology flow process was finished in 25 minutes; Measure by analysis, benzyl carbinol glycosides 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 saline cistanche quality are 23.4% (in dry), and moisture is 0.7%.
Claims (8)
1. the method for an extracting active component from saline cistanche is characterized in that the concrete steps of this method comprise:
(1) selects the fresh herba cistanches succulent stem, or adopt and to place the fresh-keeping fresh herba cistanches succulent stem of industrial freezer, or adopt the quick-frozen saline cistanche succulent stem of industrial freezer refrigeration, or select for use selected saline cistanche succulent stem and particle as raw material;
(2) selected raw material is placed the rinsing bowl cold rinse, the cold water water temperature is 1 ℃～20 ℃, or with industrial pure water rinsing, after picking up, place common industrial breaker and milling device, the saline cistanche succulent stem is broken and mill, make cell cracked, broken and mill the technical process Material control at low temperature environment below 20 ℃, perhaps adopt to charge into common food grade liquid nitrogen or CO
2, or add CO
2Frozen water perhaps adds again and selects one or more for use in the food grade ascorbic acid, citric acid, glucolactone, sodium sulfite of trace;
(3) the saline cistanche cell slurry after will milling adopts common industrial filter press press filtration, or industrial centrifugal machine separates, obtain saline cistanche cell slurries, perhaps with filter residue through once to adding for several times the technical pure water purification, or through the technical pure water purification of precooling, be 1 ℃～20 ℃ through the water temperature of the technical pure water purification of precooling, once to further grinding to form slurry through common industrial grinder for several times, again through industrial filter press press filtration, or industrial centrifugal machine separates, and obtains saline cistanche smudge cells cleaning solution;
(4) adopt common industrial ultra high temperature short time sterilization device technique, with saline cistanche cell slurries, or merge the smudge cells cleaning solution and carry out the instantaneous enzyme that goes out of superhigh temperature, temperature is 135 ℃～141 ℃;
(5) with saline cistanche cell slurries, or merging smudge cells cleaning solution, or the saline cistanche extract behind the instantaneous enzyme that goes out of superhigh temperature, adopt common industrial membrane separating technology, sieve and hold back and remove big molecular impurity by milipore filter fenestra selectivity, or further sieve and hold back and remove small molecular weight impurity by the NF membrane selectivity, separate the saline cistanche active material extract that obtains being rich in benzyl carbinol glycosides compounds and iridoid glycoside compounds; The relative molecular mass of the milipore filter that adopts is 1000～3000, and the relative molecular mass of NF membrane is 200～300;
(6) adopt common industrial vacuum concentration technology, or the industrial film evaporating and concentrating process, temperature is 45 ℃～65 ℃, obtaining solid content is the cistanche salsa extract concentrate of 20%～75% weight ratio;
(7) with the cistanche salsa extract concentrate, adopt common industrial drying process with atomizing, or three sections drying process with atomizing carry out drying, utilize high temperature drying hot gas that the instantaneous processing of concentrate superhigh temperature of atomizing is made the enzyme activity forfeiture and the temperature that obtains the effect of the instantaneous drying of superhigh temperature is 125 ℃～285 ℃; Perhaps further dehydrate through the cistanche salsa extract of second section drying tower body dry section with powdery; Perhaps cool off and the agglomeration granulation through the cistanche salsa extract of the 3rd section dry section again, obtain to be the cistanche salsa extract of fine granularity powdery;
(8) above system integration technology flow process was finished in 15～60 minutes; Measure by analysis, benzyl carbinol glycosides compounds and iridoid glycoside kind compound content 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 of wherein weighing the saline cistanche quality reach 15%～23.4% weight ratio in the dry productive rate, and moisture is 0.5%～2.8% weight ratio.
2. in accordance with the method for claim 1, it is characterized in that the saline cistanche described in the step (1) is Orobanchaceae plant (Orobanchaceae) saline cistanche or claims Desert Herba Cistanches (Cistanche deserticola Y.C.Ma), Cistanche tubulosa (Cistanche tubulosa (Schrenk) R.Wight), spend salt desert cistanche (Cistanche salsa var.albiflora P.F.Tu etZ.C.Lou) in vain, the husky raw meat desert cistanche (Cistanche sinensis G.Beck) of salt raw meat desert cistanche (Cistanche salsa (C.A.Mey) G.Beck) and husky desert cistanche or title is selected one or more for use.
3. in accordance with the method for 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 refrigeration is-52 ℃～-10 ℃; In the saline cistanche raw material, charge into liquid nitrogen or CO described in the step (2)
2Concentration be 0.1%～5.0% weight ratio, 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 ℃; The addition of the ascorbic acid of the interpolation trace that adopts, citric acid, glucolactone, sodium sulfite is 0.001%～0.03% weight ratio.
4. in accordance with the method for claim 1, it is characterized in that described in the step (3) in filter 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 precooling.
5. in accordance with the method for claim 1, it is characterized in that the fresh-keeping storehouse temperature of described industrial freezer is 4 ℃～10 ℃, the storehouse temperature of industrial freezer refrigeration is-36 ℃～-18 ℃; Cold water water temperature in the tank is 4 ℃～10 ℃; In the saline cistanche raw material, charge into liquid nitrogen or CO
2Concentration be 0.5%～1% weight ratio; In the saline cistanche raw material, add CO
2The frozen water temperature is 4 ℃～6 ℃; CO
2CO in the frozen water
2Concentration is 1%～2% weight ratio; The addition of the ascorbic acid of the interpolation trace that adopts, citric acid, glucolactone, sodium sulfite is 0.002%～0.004% weight ratio.
6. in accordance with the method for claim 1, it is characterized in that described in filter 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 precooling; Water temperature through the technical pure water purification of precooling is 4 ℃～10 ℃.
7. in accordance with the method for claim 1, it is characterized in that selectivity screening that described industrial membrane separating technology device is selected for use and the relative molecular mass of holding back the milipore filter of macromolecular substances are 1500～2500; The relative molecular mass that the small-molecule substance NF membrane was sieved and held back to selectivity is 210～250.
8. in accordance with the method for claim 1, it is characterized in that it is 190 ℃～230 ℃ that the instantaneous superhigh temperature of the spray-drying described in the step (7) is handled the temperature that makes the enzyme activity forfeiture and obtain the effect of the instantaneous drying of superhigh temperature.
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| CN101629200B (en) * | 2009-08-04 | 2012-01-11 | 中山大学 | Method for producing acteoside by fresh herba cistanches |
| CN101629198B (en) * | 2009-08-04 | 2011-12-21 | 中山大学 | Method for producing monomeric compounds of acteoside |
| CN103815405B (en) * | 2014-03-07 | 2015-08-12 | 安徽普朗膜技术有限公司 | The production system of cistanche extracts |
| CN104189099A (en) * | 2014-06-17 | 2014-12-10 | 新疆医科大学 | Application of cistanche phenylethanoid glycoside extractive to control altitude sickness |
| CN106334001A (en) * | 2016-09-30 | 2017-01-18 | 宁夏医科大学 | Application of cistanche phenylethanoid glycosides effective part in preparation of bone formation accelerating drug and drug composition |
| CN108640955A (en) * | 2018-04-26 | 2018-10-12 | 中国农业科学院特产研究所 | A method of extraction prepares crenatoside from bend pipe broomrape |
| CN111280354A (en) * | 2020-03-11 | 2020-06-16 | 王磊 | Cistanche glycolipid metabolism balance nutrition beverage and preparation method thereof |
| CN115068520A (en) * | 2022-06-09 | 2022-09-20 | 新疆汇峰农业科技有限公司 | Bitter removing method for primary cistanche pulp |
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