CN102716175A - Superfine eucommia ulmoides powder and preparation method thereof - Google Patents
Superfine eucommia ulmoides powder and preparation method thereof Download PDFInfo
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- CN102716175A CN102716175A CN2012102301894A CN201210230189A CN102716175A CN 102716175 A CN102716175 A CN 102716175A CN 2012102301894 A CN2012102301894 A CN 2012102301894A CN 201210230189 A CN201210230189 A CN 201210230189A CN 102716175 A CN102716175 A CN 102716175A
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Abstract
The invention relates to a superfine eucommia ulmoides powder and a preparation method thereof. The preparation method is characterized by comprising the following steps of performing freeze drying on fresh eucommia ulmoides bark by combining the vacuum freeze drying process technology with the supersonic airflow low-temperature grinding process technology; then, sealing; and crushing at the very first time to directly prepare the eucommia ulmoides bark into the superfine eucommia ulmoides powder. According to the preparation method, the eucommia ulmoides bark is directly prepared into the freeze-drying superfine eucommia ulmoides powder by adopting the international advanced vacuum freeze drying ultrafine grinding process technology. The original biological enzyme, the protein, the amino acid, the vitamin and the thermosensitive effective component of eucommia ulmoides are kept to the maximum limit, so that the nutritional value and the drug action of the active freeze-drying eucommia ulmoides are improved, and the freeze-drying eucommia ulmoides powder is far superior to traditional eucommia ulmoides powders prepared by drying in the sun and heated-air drying.
Description
Technical field
The present invention relates to a kind of ultra-fine Cortex Eucommiae powder and method for preparing, relate in particular to and adopt the vacuum lyophilization superfine technique to realize the preparation of the superfine powder of the Chinese medicine Cortex Eucommiae, belong to the application of vacuum lyophilization superfine powder in food and medicine.
Background technology
The Cortex Eucommiae is a kind of traditional rare Chinese medicine, and the Cortex Eucommiae is a kind of Eucommiaceae medicinal plants, deciduous tree, and the bark taupe, coarse, all contain gutta-percha together with branch, leaf, root, especially bark fractures and has drawn back many silvery white filaments.Ancient Chinese is all classified as top grade for Shennong's Herbal, Ming Dynasty's Li Shizhen (1518-1593 A.D.) work Compendium of Material Medica.Cortex Eucommiae sweet in the mouth, warm in nature, the function invigorating the liver and kidney, bone and muscle strengthening, antiabortive.Be sweet Wen Huayang, invigorating the liver and kidney, bone and muscle strengthening, strong waist knee joint can be treated lumbago due to renal deficiency and gynecologic menstrual lumbago, is the key medicine of treatment lumbago; Again can invigorating the liver and kidney, Gu Chong appoints, and can treat deficiency of the liver and kindey, the frequent fetal movement of the debility of CHONG and REN meridians.
Modern medicine research, the chemical constituent of the Cortex Eucommiae contains 15 kinds of inorganic elementss such as Cortex Eucommiae glycosides, pinoresinol diglucoside, aucubin, tannin, flavone compound and germanium, selenium, compositions such as micro-alkaloid and vitamin C.Have effects such as blood pressure lowering, blood vessel dilating, enhance immunity, calmness, analgesia, anti-stress, diuresis, slow down aging.
In recent years, the bark of eucommia is very praised highly by Japan, not only in the Chinese prescription medicine, widely uses, and has also developed bark of eucommia face, health products such as bark of eucommia tea.Specifically Eucommia face a lot of promotion, sales of 200 million packages a year is huge (103 g / bag), called longevity noodles, have lower blood pressure anti-stroke, light hand foot health, anti-aging effect.Japan does not produce the Cortex Eucommiae, and raw material is all from China.The Cortex Eucommiae mainly originates in ground such as Chinese Sichuan, Chongqing, Yunnan, Guizhou, Shaanxi, Hubei.
China Shanghai famous Chinese medicine enterprise Leiyunshang Pharmaceutical Co., Ltd. is by health Chinese traditional patent formulation WS3-B-3107-98 promulgated by the ministries or commissions of the Central Government operative norm; Developed powerful gastrodia elata-cortex capsule (the accurate word Z31020332 of traditional Chinese medicines); Have several the invigorating blood circulation of loosing; Muscles and tendons relaxing to alleviate pain cures mainly and is used for wind-induced ache tendon and vessel, numb limbs and tense tendons, walking disorder, waist and leg ache, symptoms such as headache and dizziness.
But pulverize after at present both at home and abroad the preparation of Cortex Eucommiae powder body is general heated drying, granule is all thicker, and detail position particle diameter 80～120 orders (～200 μ m) have a strong impact on the utilization rate of result of use and spice.Show to have only meta particle diameter to reach below the fineness of 10～15 μ m, at this moment the sporoderm-broken rate of crude drug cell >=95% through research in recent years when the Chinese medicine powder body.Experiment showed, take the Chinese medicine superfine powder after, intracellular effective ingredient needn't be again need could be absorbed by medicine-feeding part through the barrier that cell wall and cell membrane are set up, but directly and the medicine-feeding part absorbing contacting; Simultaneously; The specific surface area of Chinese medicine superfine powder is very big, and is big with the medicine-feeding part contact area, and its adhesion property makes the time lengthening of medicine at absorption site; Therefore can improve the infiltration rate and the degree of absorption of effective ingredient greatly, thereby reach quick-acting, efficient, long lasting therapeutic effect.Therefore develop better efficacy, the Chinese medicine superfine powder new product that kind is more excellent, new material, the novel form of formation Chinese medicine will have far-reaching theory and realistic meaning.State Scientific and Technological Commission and State Administration of Traditional Chinese Medicine list it in one of " 21 century modernization of Chinese medicine development strategy ".
The present invention plans the Cortex Eucommiae and adopts advanced in the world vacuum lyophilization to combine to process the ultra-fine Cortex Eucommiae powder body of vacuum lyophilization with the supersonic airstream freeze grinding technology, is expected to become novel healthy food and medicine, thereby is guided out the object of the invention.
Summary of the invention
The object of the present invention is to provide a kind of ultra-fine Cortex Eucommiae powder and method for preparing; Described preparation method characteristic is the vacuum freeze-drying technique technology is combined with supersonic airstream cryogenic crushing process technology; Directly with after the fresh eucommia bark lyophilization; Outlet sealing back is pulverized in the very first time and is processed ultra-fine Cortex Eucommiae powder, and the fineness of prepared ultra-fine Cortex Eucommiae powder is 1000 orders, and the meta particle diameter is 10～15 μ m.
Described vacuum lyophilization is containing the large quantity of moisture material; Lowering the temperature in advance is frozen into solid, under the condition of vacuum, water vapour is directly distilled then, and in the left ice shelf when freezing of material itself; Therefore its dry back constancy of volume loose porously will absorb heat when distillation.Cause decline and the rate of sublimation that slows down of product self-temperature,, shorten drying time, must suitably heat product in order to increase rate of sublimation.Whole drying is under lower temperature, to carry out.
Lyophilization has following characteristics:
One, lyophilization is carried out at low temperatures, and therefore the material for many thermal sensitivitys is particularly suitable for.Degeneration can not take place or lose biologos like protein, microorganism and so on, therefore pharmaceutically used widely.
When two, dry at low temperatures, some volatile ingredients losses in the material are very little, are fit to some chemical productss, medicine and food drying.
Three, in freezing dry process, the effect of microbial growth and enzyme can't be carried out, and therefore can keep the original character of material.
Four, owing under the state that freezes, carry out drying, so volume is almost constant, has kept original structure, concentration phenomena can not take place.
Five, dried matter is loose porous, is spongy, adds that dissolving almost recovers original character rapidly and fully immediately behind the water.
Six, because drying is carried out under vacuum, oxygen is few, so the material of some easy oxidations has obtained protection.
Seven, drying can be got rid of the moisture content more than 95～99%, makes dry products ability long preservation and unlikely going bad.
The Cortex Eucommiae is the very strong bark tablet of a kind of cellulose, like the drying means that uses with common Chinese medicine preparation, can not pulverize, and its water content is generally about 45%～50%.To Cortex Eucommiae directly be ground into micropowder, very difficult, and be not ground into micropowder, human body also is difficult for absorbing.The present invention is the dewatering that utilizes vacuum lyophilization, and Cortex Eucommiae Cortex Dictamni is carried out lyophilizing dehydration, only contains minimum moisture content (generally can reach＜below 2%) after will dewater, more this Cortex Eucommiae that extremely loosens of organizing is carried out superfine grinding.Can obtain superfine Cortex Eucommiae powder, the dissolubility of this superfines is fabulous, and the active ingredient in the Cortex Dictamni keeps intact.Through freeze dried ultra-fine Cortex Eucommiae powder and the contrast of traditional Cortex Eucommiae powder, no matter be on the quality composition, or incomparable advantage is all arranged on the fineness.
During vacuum lyophilization, at first because the fresh Cortex Eucommiae is the plant lamellar structure, there is not the solution tissue in the eutectic point of the GPRS Cortex Eucommiae, so eutectic point can be too not low, can goods pre-freeze temperature be reduced to below-20 ℃ and gets final product.Vacuum is adjusted in about 40～60Pa.One helps conduction of heat, and two help the overflow of vapour pressure.Maximum temperature should be controlled at about 40～50 ℃, the too high ecosystem color and the morphological element that can influence Cortex Eucommiae of temperature.To dry outlet, generally be no more than 20 hours from fresh Cortex Eucommiae inlet, after the Cortex Eucommiae sealing behind the outlet, pulverize immediately, use supersonic airstream low temperature powder machine to pulverize during pulverizing in the very first time.
A kind of in the jet mill commonly used of supersonic airstream pulverize at low temperature used in the present invention, described jet mill is the equipment through the dry process micropowder of comminution by gas stream material, therefore is called airflow milling, jet mill or fluence mill again.Used gas can be high-speed air (300～500m/s), superheated steam (300～400 ℃) or noble gas; At present; The method for preparing powder body mainly contains two kinds: a kind of is that energy through air-flow makes material particles impact mutually, collide, rub and pulverized, and prepares granule from big to small; Another kind is through the synthetic granule for preparing from small to large.Granule through the breaking method preparation the most carefully is about 0.1 μ m at present, and synthetic method can prepare the granule of several nanometers to tens micrometer ranges.Jet mill mainly can prepare the ultra-fine grain material of 0.5～20 μ m through the method for pulverizing.It is the equipment of the dry process superfine powder that is widely used at present, compares with other disintegrating apparatus, and it has following characteristics:
1, fine size the most carefully can reach 0.1 μ m, is generally 0.5～20 μ m, and can regulates, and comminution ratio is 1～10;
2, narrow particle size distribution, even can satisfy the requirement of narrow particle size distribution product powder, like abrasive material, medicine, laser printing powder, duplicating powder, NdFeB magnetic powder and lithium battery etc.;
3, cavity is few to contamination of products in operating process, purity is high, as can reach aseptic pulverizing when taking certain measure, therefore, is specially adapted to medicine etc. and does not allow by the material grinding of metal and other contaminating impurity;
4, can pulverize Mohs' hardness is 1～10 material;
5, processing temperature low (being lower than gas flow temperature), the strain rate during material fragmentation is high, is specially adapted to low melting point.
Flat jet mill mainly is made up of flat-disk cavity operating room, nozzle, feeder, finished powder outlet, air chamber and operating room's liner.
Nozzle generally all is installed in the centre position of operating room's sidewall, and nozzle-axis has an angle (30 °～58 °) with corresponding radius
The jet expansion speed of flat jet mill has three kinds of subsonic speed, velocity of sound and supersonic speed.Subsonic nozzle is directly tubular, and sonic nozzle is a tapered, and superonic flow nozzzle is reducing and expansion shape (Laval nozzle), and at present the tapered nozzle is with the most use, straight tubular usefulness seldom now, and the utility ratio of reducing and expansion shape nozzle is improving.
The number of flat comminution by gas stream machine nozzle is mainly confirmed according to the form of working medium air consumption, operating room's diameter and nozzle.Under the condition of space, operating room permission, how relatively good general number of nozzle is, helps classification.
Because flat jet mill operating room liner receives material and jet serious wear, generally inwall will paste the wear-resistant liner material in the operating room, is mainly low wear materials such as wear-resisting alloy steel, corundum and carborundum.
The operation principle of jet mill recited above is:
Compressed Gas evenly gets into each nozzle by air chamber, and the nozzle high-speed jet of gushing out is because jet pressure is low; Powder in the operating room just is involved in or sucks jet, and granule is accelerated with jet, and band material jet makes granule collide each other, rub; Also collide each other and rub, cause grain breakage with liner.Because being band α angle, jet sprays into the operating room; It can form the flow field of a high speed rotating automatically; Granules all in the operating room all is in the centrifugal force field; Fine grained can overcome centrifugal force and export away from middle finished powder, is collected as finished powder, and the granular size of finished product is relevant with effluxvelocity, entering angle α, the diameter D of operating room, outlet diameter etc.
Flat jet mill is specification standards with the pulverizing chamber internal diameter size, modular system φ 50～1060mm; Compressed air consumption 0.566～94m
3/ min; Superheated steam consumption 147～3630kg/h; Production capacity 0.2～2500kg/h, product cut size 0.5～43 μ m.
Advantage of the present invention is conspicuous:
1, Cortex Eucommiae raw material directly originate in our company in Sichuan, pollution-free base, Chongqing, do not use the chemical fertilizer medicine in the production, meet national environment protection requirement, reach export standard.
2, advanced in the world " vacuum lyophilization superfine grinding " technology and technology is adopted in processing, directly eucommia bark is processed the ultra-fine full Cortex Eucommiae powder body of lyophilizing.This does to keep to greatest extent to Cortex Eucommiae primitive organism enzyme, protein, aminoacid, vitamin, temperature-sensitive effective ingredient, and this nutritive value and drug effect with active lyophilizing Cortex Eucommiae improved, be much better than traditional dry, the Cortex Eucommiae powder of hot air drying system training.Pulverize through the Cortex Eucommiae low temperature ultrahigh speed gas flow process of vacuum lyophilization, its fineness can reach 1000 orders (about meta particle diameter 10-15 μ m), can increase operation rate greatly and the absorption of human body effect of effective ingredient.Reach effects such as consumption is few, instant effect.Be superior to common heat commonly used and do Cortex Eucommiae powder body (having only tens orders).
Description of drawings
Fig. 1 adopts the particle size distribution of the Rhizoma Gastrodiae superfine powder of process preparation of the present invention.
Electron scanning micrograph under the different amplification of Fig. 2 preparation; (a) 1000 times; (b) 4000 times.
The specific embodiment
Pass through embodiment below with further elaboration substantive distinguishing features of the present invention and obvious improvement, but the present invention only is confined to embodiment by no means.
Embodiment 1:
With the eucommia bark tablet of adopting in the base, Sichuan; Through measuring its water content is 45～50%, and the model that adopts Yucheng Driers Co Ltd, Shanghai to produce is that YRD-1030 type vacuum dryer carries out drying, and selecting the pre-freeze temperature of the Cortex Eucommiae is-20 ℃; Vacuum is adjusted to 45～55Pa; The vacuum drying temperature is controlled at 40～45 ℃, dry 15～18 hours, the water content after the Cortex Eucommiae is dewatered is controlled at less than below 2%; Put into jet mill in the very first time after the sealing then and pulverize, homemade flat jet mill is a STG-10 series.The operating room's diameter that uses during comminution by gas stream is φ 100～150mm, and number of nozzle is 4, and the angle between nozzle-axis and operating room's radius is 30 °-50 °, and nozzle is installed in the centre position of operating room.Production capacity is 10～20kg/h, and the meta particle diameter of product is about about 10-15 μ m.
Embodiment 2:
The water content of initial eucommia bark tablet is 45%～50%, and the pre-freeze temperature is to-30 ℃, baking temperature to 50 ℃, and the later stage of drying resolution phase prolongs 2 hours, 20 hours altogether, records Cortex Eucommiae water content after the dehydration below 1%.The particulate meta particle diameter of gained is at the 10-12 mu m range after crushed, and all the other are with embodiment 1.
From above 2 embodiment, the water content after the lyophilization is lower, and dehydration is more thorough, and goods are pulverized easily.
Claims (6)
1. the method for preparing of ultra-fine Cortex Eucommiae powder is characterized in that the vacuum freeze-drying technique technology is combined with supersonic airstream cryogenic crushing process technology, directly with after the fresh eucommia bark lyophilization, is sealed in the very first time to pulverize and process ultra-fine Cortex Eucommiae powder.
2. by the described method of claim 1, it is characterized in that step is:
A) adopt vacuum freeze to carry out drying fresh eucommia bark tablet; The pre-freeze temperature is reduced to below-20 ℃; Vacuum is adjusted in the 40-60Pa scope; The vacuum drying temperature is controlled at 40-50 ℃, make the flaky Cortex Eucommiae of bark dehydration back water content be controlled at＜below 2%, dry then outlet sealing;
B) put into flat jet mill immediately after the sealing and pulverize in the very first time, pulverize and use flat jet mill, the operating room's diameter that uses during pulverizing is Φ 100-150mm, and number of nozzle is 4, is ground into superfine Cortex Eucommiae powder.
3. by claim 1 or 2 described methods, the model of the vacuum freeze that it is characterized in that using is the YRD-1030 type.
4. by the described method of claim 2, it is characterized in that:
A) fresh eucommia bark tablet water content is 45-50%;
B) be no more than 20 hours from fresh eucommia bark tablet inlet pre-freeze to the dry outlet time;
Angle when c) pulverizing between nozzle and operating room's radius is 30 °-50 °, and nozzle is installed in the centre position of operating room.
5. by the Cortex Eucommiae powder of each described method preparation in the claim 1,2 or 4, the fineness that it is characterized in that described Cortex Eucommiae powder is 1000 orders.
6. by the described Cortex Eucommiae powder of claim 5, the meta particle diameter that it is characterized in that described Cortex Eucommiae powder is 10-15 μ m.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104142046A (en) * | 2014-08-25 | 2014-11-12 | 济南康众医药科技开发有限公司 | Method for drying eucommia ulmoides |
| CN104142047A (en) * | 2014-08-25 | 2014-11-12 | 济南康众医药科技开发有限公司 | Eucommia freeze-drying method |
| CN105456078A (en) * | 2015-06-26 | 2016-04-06 | 普正药业股份有限公司 | Cortex eucommiae exfoliating abrasive particles and preparation method and application thereof |
-
2012
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Non-Patent Citations (2)
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| 孙企达: "真空冷冻干燥技术在发展超微生物材料中的应用", 《第2届中国食品冷藏链新设备、新技术论坛文集》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104142046A (en) * | 2014-08-25 | 2014-11-12 | 济南康众医药科技开发有限公司 | Method for drying eucommia ulmoides |
| CN104142047A (en) * | 2014-08-25 | 2014-11-12 | 济南康众医药科技开发有限公司 | Eucommia freeze-drying method |
| CN105456078A (en) * | 2015-06-26 | 2016-04-06 | 普正药业股份有限公司 | Cortex eucommiae exfoliating abrasive particles and preparation method and application thereof |
| CN105456078B (en) * | 2015-06-26 | 2018-01-23 | 普正药业股份有限公司 | A kind of bark of eucommia exfoliating abrasive particle and preparation method and application |
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