CN108143762A - The production technology of Cortex Eucommiae fine powder - Google Patents
The production technology of Cortex Eucommiae fine powder Download PDFInfo
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- CN108143762A CN108143762A CN201810074956.4A CN201810074956A CN108143762A CN 108143762 A CN108143762 A CN 108143762A CN 201810074956 A CN201810074956 A CN 201810074956A CN 108143762 A CN108143762 A CN 108143762A
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- cortex eucommiae
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/46—Eucommiaceae (Eucommia family), e.g. hardy rubber tree
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/19—Preparation or pretreatment of starting material involving fermentation using yeast, bacteria or both; enzymatic treatment
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
Abstract
The invention belongs to the processing technique fields of Cortex Eucommiae, and in particular to a kind of production technology of Cortex Eucommiae fine powder.The production technology of Cortex Eucommiae fine powder, which is characterized in that as raw material, centrifugation precipitation, concentration, alcohol precipitation isolate and purify, connect and dry through cyclodextrin packet the enzymolysis liquid filtrate obtained using biological enzyme degradation folium cortex eucommiae or eucommia bark, and must shut out kind of a fine powder.Maximum improvement of the invention is to have passed through centrifugal treating twice before alcohol precipitation; filtering; concentration; be conducive to put forward highly enriched efficiency; production cost is reduced, and is effectively protected the quality of product, while heat exchange efficiency is held essentially constant; the efficiency of evaporation and concentration is improved, has effectively saved energy consumption.
Description
Technical field
The invention belongs to the processing technique fields of Cortex Eucommiae, and in particular to a kind of production technology of Cortex Eucommiae fine powder.
Background technology
The production technology for the health care Cortex Eucommiae fine powder that CN106954852A is disclosed, it is characterised in that include the following steps：
(1) raw material is chosen, and chooses the raw materials for production of folium cortex eucommiae and eucommia bark as health care Cortex Eucommiae fine powder, wherein folium cortex eucommiae
Mass ratio with eucommia bark is 2:1, folium cortex eucommiae acquires in September~November, and the folium cortex eucommiae of selection and eucommia bark selection by winnowing are removed
It is spare after dirt；
(2) raw materials for production of selection are placed in enzymolysis device, then choose raw materials for production weight 3% by protease hydrolyzed
Protease be dissolved into protein enzyme solution, then protein enzyme solution is added in enzymolysis device and be digested, wherein protein enzyme solution with
The mass ratio of raw materials for production is 4:1, enzymolysis time is 6 hours~8 hours, and solution is collected after enzymolysis and filtering and removing slag obtain egg
White enzyme enzymolysis liquid；
(3) pectinase enzymatic hydrolysis, the pectase for choosing raw materials for production weight 2% are dissolved into pectinase solution, are then digesting
It continuously adds pectinase solution in device to be digested, wherein the mass ratio of pectinase solution and folium cortex eucommiae is 3:1, enzymolysis time
It is 4 hours~6 hours, solution is collected after enzymolysis and filtering and removing slag obtain pectinase enzymatic hydrolysis liquid；
(4) cellulase degradation, the cellulase for choosing raw materials for production weight 2% are dissolved into cellulase solution, then
Cellulase solution is continuously added in device is digested to be digested, wherein the mass ratio of cellulase solution and folium cortex eucommiae is 3:
1, enzymolysis time is 4 hours~6 hours, and solution is collected after enzymolysis and filtering and removing slag obtain cellulase degradation liquid；
(5) mixing concentration passes through the protease hydrolyzed liquid, pectinase enzymatic hydrolysis liquid, cellulase degradation liquid of acquisition refined
Purifying is mixed, and obtains uniform mixed liquor, then mixed liquor is placed in low-temperature vacuum thickener and is concentrated, is obtained after concentration
Enzymolysis liquid medicinal extract is obtained, then enzymolysis liquid medicinal extract is placed in ethyl alcohol blending tank, it is molten that edible ethanol is then added in blending tank
Liquid carries out low temperature sterilization and the separation without effective component precipitation, and the ultimate density for making alcohol mixeding liquid is 75%~80%, enzymolysis
The mass ratio of liquid medicinal extract and ethanol solution is 1:3, the upper strata ethanol solution clear liquid containing Cortex Eucommiae effective component is obtained after separation；
(6) prepared by health care Cortex Eucommiae fine powder, and it is true that the upper strata ethanol solution clear liquid containing Cortex Eucommiae effective component is placed to rotation
It in empty evaporator, while adds in addition food-grade beta-cyclodextrin and is uniformly mixed, then the evaporation recycling ethyl alcohol in vacuum drying tank
And moisture, drying temperature are 50 DEG C~60 DEG C, obtain health care Cortex Eucommiae fine powder after dry, wherein contain Cortex Eucommiae in health care Cortex Eucommiae fine powder
Extract and food-grade beta-cyclodextrin；
(7) packed products, by the health care Cortex Eucommiae fine powder of acquisition be placed to sealing Multidimensionblender in it is sterile be uniformly mixed, then
It is encased in vinyl bag, is packaged as finished product health care Cortex Eucommiae fine powder.
It during the Cortex Eucommiae fine powder that above-mentioned method obtains, connects, does by the direct alcohol precipitation of enzymolysis liquid, then by dextrin packet
It is dry；Lead to the yield relative reduction of product；In addition, alcohol is increased since the concentration of active ingredient in enzymolysis liquid is relatively low during alcohol precipitation
Dosage, while also increase subsequent wastewater treatment capacity, production cost is relatively high, this technical problem is equally also
It is solved to effective.
Technique therefore, it is necessary to be directed to above-mentioned is improved, and is invented a kind of method that can overcome above-mentioned technological deficiency, is made institute
Its recovery rate of the Cortex Eucommiae fine powder of acquisition is high and content is also relatively high, while can reduce production cost.
Invention content
In order to solve the technical issues of above-mentioned, obtained the present invention provides one kind with enzymic degradation folium cortex eucommiae or eucommia bark
Enzymolysis liquid filtrate for Cortex Eucommiae fine powder made from raw material, Cortex Eucommiae medicament contg is 22%~28% in the Cortex Eucommiae fine powder.
The present invention is realized by following technical solutions：
The production technology of Cortex Eucommiae fine powder, the enzymolysis liquid obtained using the biological enzyme preparation thick glue of Cortex Eucommiae is raw material, centrifugation point
It isolates and purifies from precipitation, filtering, concentration, alcohol precipitation, connect and dry through cyclodextrin packet, must shut out and plant a fine powder.
Step with centrifugal separation includes primary centrifugation and is detached with secondary centrifuging；
The condition once centrifuged is：Rotary drum rotating speed 1000r/h, spiral differential speed：10-25r/h, separation factor：
3000；
Secondary centrifuging separation condition be：Rotating speed 16300r/min, separation factor：15620；
During filtering, the condition of PP membrane filtrations is：Temperature≤35 DEG C, pH value：3-11, pressure after film：P<0.2MPa, retention point
Son amount：250000 dalton.
The temperature of concentration is less than or equal to 60 DEG C, and vacuum degree during concentration is -0.08MPa~0.09MPa, is concentrated into protoenzyme
Solve the 10% of liquid product.
Ethyl alcohol or absolute ethyl alcohol of the volumetric concentration for 80%-95% are used in alcohol precipitation separation；The alcohol precipitation time is small for 10-20
When；
The medicinal extract of gained carries out wrapping in the liquid phase connecing with inclusion agents cyclodextrin after alcohol precipitation separation, and wrapping the condition connect is：Packet connects
40-60 DEG C of temperature, packet meet time 1-2h, and packet connects ratio and is：Medicinal extract:Cyclodextrin weight ratio is 1-3:6-10.
Packet connects completion and is dried in vacuo under the conditions of 50 DEG C~90 DEG C, and vacuum degree is -0.08MPa~0.09MPa, is done
Cortex Eucommiae powder is obtained after dry.
Preferably, the production technology of Cortex Eucommiae fine powder, including following steps：
(1) it using the enzymolysis liquid that enzymic degradation folium cortex eucommiae or eucommia bark are obtained as raw material, centrifuges, which includes
Primary centrifuge detaches with secondary centrifuging；
The condition once centrifuged is：Rotary drum rotating speed 1000r/h, spiral differential speed：10-25r/h, separation factor：
3000；
Secondary centrifuging separation condition be：Rotating speed 16300r/min, separation factor：15620；
During filtering, the condition of PP membrane filtrations is：Temperature≤35 DEG C, pH value：3-11, pressure after film：P<0.2MPa, retention point
Son amount：250000 dalton.
(2) by the supernatant concentration of gained, the 10% of protoenzyme solution liquid product is concentrated into, the temperature of concentration is less than or equal to 60
DEG C, vacuum degree during concentration is -0.08MPa~0.09MPa；
(3) ethyl alcohol or absolute ethyl alcohol that volumetric concentration is 80-95%, alcohol precipitation separation 10- are added in medicinal extract after concentration
20 hours；
(4) it wraps and connects in the liquid phase with cyclodextrin in the ethanol solution medicinal extract of the drug containing Cortex Eucommiae of the middle gained of step (3)；Packet connects
40-60 DEG C of temperature, packet meet time 1-2h, and packet connects ratio and is：Medicinal extract:Cyclodextrin weight ratio is 1-3:6-10；
(5) raw material after packet connects in step (4) is taken to be placed at 50 DEG C~80 DEG C to be dried in vacuo, must shut out kind of a fine powder.
More specifically, the production technology of Cortex Eucommiae fine powder, including following steps：
(1) the enzymolysis liquid filtrate obtained using enzymic degradation folium cortex eucommiae or eucommia bark centrifuges precipitation as raw material；From
Heart separating step includes primary centrifugation and is detached with secondary centrifuging；
The condition once centrifuged is：Rotary drum rotating speed 1000r/h, spiral differential speed：10-25r/h, maximum separation because
Number：3000；
Secondary centrifuging separation condition be：Rotating speed 16300r/min, separation factor：15620；
During filtering, the condition of PP membrane filtrations is：Temperature≤35 DEG C, pH value：3-11, pressure after film：P<0.2MPa, retention point
Son amount：250000 dalton.
(2) by the supernatant concentration of gained, the 10% of protoenzyme solution liquid product is concentrated into, the temperature of concentration is less than or equal to 60
DEG C, vacuum degree during concentration is -0.08MPa~0.09MPa；
(3) ethyl alcohol that volumetric concentration is 95% is added in medicinal extract after concentration, alcohol precipitation detaches 15 hours；
(4) it wraps and connects in the liquid phase with cyclodextrin in the ethanol solution medicinal extract of the drug containing Cortex Eucommiae of the middle gained of step (3)；Packet connects
Temperature 50 C, packet meet time 1h, and packet connects ratio and is：Medicinal extract:Cyclodextrin weight ratio is 3:8.
(5) raw material after packet connects in step (4) is taken to be placed at 50 DEG C~80 DEG C to be dried in vacuo, must shut out kind of a fine powder.
Cortex Eucommiae medicament contg is 22%~28% in the Cortex Eucommiae powder obtained by above-mentioned method.
The preparation method of raw material enzymolysis liquid is as follows：To use SUKAPro AC enzymes, pectase and cellulase substep successively
The obtained enzymolysis liquid of enzymolysis is raw material.
The present invention with respect to the background art in technique, difference it is as follows：
Technique in background technology is that enzymolysis liquid medicinal extract and ethanol solution are carried out low temperature sterilization and precipitated without effective component
Separation, obtain upper strata ethanol solution clear liquid；Rotatory vacuum evaporates, and adds in food-grade beta-cyclodextrin and is uniformly mixed, then true
Evaporation recycling ethyl alcohol and moisture in empty drying chamber, Cortex Eucommiae fine powder is obtained after dry.
Simplicity is expressed as follows：
Technique i.e. in background technology is：
Enzymolysis liquid+ethanol solution → supernatant liquor → vacuum evaporation → cyclodextrin packet connects → is dried in vacuo → Cortex Eucommiae fine powder；
The present invention technique be：
Enzymolysis liquid → primary centrifugation → secondary centrifuging separation → filtering → concentration → alcohol precipitation → dextrin packet connects → is dried；
The technique of the present invention with respect to the background art in technique, maximum improvement is to have passed through twice before alcohol precipitation
Centrifugal treating, filtering, the technique of concentration.The advantages of so improving is that material is centrifuged before it is concentrated using sleeping spiral shell successively
Machine, tube centrifuge, PP membrane filtrations into being transparent liquid when being concentrated in vacuo, are conducive to carry out subsequent alcohol precipitation, drying etc.
Working process.
Before alcohol precipitation, also to material concentration, the concentration of active ingredient in feed liquid is improved, reduces the material of alcohol precipitation
Liquid measure, so as to reduce the dosage of alcohol；The water obtained after concentrating simultaneously can be reused, and reduce the dosage of water.Dense
In compression process, the quality of product is effectively protected, while heat exchange efficiency is held essentially constant, improves the effect of evaporation and concentration
Rate has effectively saved energy consumption.
Specific embodiment
The present invention is further described with reference to specific embodiment, so that those skilled in the art knows more about
The present invention, but be not intended to limit the present invention.
Enzymolysis liquid used in the present invention is the enzymolysis liquid and the applicant obtained with reference to the mode of action of the prior art
Homemade enzymolysis liquid has versatility in the method for the verification present invention.The method of the present invention is suitable for all and uses biological enzyme pair
Folium cortex eucommiae or eucommia bark are digested obtained enzymolysis liquid；It is not limited to certain specific biological enzyme or certain several biology
The enzymolysis liquid that enzyme is obtained, but the enzymolysis liquid must be have an effect to folium cortex eucommiae or eucommia bark by its argillization, disintegrate into
And obtained enzymolysis liquid is smoothly digested, and the enzyme solution not acted to folium cortex eucommiae or eucommia bark not.
SUKAPro AC enzymes：Xia Sheng bio tech ltd provides.
Pectase：Summer contains biotechnology.
Neutral cellulase：Golden source biochemical industry.
Embodiment 1
The production technology of Cortex Eucommiae fine powder, including following steps：
(1) using the enzymolysis liquid that enzymic degradation folium cortex eucommiae is obtained as raw material,
Centrifuge precipitation；Step with centrifugal separation includes primary centrifugation and is detached with secondary centrifuging；
The condition once centrifuged is：It is centrifuged using decanter centrifuge, rotary drum rotating speed 1000r/h, spiral differential speed：
10-25r/h, maximum separation factor：3000；
Secondary centrifuging separation condition be：It is centrifuged using tube centrifuge, rotating speed 16300r/min, separation factor：
15620；
During filtering, the condition of PP membrane filtrations is：Temperature≤35 DEG C, pH value：3-11, pressure after film：P<0.2MPa, retention point
Son amount：250000 dalton.
(2) by the supernatant concentration of gained, the 10% of protoenzyme solution liquid product is concentrated into, the temperature of concentration is less than or equal to 60
DEG C, vacuum degree during concentration is -0.08MPa~0.09MPa；
(3) ethyl alcohol that volumetric concentration is 95% is added in medicinal extract after concentration, alcohol precipitation detaches 15 hours；
(4) it wraps and connects in the liquid phase with cyclodextrin in the ethanol solution medicinal extract of the drug containing Cortex Eucommiae of the middle gained of step (3)；Packet connects
Temperature 50 C, packet meet time 1h, and packet connects ratio and is：Medicinal extract:Cyclodextrin weight ratio is 3:8；
(5) raw material after packet connects in step (4) is taken to be placed at 65 DEG C to be dried in vacuo 10 hours or so, makes the moisture content of material
Less than 10%, must shut out kind of a fine powder.
Comparative example 1
Comparative example 1 has lacked second of process centrifuged relative to embodiment 1；
The production technology of Cortex Eucommiae fine powder, including following steps：
(1) it using the enzymolysis liquid that enzymic degradation folium cortex eucommiae is obtained as raw material, centrifuges and filters,
The condition of centrifugation is：It is centrifuged using decanter centrifuge, rotary drum rotating speed 1000r/h, spiral differential speed：10-
25r/h, maximum separation factor：3000；
During filtering, the condition of PP membrane filtrations is：Temperature≤35 DEG C, pH value：3-11, pressure after film：P<0.2MPa, retention point
Son amount：250000 dalton；
(2) by the supernatant concentration of gained, the 10% of protoenzyme solution liquid product is concentrated into, the temperature of concentration is less than or equal to 60
DEG C, vacuum degree during concentration is -0.08MPa~0.09MPa；
(3) ethyl alcohol that volumetric concentration is 95% is added in medicinal extract after concentration, alcohol precipitation detaches 10-20 hours；
(4), (5) must shut out with embodiment 1 and plant a fine powder.
Comparative example 2
Comparative example 2 has lacked the process centrifuged for the first time relative to embodiment 1；
The production technology of Cortex Eucommiae fine powder, including following steps：
(1) it using the enzymolysis liquid that enzymic degradation folium cortex eucommiae is obtained as raw material, centrifuges and filters,
The condition of centrifugation is：It is centrifuged using tube centrifuge, condition is：Rotating speed 16300r/min, separation factor：
15620；
During filtering, the condition of PP membrane filtrations is：Temperature≤35 DEG C, pH value：3-11, pressure after film：P<0.2MPa, retention point
Son amount：250000 dalton；
(2) by the supernatant concentration of gained, the 10% of protoenzyme solution liquid product is concentrated into, the temperature of concentration is less than or equal to 60
DEG C, vacuum degree during concentration is -0.08MPa~0.09MPa；
(3) ethyl alcohol that volumetric concentration is 95% is added in medicinal extract after concentration, alcohol precipitation detaches 10-20 hours；
(4), (5) must shut out with embodiment 1 and plant a fine powder.
Comparative example 3
Comparative example 3, without centrifugal treating, is directly filtered relative to embodiment 1；
The production technology of Cortex Eucommiae fine powder, including following steps：
(1) it using the enzymolysis liquid that enzymic degradation folium cortex eucommiae is obtained as raw material, filters, the condition of PP membrane filtrations is：Temperature≤
35 DEG C, pH value：3-11, pressure after film：P<0.2MPa, molecular cut off：250000 dalton；
(2) by the supernatant concentration of gained, the 10% of protoenzyme solution liquid product is concentrated into, the temperature of concentration is less than or equal to 60
DEG C, vacuum degree during concentration is -0.08MPa~0.09MPa；
(3) ethyl alcohol that volumetric concentration is 95% is added in medicinal extract after concentration, alcohol precipitation detaches 10-20 hours；
(4), (5) must shut out with embodiment 1 and plant a fine powder.
Comparative example 4
Compared with Example 1, in comparative example 4 without concentration, remaining condition is identical with embodiment 1；
The production technology of Cortex Eucommiae fine powder, including following steps：
(1) it using the enzymolysis liquid that enzymic degradation folium cortex eucommiae is obtained as raw material, centrifuges, which includes primary centrifugation point
It is detached from secondary centrifuging；
The condition once centrifuged is：Using decanter centrifuge, rotary drum rotating speed 1000r/h, spiral differential speed：10-
25r/h, maximum separation factor：3000；
Secondary centrifuging separation condition be：Rotating speed 16300r/min, separation factor：15620；
During filtering, the condition of PP membrane filtrations is：Temperature≤35 DEG C, pH value：3-11, pressure after film：P<0.2MPa, retention point
Son amount：250000 dalton.
(2) ethyl alcohol that volumetric concentration is 95% is added in the filtrate obtained by filtering, alcohol precipitation detaches 10-20 hours；
(4), (5) of step (3), (4) with embodiment 1, must shut out kind of a fine powder.
Comparative example 5
Compared with Example 1, the step of in comparative example 5 not using filtering；Remaining step is identical；
The production technology of Cortex Eucommiae fine powder, including following steps：
(1) it using the enzymolysis liquid that enzymic degradation folium cortex eucommiae is obtained as raw material, centrifuges, which includes primary centrifugation point
It is detached from secondary centrifuging；
The condition once centrifuged is：Using decanter centrifuge, rotary drum rotating speed 1000r/h, spiral differential speed：10-
25r/h, separation factor：3000；
Secondary centrifuging separation condition be：Using tube centrifuge, rotating speed 16300r/min, separation factor：15620；
(2) supernatant concentration that will centrifuge gained is concentrated into the 10% of protoenzyme solution liquid product, and the temperature of concentration is less than or waits
Vacuum degree when 60 DEG C, concentration is -0.08MPa~0.09MPa；
(3) ethyl alcohol that volumetric concentration is 95% is added in medicinal extract after concentration, alcohol precipitation detaches 10-20 hours；
(4), (5) must shut out with embodiment 1 and plant a fine powder.
Comparative example 6
Compared with Example 1, the step of centrifugal filtration is not used in comparative example 6, directly handles enzymolysis liquid alcohol precipitation；Remaining
Condition is identical；
The production technology of Cortex Eucommiae fine powder, including following steps：
(1) using the enzymolysis liquid that enzymic degradation folium cortex eucommiae is obtained as raw material；It is 95% that volumetric concentration is added in the raw material
Ethyl alcohol, alcohol precipitation detach 10-20 hours；
(2) it wraps and connects in the liquid phase with cyclodextrin in the ethanol solution medicinal extract of the drug containing Cortex Eucommiae of the middle gained of step (1)；
(3) the material vacuum drying after packet connects in step (2) is taken, must shut out kind of a fine powder.Specific packet connects and drying condition is same
Embodiment 1.
Comparative example 7
The production technology of Cortex Eucommiae fine powder, including following steps：
(1) using the enzymolysis liquid that enzymic degradation folium cortex eucommiae is obtained as raw material, enzymolysis liquid is concentrated, is concentrated into protoenzyme solution liquid
Long-pending 10%, the temperature of concentration are less than or equal to 60 DEG C, and vacuum degree during concentration is -0.08MPa~0.09MPa；
(2) ethyl alcohol that volumetric concentration is 95% is added in medicinal extract after concentration, alcohol precipitation detaches 10-20 hours；
(3) it wraps and connects in the liquid phase with cyclodextrin in the ethanol solution medicinal extract of the drug containing Cortex Eucommiae of the middle gained of step (2)；
(4) the material vacuum drying after packet connects in step (3) is taken, must shut out kind of a fine powder.
The processing step abridged table of embodiment 1, comparative example 1-7
| Embodiment 1 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | Comparative example 6 | Comparative example 7 | |
| Primary centrifugation | √ | √ | √ | √ | ||||
| Secondary centrifuging | √ | √ | √ | √ | ||||
| Filtering | √ | √ | √ | √ | √ | |||
| Concentration | √ | √ | √ | √ | √ | √ | ||
| Alcohol precipitation | √ | √ | √ | √ | √ | √ | √ | √ |
| Packet connects | √ | √ | √ | √ | √ | √ | √ | √ |
| It is dry | √ | √ | √ | √ | √ | √ | √ | √ |
Note：It is to employ this step that " √ " is drawn in table, and unlabelled is not use this step.
In this scheme implementation process, the recovery rate of Cortex Eucommiae fine powder property of traditional Chinese ingredient, content are main parameters, wherein
Recovery rate is according to computational methods once：
The computational methods of content：
Detection method in following embodiment and comparative example herewith, but specified otherwise.
It is calculated according to above formula, the recovery rate of example 1 is 86.5%, and content is 25.4%.
In comparative example 1, the separation of tube centrifuge is not carried out, since residue does not remove fully, is caused in follow-up PP
In membrane separating process, residue is easy to the duct of film, causes the unstable of production；
In comparative example 2, not using decanter centrifuge, only with a kind of centrifugation so that larger, thicker is residual
Slag cannot detach so that subsequent separation process is more difficult to realize.
In comparative example 3, without centrifugation, the rate of filtration is slow, and big residue is easily deposited on the surface of film, easily blocks
Filter membrane reduces filter efficiency.
In comparative example 4, without the technique of concentration, in the alcohol precipitation stage, the consumption of alcohol is increased, causes energy consumption, object
Consumption is higher；Secondly moisture cannot recycle, and the wastewater flow rate of generation is big, and burden is increased for subsequent wastewater treatment.
Without carrying out membrane filtration in comparative example 5, the content of fine powder is reduced, reduces the performance of pharmacological property ingredient.Comparative example 5
In, the recovery rate of Cortex Eucommiae fine powder is 82.2%, content 19.3%.
Secondary centrifuging processing is not carried out to enzymolysis liquid in comparative example 6, also do not filter, concentrate, during actual experiment, by
Effective constituent concentration content is low in enzymolysis liquid, the amount of alcohol used during alcohol precipitation is caused to increase several times, cost is big
It is big to improve, and due to without centrifugation, filtration treatment, the nontransparent liquid of product when entering vacuum concentration, after being unfavorable for
The working processes such as continuous alcohol precipitation and drying；
Likewise, in comparative example 7, the phenomenon that also producing as generated in comparative example 6.
Embodiment 2
The production technology of Cortex Eucommiae fine powder, including following steps：
(1) it using the enzymolysis liquid that enzymic degradation folium cortex eucommiae is obtained as raw material, centrifuges, which includes primary centrifugation point
It is detached from secondary centrifuging；
The condition once centrifuged is：Using decanter centrifuge, rotary drum rotating speed 1000r/h, spiral differential speed：10-
25r/h, maximum separation factor：3000；
Secondary centrifuging separation condition be：Using tube centrifuge, rotating speed 16300r/min, separation factor：15620；
During filtering, the condition of PP membrane filtrations is：Temperature≤35 DEG C, pH value：3-11, pressure after film：P<0.2MPa, retention point
Son amount：250000 dalton.
(2) by the supernatant concentration of gained, the 10% of protoenzyme solution liquid product is concentrated into, the temperature of concentration is less than or equal to 60
DEG C, vacuum degree during concentration is -0.08MPa~0.09MPa；
(3) ethyl alcohol that volumetric concentration is 95% is added in medicinal extract after concentration, alcohol precipitation detaches 10 hours；
(4) it wraps and connects in the liquid phase with cyclodextrin in the ethanol solution medicinal extract of the drug containing Cortex Eucommiae of the middle gained of step (3)；Packet connects
40~60 DEG C of temperature, packet meet 1~2h of time；Packet connects ratio and is：Medicinal extract:Cyclodextrin=2:8；
(5) raw material after packet connects in step (4) is taken to be placed at 60 DEG C to be dried in vacuo 12 hours or so, must shut out kind of a fine powder.
By detection, the recovery rate of Cortex Eucommiae active constituent is 85.6% in Cortex Eucommiae fine powder in embodiment 2, and content is
25.8%.
Embodiment 3
The production technology of Cortex Eucommiae fine powder, including following steps：
(1) it using the enzymolysis liquid that enzymic degradation eucommia bark is obtained as raw material, centrifuges, which includes primary centrifugation
Separation is detached with secondary centrifuging；
The condition once centrifuged is：Using decanter centrifuge, rotary drum rotating speed 1000r/h, spiral differential speed：10-
25r/h, maximum separation factor：3000；
The condition of secondary centrifuging separation is, using tube centrifuge：Rotating speed 16300r/min, separation factor：15620；
During filtering, the condition of PP membrane filtrations is：Temperature≤35 DEG C, pH value：3-11, pressure after film：P<0.2MPa, retention point
Son amount：250000 dalton.
(2) by the supernatant concentration of gained, the 10% of protoenzyme solution liquid product is concentrated into, the temperature of concentration is less than or equal to 60
DEG C, vacuum degree during concentration is -0.08MPa~0.09MPa；
(3) ethyl alcohol that volumetric concentration is 90% is added in medicinal extract after concentration, alcohol precipitation detaches 20 hours；
(4) it wraps and connects in the liquid phase with cyclodextrin in the ethanol solution medicinal extract of the drug containing Cortex Eucommiae of the middle gained of step (3)；
(5) raw material after packet connects in step (4) is taken to be placed at 80 DEG C to be dried in vacuo, must shut out kind of a fine powder.
By detection, the recovery rate of Cortex Eucommiae active constituent is 84.9% in Cortex Eucommiae fine powder in embodiment 3, and content is
24.7%.
Embodiment 4
The present embodiment employs the homemade enzymolysis liquid of applicant, but the method for the present invention is not limited to such enzymolysis liquid, and
It is with universality.
The production technology of Cortex Eucommiae fine powder, including following steps：
(1) using the enzymolysis liquid that enzymic degradation folium cortex eucommiae is obtained as raw material, the specific preparation method of the raw material is as follows：
Using the folium cortex eucommiae of non-landing as raw material, silt and sundries are removed；
By Na2HPO4, sodium citrate the buffer solution I that pH is 2.8-4.0 is made, take and account for the 3~6% of raw material weight
SUKAPro AC enzymes are dissolved in buffer solution I, obtain enzyme solution I；
Raw material and enzyme solution I are added in enzymatic vessel and digest 6~12h in 48 DEG C~55 DEG C, obtains enzymolysis liquid I and solid residue
Ⅰ；
The weight ratio of raw material and enzyme solution I is：1: 2~1: 6；
Enzymolysis liquid I is discharged, it is spare in enzymatic vessel to retain solid residue I；
By Na2HPO4The buffer solution II for the pH3.4-4.4 being configured to sodium citrate；
4~6% pectase for accounting for raw material weight is taken to be dissolved in buffer solution II, obtains enzyme solution II；Raw material and enzyme solution II
Weight ratio is 1: 2~1: 3；
Enzyme solution II is added in enzyme digestion reaction rotary tank and is mixed with solid residue I, 8- is digested at 44 DEG C~48 DEG C
10h obtains enzymolysis liquid II and solid residue II；
The enzymolysis liquid II of gained is given off, it is spare in enzymatic vessel to retain solid residue II；
By Na2HPO4The buffer solution III of pH=3.5~5.4 is configured to sodium citrate；Take the 2-4% for accounting for raw material weight
Neutral cellulase be dissolved in buffer solution III, obtain enzyme solution III；The weight ratio of raw material and enzyme solution III is 1: 2~1: 5；
Enzyme solution III is added in enzyme digestion reaction tank and is mixed with solid residue II, it is small in 45 DEG C~60 DEG C enzymolysis 10~14
When, enzymolysis liquid III and solid residue III are obtained,
The enzymolysis liquid III of gained is given off, it is spare in enzymatic vessel to retain solid residue III；
Centrifuging treatment after above enzymolysis liquid I, enzymolysis liquid II and enzymolysis liquid III are merged, including once centrifuging
It is detached with secondary centrifuging；
The condition once centrifuged is：Using decanter centrifuge, rotary drum rotating speed 1000r/h, spiral differential speed：10-
25r/h, maximum separation factor：3000；
The condition of secondary centrifuging separation is, using tube centrifuge：Rotating speed 16300r/min, separation factor：15620；
During filtering, the condition of PP membrane filtrations is：Temperature≤35 DEG C, pH value：3-11, pressure after film：P<0.2MPa, retention point
Son amount：250000 dalton.
(2) by the supernatant concentration of gained, the 10% of protoenzyme solution liquid product is concentrated into, the temperature of concentration is less than or equal to 60
DEG C, vacuum degree during concentration is -0.08MPa~0.09MPa；
(3) ethyl alcohol that volumetric concentration is 90% is added in medicinal extract after concentration, alcohol precipitation detaches 20 hours；
(4) it wraps and connects in the liquid phase with cyclodextrin in the ethanol solution medicinal extract of the drug containing Cortex Eucommiae of the middle gained of step (3)；Packet connects
40~60 DEG C of temperature, packet meet 1~2h of time；Packet connects ratio and is：Medicinal extract:Cyclodextrin=2:8；
(5) raw material after packet connects in step (4) is taken to be placed at 80 DEG C to be dried in vacuo, must shut out kind of a fine powder.
By detection, the recovery rate of Cortex Eucommiae active constituent is 86.2% in Cortex Eucommiae fine powder in embodiment 3, and content is
25.5%.
Embodiment 5
The production technology of Cortex Eucommiae fine powder, including following steps：
(1) using the enzymolysis liquid that enzymic degradation eucommia bark is obtained as raw material, the specific preparation method of the raw material is as follows：
It using eucommia bark as raw material, polishes through coarse plain emery wheel and removes the tertia of bark surface, retain internal layer bast containing glue；
Remaining the step of, is the same as embodiment 4.
By detection, the recovery rate of Cortex Eucommiae active constituent is 86.4% in Cortex Eucommiae fine powder in embodiment 5, and content is
24.9%.
Claims (9)
1. the production technology of Cortex Eucommiae fine powder, which is characterized in that the enzymolysis liquid obtained using the biological enzyme preparation thick glue of Cortex Eucommiae is original
Material, centrifugation precipitation, filtering, concentration, alcohol precipitation isolate and purify, connect and dry through cyclodextrin packet, and must shut out kind of a fine powder.
2. the production technology of Cortex Eucommiae fine powder as described in claim 1, which is characterized in that step with centrifugal separation includes primary centrifugation
Separation is detached with secondary centrifuging；
The condition once centrifuged is：Rotary drum rotating speed 1000r/h, spiral differential speed：10-25r/h, separation factor：3000；
Secondary centrifuging separation condition be：Rotating speed 16300r/min, separation factor：15620；
During filtering, the condition of PP membrane filtrations is：Temperature≤35 DEG C, pH value：3-11, pressure after film：P<0.2MPa retains molecule
Amount：250000 dalton.
3. the production technology of Cortex Eucommiae fine powder as described in claim 1, which is characterized in that the temperature of concentration is less than or equal to 60
DEG C, vacuum degree during concentration is -0.08MPa~0.09MPa, is concentrated into the 10% of protoenzyme solution liquid product.
4. the production technology of Cortex Eucommiae fine powder as described in claim 1, which is characterized in that alcohol precipitation separation in use volumetric concentration for
The ethyl alcohol or absolute ethyl alcohol of 80%-95%；The alcohol precipitation time is 10-20 hours.
5. the production technology of Cortex Eucommiae fine powder as described in claim 1, which is characterized in that the medicinal extract and packet of gained after alcohol precipitation separation
Mixture cyclodextrin carries out packet and connects in the liquid phase, and wrapping the condition connect is：40-60 DEG C of packet jointing temp, packet meet time 1-2h, and packet connects ratio
For：Medicinal extract:Cyclodextrin weight ratio is 1-3:6-10.
6. the production technology of Cortex Eucommiae fine powder as described in claim 1, which is characterized in that packet connects completion after 50 DEG C~80 DEG C items
It is dried in vacuo under part, vacuum degree is -0.08MPa~0.09MPa, and Cortex Eucommiae powder is obtained after dry.
7. the production technology of Cortex Eucommiae fine powder as described in claim 1, including following steps：
(1) it using the enzymolysis liquid that enzymic degradation folium cortex eucommiae or eucommia bark are obtained as raw material, centrifuges, which includes primary
Centrifugation is detached with secondary centrifuging；
The condition once centrifuged is：Rotary drum rotating speed 1000r/h, spiral differential speed：10-25r/h, separation factor：3000；
Secondary centrifuging separation condition be：Rotating speed 16300r/min, separation factor：15620；
During filtering, the condition of PP membrane filtrations is：Temperature≤35 DEG C, pH value：3-11, pressure after film：P<0.2MPa retains molecule
Amount：250000 dalton.
(2) by the supernatant concentration of gained, the 10% of protoenzyme solution liquid product is concentrated into, the temperature of concentration is less than or equal to 60 DEG C,
Vacuum degree during concentration is -0.08MPa~0.09MPa；
(3) ethyl alcohol or absolute ethyl alcohol that volumetric concentration is 80-95% are added in medicinal extract after concentration, alcohol precipitation separation 10-20 is small
When；
(4) it wraps and connects in the liquid phase with cyclodextrin in the ethanol solution medicinal extract of the drug containing Cortex Eucommiae of the middle gained of step (3)；Packet jointing temp
40-60 DEG C, packet meets time 1-2h, and packet connects ratio and is：Medicinal extract:Cyclodextrin weight ratio is 1-3:6-10；
(5) raw material after packet connects in step (4) is taken to be placed at 50 DEG C~80 DEG C to be dried in vacuo, must shut out kind of a fine powder.
8. the production technology of Cortex Eucommiae fine powder as described in claim 1, including following steps：
(1) the enzymolysis liquid filtrate obtained using enzymic degradation folium cortex eucommiae or eucommia bark centrifuges precipitation as raw material；Centrifugation point
Include primary centrifuge from step to detach with secondary centrifuging；
The condition once centrifuged is：Rotary drum rotating speed 1000r/h, spiral differential speed：10-25r/h, maximum separation factor：
3000；
Secondary centrifuging separation condition be：Rotating speed 16300r/min, separation factor：15620；
During filtering, the condition of PP membrane filtrations is：Temperature≤35 DEG C, pH value：3-11, pressure after film：P<0.2MPa retains molecule
Amount：250000 dalton.
(2) by the supernatant concentration of gained, the 10% of protoenzyme solution liquid product is concentrated into, the temperature of concentration is less than or equal to 60 DEG C,
Vacuum degree during concentration is -0.08MPa~0.09MPa；
(3) ethyl alcohol that volumetric concentration is 95% is added in medicinal extract after concentration, alcohol precipitation detaches 15 hours；
(4) it wraps and connects in the liquid phase with cyclodextrin in the ethanol solution medicinal extract of the drug containing Cortex Eucommiae of the middle gained of step (3)；Packet jointing temp
50 DEG C, packet meets time 1h, and packet connects ratio and is：Medicinal extract:Cyclodextrin weight ratio is 3:8.
(5) raw material after packet connects in step (4) is taken to be placed at 50 DEG C~80 DEG C to be dried in vacuo, must shut out kind of a fine powder.
9. the production technology of Cortex Eucommiae fine powder as described in claim 1, which is characterized in that Cortex Eucommiae drug contains in the Cortex Eucommiae powder of gained
Measure is 22%~28%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111973649A (en) * | 2020-09-04 | 2020-11-24 | 山东贝隆杜仲生物工程有限公司 | Production process and system of eucommia ulmoides fine powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1757324A2 (en) * | 2000-09-05 | 2007-02-28 | Kao Corporation | Agent for preventing, improving or treating hypertension |
| CN106954852A (en) * | 2017-01-19 | 2017-07-18 | 浙江旭源杜仲生物科技有限公司 | Health care bark of eucommia fine powder |
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2018
- 2018-01-25 CN CN201810074956.4A patent/CN108143762A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1757324A2 (en) * | 2000-09-05 | 2007-02-28 | Kao Corporation | Agent for preventing, improving or treating hypertension |
| CN106954852A (en) * | 2017-01-19 | 2017-07-18 | 浙江旭源杜仲生物科技有限公司 | Health care bark of eucommia fine powder |
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| 叶勇: "《制药工艺学》", 28 February 2014, 华南理工大学 * |
Cited By (1)
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| CN111973649A (en) * | 2020-09-04 | 2020-11-24 | 山东贝隆杜仲生物工程有限公司 | Production process and system of eucommia ulmoides fine powder |
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