Background technology
Superfine communication technique is a special kind of skill emerging in recent years, and raw material can be processed into the even nano level super fine of micron by it, is used widely in all trades and professions.In recent years, developing rapidly and interdisciplinaryly to interpenetrate along with modern industrial technology and medical science, the application of superfine technique in Chinese medicine processing more and more causes the concern of people, and Traditional Chinese Medicine is just experiencing huge change.For adapting to the demand of the modernization of Chinese medicine, the preparing new-type medical herbs drink tablets that superfine communication technique basis is developed-Chinese medicine ultra-fine powder decoction pieces arises at the historic moment, it had both maintained the composition qualities of Chinese medicine decoction pieces, also possessed the administration form of modern Chinese medicine, was a kind of novel, efficient modern CMM processing piece.
Herba Dendrobii (Dendrobium officinale Kimura et Migo) is the orchid family Dendrobium Sw, is one of orchid recorded the earliest in China's ancient documents.The kind of Herba Dendrobii, just there is kind more than 1500 in the whole world, and China about has 76 kinds.Herba Dendrobii is the kind that wherein the famousst and precious, medical value is the highest, Shennong's Herbal is classified as top grade, point out Herba Dendrobii have promote the production of body fluid, quench the thirst, effect of edema of easing pain, eliminate, cure mainly the calentura deficiency of YIN, order be dark, stomach is weak, the disease such as hoarseness,, hoarseness tired to vocal cords, recovering its U.S. sound has special efficacy.Herba Dendrobii is classified as first of China's nine large Herba mesonae chinensis by Taoist school's ancient books and records " Taoist Scriptures ".Modern study shows, the main component of Herba Dendrobii comprises polysaccharide, alkaloid, stilbenes compound, sesquiterpenoids, phenolic acid, lignanoids etc.The polysaccharide composition of Herba Dendrobii can promote humoral immunity of organism, cellular immune function and induce cytokine profiles to have the effect of enhancing human body immunity power, and stilbenes compound then has obvious antitumor action.Dendrobium candidum tissue culture has the ability of stronger Scavenger of ROS, by significantly improving superoxide dismutase (SOD) level, reducing lipid peroxide (LPO) effect, finally removing interior free yl.Herba Dendrobii also has the effects such as resisting fatigue, blood sugar lowering, eliminating phlegm and relieving cough, is all widely used in the auxiliary treatment, chronic gastritis, diabetes, chronic pharyngitis, weakness due to chronic disease immunologic hypofunction, eye health etc. of malignant tumor.
Because Herba Dendrobii natural propagation rate is extremely low, adds people and excavate without limit for a long time, cause this species wild resource seriously poor, be listed in national secondary endangered protective plant at present.Although artificial growth scale constantly expands in recent years, its price still remains high.The traditional diamond-making technique of Herba Dendrobii, usually adopt cure, the method such as curling, oven dry is processed into Herba Dendrobii extract.Part effective ingredient is destroyed in the course of processing.And after being processed into Herba Dendrobii extract, owing to containing a large amount of phlegmatic temperaments and polysaccharide in Herba Dendrobii, during decocting, effective ingredient is difficult to fried, also has more effective ingredient to stay in medicinal residues, causes waste.For promoting active ingredient absorption in vivo, improve utilization rate and the extraction efficiency of drug resource, the research broken to dendrobium candidum ultrafine powder is necessary very much.
A kind of processing method of dendrobium candidum ultrafine powder of the disclosure of the invention of CN102380043A, the Herba Dendrobii cleaned up is put into high steam pot complete, complete and terminate to cut off, Herba Dendrobii after cut-out is put into baking box to be baked to constant weight, be crushed to all by the coarse powder of a sieve, pulverized by high-frequency resonance grinder again, till all by 900 eye mesh screens, namely obtain the micropowder of 12-18 μm.The technology of this invention extends product storage life, improves stripping and the absorption of effective ingredient, but owing to adopting high steam to complete, the high temperature processing links such as baking box oven dry, heat-labile effective ingredient is destroyed, and reduces curative effect.
CN102552699A has invented a kind of preparation method of dendrobium candidum ultrafine powder, iron-sheet dendrobe fresh product stem section is cleaned, drains away the water; The Herba Dendrobii drained away the water is placed in freeze drying equipment, at-30 ± 5 DEG C of pre-freeze 1-3h, when temperature drops to-35 DEG C, constant temperature 2-4h; When low temperature, dried Herba Dendrobii nano-machine pulverizer is pulverized, is prepared into nano-particle.This invention improves stripping and the absorption of effective ingredient, extends product storage life, but owing to taking co-60 radiation sterilizing, some compositions of plant can be destroyed, and co-60 radiation sterilizing, although effective, sterilizing is convenient, but must indicate through radiation sterilization on the packaging according to relevant laws and regulations.
Summary of the invention
The object of this invention is to provide a kind of preparation method of dendrobium candidum ultrafine powder, the method is carried out at low temperatures, effectively can keep the activity of Herba Dendrobii functional component, the mean diameter of obtained dendrobium candidum ultrafine powder can reach 10-300 nanometer, can significantly improve stripping and the absorption of wherein effective ingredient.
For achieving the above object, the present invention adopts following technical scheme:
A preparation method for dendrobium candidum ultrafine powder, comprises the steps:
1) pretreatment: get fresh Herba Dendrobii medical material, removing impurity, washes, cuts into chunks;
2) freezing: the Herba Dendrobii section that step (1) obtains spread out and carry out freezing, cryogenic temperature is-5 ~-40 DEG C;
3) pulverize at low temperature: Herba Dendrobii section step (2) obtained is pulverized under the cryogenic conditions of-5 ~-40 DEG C, sieves, and obtains 40 ~ 100 object coarse powder;
4) low-temperature vacuum microwave is dry: the Herba Dendrobii coarse powder that step (3) obtains is carried out low-temperature vacuum microwave drying, obtains Herba Dendrobii xeraphium; Wherein microwave power: 1 ~ 15kw, temperature :-5 ~-40 DEG C, vacuum: 0.04 ~ 0.09Pa, microwave drying total time: 0.2 ~ 2h;
5) low temperature supersonic jet mill: the Herba Dendrobii xeraphium that step (4) obtains is carried out superfine grinding in low temperature supersonic jet mill under the cryogenic conditions of 0 ~-40 DEG C, to 300 orders, obtains dendrobium candidum ultrafine powder;
6) co-vibration mill is pulverized: the dendrobium candidum ultrafine powder that step (5) obtains is carried out micronizing in co-vibration mill, temperature controls below 30 DEG C, make its particle diameter reach (detection of its particle diameter can be detected by the method such as scanning electron microscope, laser particle analyzer) between 10 ~ 300 nanometers, obtain superfine powder;
7) subpackage and packaging: get the superfine powder that step (6) is obtained, carry out subpackage in aseptic subpackaged room after microwave sterilizating, carry out subpackage and outer package according to the specification of often wrapping 1 ~ 5 gram, obtained dendrobium candidum ultrafine powder finished product.
The herb that the fresh Herba Dendrobii medical material that the present invention uses is Herba Dendrobii.
As preferably, interval 30 ~ 90s is taked in microwave drying process in step (4), the microwave treatment mode (namely often heat 30 ~ 60s just to stop heating 30 ~ 90s and then continue heating 30 ~ 60s stopping heating 30 ~ 90s again, circulate successively) of heating 30 ~ 60s.Such operation is heated too fast in order to avoid dendrobium officinale powder and destroys effective ingredient and coking, and the total time of microwave treatment was at 0.2 ~ 2 hour.
As preferably, in step (7), aseptic subpackaged room temperature is at 18 ~ 26 DEG C, and relative humidity is below 65%.The object of such process avoids powder moisture absorption and microbiological contamination.
As preferably, the microwave sterilizating described in step (7) is sterilizing 2 ~ 10min under the microwave condition of power 1 ~ 3kw, frequency 2450 ~ 3000MHz.
The dendrobium candidum ultrafine powder that the present invention obtains can directly be taken, and also can be processed further by techniques such as extracting and developing again, can improve extraction efficiency, reduces production cost.In addition, the dendrobium candidum ultrafine powder that the present invention obtains can also use as prepared slices of Chinese crude drugs compatibility.
Compared with prior art, the present invention has following obvious advantage: 1, the inventive method makes the mean diameter of dendrobium candidum ultrafine powder reach 10 ~ 300 nanometers, make the cell wall of Herba Dendrobii by complete breaking cellular wall, various compositions contained in Herba Dendrobii plant cell are allowed to discharge completely, very big raising penetration, increase the absorption of active ingredient, be beneficial to the performance of its drug effect; 2, preparation process of the present invention is carried out at low temperatures, prevents high temperature from causing effective ingredient inactivation, fully maintains the activity of Herba Dendrobii functional component, can ensure the drug effect of Herba Dendrobii; 3, do not add any adjuvant in the course of processing, use pure physical method processing, ensure that the pure of goods; 4, in the course of processing, Herba Dendrobii consumes less, and yield is high, saves Herba Dendrobii resource; 5, product stock is convenient, is convenient to application, is easy to molding and steady quality.
Detailed description of the invention
Below by specific embodiment, technical scheme of the present invention is described in further detail, but protection scope of the present invention is not limited thereto.
In the present invention, if not refer in particular to, the raw material adopted and equipment etc. all can be buied from market or this area is conventional.Method in following embodiment, is the conventional method of this area if no special instructions.
Embodiment 1:
1) pretreatment: get fresh Herba Dendrobii medical material, removing impurity, washes, is cut into 2 ~ 4cm section;
2) freezing: the Herba Dendrobii section that step (1) obtains spread out and carry out freezing, cryogenic temperature is-5 DEG C.
3) pulverize at low temperature: the Herba Dendrobii section that step (2) obtains pulverized under the cryogenic conditions of-5 DEG C, sieve, obtains 40 ~ 100 object coarse powder.
4) low-temperature vacuum microwave is dry: the Herba Dendrobii coarse powder that step (3) obtains is carried out low-temperature vacuum microwave drying, power-on, adjustment microwave power: 1kw, microwave drying total time, 2h, baking temperature :-5 DEG C; Vacuum: 0.04Pa.Interval 30s can be taked, the microwave treatment mode (namely often heat 30s just to stop heating 30s and then continue heating 30s stopping again heating 30s, circulate successively) of heating 30s in microwave drying process.
5) low temperature supersonic jet mill: Herba Dendrobii xeraphium step (4) obtained carries out superfine grinding, to 300 orders under the cryogenic conditions of 0 DEG C.
6) co-vibration mill is pulverized: the dendrobium candidum ultrafine powder that step (5) obtains is carried out nano-pulverization in co-vibration mill, temperature controls below 30 DEG C, makes its particle diameter reach (detection of its particle diameter can be detected by the method such as scanning electron microscope, laser particle analyzer) between 10 ~ 300 nanometers.
7) subpackage and packaging: get the dendrobium candidum ultrafine powder that step (6) is obtained, through power 1kw, under the condition of frequency 2450MHZ after microwave sterilizating sterilizing 2min temperature 18 ~ 26 DEG C, subpackage is carried out in the aseptic subpackaged room of humidity less than 65%, subpackage and outer package is carried out, obtained finished product according to the specification of often wrapping 1 ~ 5 gram.
Embodiment 2:
1) pretreatment: get fresh Herba Dendrobii medical material, removing impurity, washes, is cut into 2 ~ 4cm section;
2) freezing: the Herba Dendrobii section that step (1) obtains spread out and carry out freezing, cryogenic temperature is-40 DEG C.
3) pulverize at low temperature: the Herba Dendrobii section that step (2) obtains pulverized under the cryogenic conditions of-40 DEG C, sieve, obtains 40 ~ 100 object coarse powder.
4) low-temperature vacuum microwave is dry: the Herba Dendrobii coarse powder that step (3) obtains is carried out low-temperature vacuum microwave drying, power-on, adjustment microwave power: 15kw, microwave drying total time, 0.5h, baking temperature :-40 DEG C; Vacuum: 0.09Pa.Interval 30s can be taked, the microwave treatment mode (namely often heat 30s just to stop heating 30s and then continue heating 30s stopping again heating 30s, circulate successively) of heating 30s in microwave drying process,
5) low temperature supersonic jet mill: the Herba Dendrobii xeraphium that step (4) obtains is carried out low temperature supersonic jet mill, to 300 orders under the cryogenic conditions of-40 DEG C.
6) co-vibration mill is pulverized: the dendrobium candidum ultrafine powder that step (5) obtains is carried out nano-pulverization in co-vibration mill, temperature controls below 10 DEG C, makes its particle diameter reach (detection of its particle diameter can be detected by the method such as scanning electron microscope, laser particle analyzer) between 10 ~ 300 nanometers.
7) subpackage and packaging: get the superfine powder that step (6) is obtained, through power 1kw, under the condition of frequency 2450MHZ after microwave sterilizating sterilizing 2min temperature 18 ~ 26 DEG C, subpackage is carried out in the aseptic subpackaged room of humidity less than 65%, subpackage and outer package is carried out, obtained finished product according to the specification of often wrapping 1 ~ 5 gram.
Embodiment 3:
1) pretreatment: get fresh Herba Dendrobii medical material, removing impurity, washes, is cut into 2 ~ 4cm section;
2) freezing: the Herba Dendrobii section that step (1) obtains spread out and carry out freezing, cryogenic temperature is-20 DEG C.
3) pulverize at low temperature: the Herba Dendrobii section that step (2) obtains pulverized under the cryogenic conditions of-20 DEG C, sieve, obtains 40 ~ 100 object coarse powder.
4) low-temperature vacuum microwave is dry: the Herba Dendrobii coarse powder that step (3) obtains is carried out low-temperature vacuum microwave drying, power-on, adjustment microwave power: 6kw, microwave drying total time: 1h, baking temperature :-20 DEG C; Vacuum: 0.06Pa.Interval 30s can be taked, the microwave treatment mode (namely often heat 30s just to stop heating 30s and then continue heating 30s stopping again heating 30s, circulate successively) of heating 30s in microwave drying process.
5) low temperature supersonic jet mill: the Herba Dendrobii xeraphium that step (4) obtains is carried out superfine grinding, to 300 orders under the cryogenic conditions of-20 DEG C.
6) co-vibration mill is pulverized: the dendrobium candidum ultrafine powder that step (5) obtains is carried out micronizing in co-vibration mill, temperature controls below 20 DEG C, makes its particle diameter reach (detection of its particle diameter can be detected by the method such as scanning electron microscope, laser particle analyzer) between 10 ~ 300 nanometers.
7) subpackage and packaging: get the superfine powder that step (6) is obtained, through power 1kw, under the condition of frequency 2450MHZ after microwave sterilizating sterilizing 2min temperature 18 ~ 26 DEG C, subpackage is carried out in the aseptic subpackaged room of humidity less than 65%, subpackage and outer package is carried out, obtained finished product according to the specification of often wrapping 1 ~ 5 gram.
Comparative example 1:
1) pretreatment: get fresh Herba Dendrobii medical material, removing impurity, washes, is cut into 2 ~ 4cm section;
2) freezing: the Herba Dendrobii section that step (1) obtains spread out and carry out freezing, cryogenic temperature is-20 DEG C.
3) pulverize at low temperature: the Herba Dendrobii section that step (2) obtains pulverized under the cryogenic conditions of-20 DEG C, sieve, obtains 40 ~ 100 object coarse powder.
4) low-temperature vacuum microwave is dry: the Herba Dendrobii coarse powder that step (3) obtains is carried out low-temperature vacuum microwave drying, power-on, adjustment microwave power: 6kw, microwave drying total time: 1h, baking temperature :-20 DEG C; Vacuum: 0.06Pa.Interval 30s can be taked, the microwave treatment mode (namely often heat 30s just to stop heating 30s and then continue heating 30s stopping again heating 30s, circulate successively) of heating 30s in microwave drying process.
5) low temperature supersonic jet mill: the Herba Dendrobii xeraphium that step (4) obtains is carried out superfine grinding, to impalpable powder under the cryogenic conditions of-20 DEG C.
6) subpackage and packaging: get the superfine powder that step (5) is obtained, through power 1kw, under the condition of frequency 2450MHZ after microwave sterilizating sterilizing 2min temperature 18 ~ 26 DEG C, subpackage is carried out in the aseptic subpackaged room of humidity less than 65%, subpackage and outer package is carried out, obtained finished product according to the specification of often wrapping 1 ~ 5 gram.
Comparative example 2:
1) pretreatment: get fresh Herba Dendrobii medical material, removing impurity, washes, is cut into 2 ~ 4cm section;
2) freezing: the Herba Dendrobii section that step (1) obtains spread out and carry out freezing, cryogenic temperature is-20 DEG C.
3) pulverize at low temperature: the Herba Dendrobii section that step (2) obtains pulverized under the cryogenic conditions of-20 DEG C, sieve, obtains 40 ~ 100 object coarse powder.
4) low-temperature vacuum microwave is dry: the Herba Dendrobii coarse powder that step (3) obtains is carried out low-temperature vacuum microwave drying, power-on, adjustment microwave power: 6kw, microwave drying total time: 1h, baking temperature :-20 DEG C; Vacuum: 0.06Pa.Interval 30s can be taked, the microwave treatment mode (namely often heat 30s just to stop heating 30s and then continue heating 30s stopping again heating 30s, circulate successively) of heating 30s in microwave drying process.
5) co-vibration mill is pulverized: the dendrobium candidum ultrafine powder that step (4) obtains is carried out micronizing in co-vibration mill, temperature controls below 20 DEG C, is crushed to impalpable powder (detection of its particle diameter can be detected by the method such as scanning electron microscope, laser particle analyzer).
6) subpackage and packaging: get the superfine powder that step (5) is obtained, through power 1kw, under the condition of frequency 2450MHZ after microwave sterilizating sterilizing 2min temperature 18 ~ 26 DEG C, subpackage is carried out in the aseptic subpackaged room of humidity less than 65%, subpackage and outer package is carried out, obtained finished product according to the specification of often wrapping 1 ~ 5 gram.
Table 1 is that alone a kind of micronizing machinery and two kinds of micronizing machineries combine the fineness ratio of products obtained therefroms comparatively
Table 1
|
Comparative example 2 |
Comparative example 1 |
Embodiment 3 |
Breaking method |
Co-vibration mill is pulverized |
Supersonic jet mill |
Two kinds of size reduction machineries share |
Product fineness |
200 ~ 500 nanometers |
200 ~ 500 nanometers |
10 ~ 300 nanometers |
The dendrobium candidum ultrafine powder that the present invention obtains and decocting liquid polyoses content contrast as shown in table 2:
Table 2
As shown in Table 2, after Herba Dendrobii carries out micronizing, the stripping of effective ingredient significantly improves, and is conducive to promoting its body absorption, improves bioavailability.