CN111449957A - Preparation method of traditional Chinese medicine decoction pieces - Google Patents
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Abstract
The invention discloses a preparation method of traditional Chinese medicine decoction pieces, and relates to the technical field of traditional Chinese medicine processing. The preparation method of the traditional Chinese medicine decoction pieces comprises the following steps of: freezing the selected traditional Chinese medicinal materials at low temperature, then putting the traditional Chinese medicinal materials into a bulking machine, bulking at low temperature and high pressure, and cooling to room temperature after the bulking is completed to obtain bulked traditional Chinese medicinal materials; and (3) pulse discharge plasma treatment: mixing the puffed traditional Chinese medicinal materials and the composite particles, performing pulse discharge plasma treatment, and separating the composite particles by magnetic separation after the treatment is finished to obtain the traditional Chinese medicinal materials with the wall broken in advance; mechanical wall breaking: mechanically breaking the wall of the Chinese medicinal materials to obtain Chinese medicinal decoction pieces. The invention discloses a preparation method of traditional Chinese medicine decoction pieces, which combines high-pressure puffing, pulse discharge plasma treatment and mechanical wall breaking, wherein the one-time wall breaking rate can reach more than 99 percent, and the one-time wall breaking rate is high, so that the preparation method is suitable for popularization and application.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicine processing, in particular to a preparation method of traditional Chinese medicine decoction pieces.
Background
The beneficial active ingredients of many traditional Chinese medicinal materials are usually stored in cells, and if the traditional Chinese medicinal materials are directly used, the effective ingredients of protoplasm of the traditional Chinese medicinal materials are slowly absorbed by a human body and are usually discharged from the body without being subjected to enzymolysis in the digestive tract, so that the traditional Chinese medicinal materials need to be subjected to wall breaking treatment.
At present, wall breaking technologies at home and abroad are researched more, and mainly comprise a biological enzymolysis method, a physical method and a chemical method. Wherein, the biological enzyme method process is complex and other impurities are easy to be introduced; the physical method has complex processing procedures and large equipment investment; the chemical method broken wall effect is unsatisfactory, and harmful residue is high in the product, and the physical method commonly used is when carrying out the broken wall, in order to reach higher broken wall rate, often need carry out broken wall processing many times repeatedly, and because current broken wall machine mostly can not reach and seal the inner loop, adopts the mode of artifical material loading usually, extravagant manpower, consequently, it is necessary to develop a preparation method that has the herbal pieces-for-chinese-medicine that once broken wall rate is high.
Disclosure of Invention
Aiming at the problems, the invention aims to disclose a preparation method of traditional Chinese medicine decoction pieces, which combines high-pressure puffing, pulse discharge plasma treatment and mechanical wall breaking, has the one-time wall breaking rate of more than 99 percent and high one-time wall breaking rate, and is suitable for popularization and use.
Specifically, the preparation method of the traditional Chinese medicine decoction pieces comprises the following steps:
high-pressure puffing: freezing the selected traditional Chinese medicinal materials at low temperature, then putting the traditional Chinese medicinal materials into a bulking machine, bulking at low temperature and high pressure, and cooling to room temperature after the bulking is completed to obtain bulked traditional Chinese medicinal materials;
and (3) pulse discharge plasma treatment: mixing the puffed traditional Chinese medicinal materials and the composite particles, performing pulse discharge plasma treatment, and separating the composite particles by magnetic separation after the treatment is finished to obtain the traditional Chinese medicinal materials with the wall broken in advance;
mechanical wall breaking: mechanically breaking the wall of the Chinese medicinal materials to obtain Chinese medicinal decoction pieces.
The preparation method of the traditional Chinese medicine decoction pieces comprises the steps of firstly carrying out primary destruction on cellulose, lignin and the like in the wall shells of the traditional Chinese medicine materials through high-pressure puffing to enable the cellulose, the lignin and the like to become loose, then carrying out pulse discharge plasma treatment, instantly releasing a large amount of energy during pulse discharge to form large pulse impact to enable the wall shells to break, and then carrying out subsequent mechanical wall breaking to enable the wall shells to be more easily broken, so that the primary wall breaking rate is effectively improved, the wall breaking time is relatively short, simultaneously the generated plasma also has a certain sterilization effect, in addition, by adding composite particles in powder, the traditional Chinese medicine materials can be prevented from generating static electricity to agglomerate and agglomerate through the composite particles, the flowability of the traditional Chinese medicine materials is ensured, meanwhile, the composite particles also have good heat conductivity, the heat can be timely led out, and the local heating of the traditional Chinese medicine materials is avoided, the probability of losing activity of the effective substances of the traditional Chinese medicinal materials due to heating is reduced.
Further, the temperature of the low-temperature freezing treatment is-20 to-5 ℃, and the treatment time is 10 to 12 hours.
Further, nitrogen is used as pressurizing gas during the low-temperature high-pressure puffing treatment, the temperature is 85-90 ℃, the pressure is 10-12MPa, and the treatment time is 1-2 min.
Further, the pulse discharge plasma treatment takes argon as working gas, the pulse discharge voltage is 25-35kV, the pulse frequency is 500-550Hz, and the treatment time is 5-8 min.
Argon belongs to inert gas, and the argon is used as a pulse discharge plasma processing working gas, so that the probability that the activity of the traditional Chinese medicinal materials is reduced by oxidation can be reduced to a certain extent.
Further, the method also comprises a germination culture step before the high-pressure puffing step, wherein the germination culture step specifically comprises the following steps: adjusting water content of the Chinese medicinal materials to 75-85% with deionized water, and culturing at 25-30 deg.C under shading and heat preservation for 30-48 h.
Traditional Chinese medicinal materials capable of being subjected to germination culture, such as ganoderma spore powder, pollen and the like, enter a germination phase after the germination culture, the toughness of the shell wall of the traditional Chinese medicinal materials in the germination phase can be obviously reduced, the improvement of the wall breaking rate is facilitated, and stronger active substances are arranged inside the traditional Chinese medicinal materials in the germination phase.
Further, the traditional Chinese medicinal materials are ganoderma lucidum spore powder or pollen.
Further, the composite particles are prepared by wrapping nano ferroferric oxide with titanium nitride, and then mixing and firing the wrapped nano ferroferric oxide with porous zirconia and rodlike nano alumina.
The nano ferroferric oxide is added into the composite particles, the magnetic property of the nano ferroferric oxide is utilized to conveniently and quickly separate the composite particles from the traditional Chinese medicine materials, titanium nitride is utilized to wrap the ferroferric oxide, on one hand, the ferroferric oxide can be protected, because the ferroferric oxide can react with oxygen at low temperature to generate the ferric oxide, the ferric oxide can be heated and decomposed at high temperature to generate the ferroferric oxide and the oxygen, therefore, the titanium nitride is utilized to wrap the ferroferric oxide, the ferroferric oxide can be prevented from being oxidized into the ferric oxide firstly in the production process, the ferroferric oxide is prevented from being decomposed to generate gas in the calcining process, the strength of the composite particles is influenced, the composite particles are prevented from being cracked in the using process, on the other hand, the ferroferric oxide and the traditional Chinese medicine materials can be prevented from contacting in the using process to a certain, the traditional Chinese medicine is affected on the property or safety of the traditional Chinese medicine, and the titanium nitride and the ferroferric oxide have good heat conducting property and electric conducting property, so that the composite particles can conduct away heat and static electricity accumulated on the surface of the traditional Chinese medicine in time, and the traditional Chinese medicine can be effectively prevented from agglomerating or locally heating due to the electrostatic action during the pulse discharge plasma treatment to a certain extent.
In addition, the composite particles of the invention take zirconia as a main material, the zirconia has stable property and high hardness, a ceramic material is formed after sintering, traditional Chinese medicinal materials are not easy to mix in the using process, the use is safer, the mixed alumina can effectively inhibit abnormal growth of zirconia matrix grains, so that the matrix material has a more uniform microstructure, the zirconia can be enhanced to a certain degree, and meanwhile, the porous structure of the zirconia enables nano ferroferric oxide wrapped by nano alumina and titanium nitride to be partially filled in pores of the zirconia, so that the combination of all raw materials is tighter, and the composite particle structure is more stable.
Further, the preparation method of the composite particle comprises the following steps:
s1: adding nano ferroferric oxide and cyanamide into absolute ethyl alcohol, magnetically stirring for 2 hours, drying in an oven at 60-80 ℃ for 20-24 hours, putting into a tubular furnace after drying, introducing titanium tetrachloride preheated to 60 ℃ into the tubular furnace by taking nitrogen as a carrier, simultaneously introducing ammonia for deposition reaction for 45-60 minutes, stopping introducing ammonia and nitrogen carrying titanium tetrachloride after the reaction is finished, introducing inert gas, and calcining at 900 ℃ for 5-8 hours to obtain nano ferroferric oxide particles coated with titanium nitride;
s2: placing the product prepared in the step S1 in a ball mill, adding rodlike nano alumina and porous zirconia, adding deionized water, performing ball milling and mixing, adding a PVA (polyvinyl alcohol) adhesive, continuing ball milling and mixing, and performing spray granulation to obtain a composite particle blank;
s3: and (3) placing the prepared composite particle blank in a muffle furnace, heating to 400-ion-doped 500 ℃ at the speed of 10-12 ℃/min, preserving heat for 2-3h, heating to 1450-ion-doped 1550 ℃ at the speed of 5-8 ℃/min, preserving heat, calcining for 2-3h, cooling to room temperature after calcining is finished, and taking out to obtain the composite particle.
Further, in the step S2, the mass ratio of the titanium nitride-coated nano ferroferric oxide to the rod-shaped nano alumina to the porous zirconia is as follows: 0.2:0.01:1
The invention has the beneficial effects that:
1. the invention discloses a preparation method of traditional Chinese medicine decoction pieces, which combines high-pressure puffing, pulse discharge plasma treatment and mechanical wall breaking, wherein the one-time wall breaking rate can reach more than 99 percent, and the one-time wall breaking rate is high, so that the preparation method is suitable for popularization and application.
2. The composite particles have good electrical conductivity and heat conductivity, can prevent the Chinese medicinal materials from generating static electricity to agglomerate and agglomerate, ensure the flowability of the Chinese medicinal materials, can lead out heat in time, avoid the local heating of the Chinese medicinal materials to a certain extent, and reduce the probability of losing activity of effective substances of the Chinese medicinal materials due to heating.
Detailed Description
The present invention will be described in detail with reference to specific examples below:
according to the preparation method of the traditional Chinese medicine decoction pieces, high-pressure puffing, pulse discharge plasma treatment and mechanical wall breaking are combined, the primary wall breaking rate is high, compared with the traditional mechanical wall breaking mode, repeated feeding is avoided, manual operation is reduced to a certain extent, and according to the characteristic that large energy is released in the pulse discharge plasma treatment process and static electricity is easily generated on the surfaces of traditional Chinese medicine materials to generate agglomeration, composite particles are mixed in the traditional Chinese medicine materials, and the composite particles are formed by wrapping nano ferroferric oxide with titanium nitride and then mixing and firing the wrapped nano ferroferric oxide with porous zirconia and rodlike nano alumina, have good electric conductivity and heat conductivity, and can conduct away static electricity and heat on the surfaces of the traditional Chinese medicine materials in time, and are as follows:
example one
Preparation of composite particles
S1, adding 0.75Kg of nano ferroferric oxide and 0.5Kg of cyanamide into 45L of anhydrous ethanol, magnetically stirring for 2 hours, drying in an oven at 80 ℃ for 20 hours, putting in a tubular furnace after drying, introducing titanium tetrachloride preheated to 60 ℃ into the tubular furnace by taking nitrogen as a carrier, preheating the titanium tetrachloride in a bubbler, controlling the volume flow of the nitrogen to be 200L/min, passing the titanium tetrachloride in the bubbler, then introducing the titanium tetrachloride into the tubular furnace, introducing ammonia for deposition reaction for 45 minutes at the flow of 100L/min, stopping introducing the nitrogen carrying the ammonia and the titanium tetrachloride after the reaction is finished, introducing inert gas, selecting the nitrogen for explanation in the embodiment, and calcining at 900 ℃ for 8 hours in nitrogen atmosphere to obtain the nano ferroferric oxide particles coated with titanium nitride;
s2: weighing 1Kg of product prepared in the step S1, placing the product in a ball mill, adding 0.05Kg of rodlike nano alumina and 5Kg of porous zirconia, adding 3Kg of deionized water, performing ball milling and mixing, adding 0.01Kg of adhesive PVA, continuing ball milling and mixing, and performing spray granulation to obtain a composite particle blank;
s3: and (3) placing the prepared composite particle blank in a muffle furnace, heating to 500 ℃ at the speed of 10 ℃/min, preserving heat for 3h, heating to 1450 ℃ at the speed of 5 ℃/min, preserving heat, calcining for 3h, cooling to room temperature after calcining is finished, and taking out the composite particle.
The method for breaking the wall of the ganoderma lucidum spore powder by using the prepared composite particles specifically comprises the following steps:
high-pressure puffing: freezing 5Kg of Ganoderma spore powder at-5 deg.C for 11h, puffing at 85 deg.C and 12MPa in a puffing machine, and cooling to room temperature to obtain puffed Ganoderma spore powder;
and (3) pulse discharge plasma treatment: stirring and mixing 5Kg of puffed ganoderma spore powder and 5Kg of composite particles uniformly, performing pulse discharge plasma treatment for 5min by using argon as working gas under the conditions that the pulse discharge voltage is 25kV and the pulse frequency is 500Hz, and separating the composite particles by magnetic separation after the treatment is finished to obtain pre-wall-broken ganoderma spore powder;
mechanical wall breaking: and (3) placing the pre-wall-broken ganoderma lucidum spore powder into a wall breaking machine to carry out mechanical wall breaking to obtain the wall-broken ganoderma lucidum spore powder traditional Chinese medicine decoction pieces.
The wall breaking rate of the ganoderma lucidum spore powder after wall breaking by microscopic examination is 99.4%.
Example two
Preparation of composite particles
S1, adding 1Kg of nano ferroferric oxide and 0.84Kg of cyanamide into 50L of anhydrous ethanol, magnetically stirring for 2 hours, drying in a 75 ℃ oven for 22 hours, putting in a tubular furnace after drying, introducing titanium tetrachloride preheated to 60 ℃ into the tubular furnace by taking nitrogen as a carrier, preheating the titanium tetrachloride in a bubbler, controlling the volume flow of the nitrogen to be 250L/min, passing the titanium tetrachloride in the bubbler, then introducing the titanium tetrachloride into the tubular furnace, introducing ammonia for deposition reaction for 60 minutes at the flow of 120L/min, stopping introducing ammonia and nitrogen carrying titanium tetrachloride after the reaction is finished, introducing inert gas, selecting nitrogen for illustration, and calcining at 900 ℃ for 6 hours in nitrogen atmosphere to obtain the nano ferroferric oxide particles coated with titanium nitride;
s2: weighing 1.5Kg of S1, putting the product prepared in the step into a ball mill, adding 0.075Kg of rodlike nano alumina and 7.5Kg of porous zirconia, adding 4.5Kg of deionized water, carrying out ball milling and mixing, adding 0.015Kg of adhesive PVA, continuing ball milling and mixing, and carrying out spray granulation to obtain a composite particle blank;
s3: and (3) placing the prepared composite particle blank in a muffle furnace, heating to 450 ℃ at the speed of 11 ℃/min, preserving heat for 3h, heating to 1550 ℃ at the speed of 8 ℃/min, preserving heat, calcining for 2h, cooling to room temperature after calcining is finished, and taking out the composite particle.
The method for breaking the pollen wall by using the prepared composite particles specifically comprises the following steps:
high-pressure puffing: freezing 6.5kg of pollen at-20 deg.C for 10 hr, puffing at 90 deg.C under 10MPa in a puffing machine, and cooling to room temperature to obtain puffed pollen;
and (3) pulse discharge plasma treatment: uniformly stirring and mixing 6.5kg of puffed pollen and 6.5kg of composite particles, carrying out pulse discharge plasma treatment for 8min by taking argon as working gas under the conditions that the pulse discharge voltage is 30kV and the pulse frequency is 520Hz, and separating out the composite particles by magnetic separation after the treatment is finished to obtain pre-wall-broken pollen;
mechanical wall breaking: and (3) placing the pre-wall-broken pollen into a wall-breaking machine to perform mechanical wall breaking to obtain the wall-broken pollen traditional Chinese medicine decoction pieces.
The wall breaking rate of the pollen after wall breaking by microscopic examination is 99.1%.
EXAMPLE III
Preparation of composite particles
S1, adding 0.92Kg of nano ferroferric oxide and 0.69Kg of cyanamide into 45L of anhydrous ethanol, magnetically stirring for 2 hours, drying in a 60 ℃ oven for 24 hours, putting into a tubular furnace after drying, introducing titanium tetrachloride preheated to 60 ℃ into the tubular furnace by taking nitrogen as a carrier, preheating the titanium tetrachloride in a bubbler, controlling the volume flow of the nitrogen to be 200L/min, passing the titanium tetrachloride in the bubbler, then introducing into the tubular furnace, introducing ammonia for deposition reaction for 50 minutes at the flow of 100L/min, stopping introducing ammonia and nitrogen carrying titanium tetrachloride after the reaction is finished, introducing inert gas, selecting nitrogen for explanation, and calcining at 900 ℃ for 5 hours in nitrogen atmosphere to obtain nano ferroferric oxide particles coated with titanium nitride;
s2: weighing 1.2Kg of product prepared in the step S1, placing the product in a ball mill, adding 0.06Kg of rodlike nano alumina and 6Kg of porous zirconia, adding 3.5Kg of deionized water, performing ball milling and mixing, adding 0.011Kg of adhesive PVA, continuing ball milling and mixing, and performing spray granulation to obtain a composite particle blank;
s3: and (3) placing the prepared composite particle blank in a muffle furnace, heating to 400 ℃ at the speed of 12 ℃/min, preserving heat for 2h, heating to 1500 ℃ at the speed of 6 ℃/min, preserving heat, calcining for 2h, cooling to room temperature after calcining is finished, and taking out the composite particle.
The method for breaking the wall of the ganoderma lucidum spore powder by using the prepared composite particles specifically comprises the following steps:
germination and culture: selecting fresh and plump Ganoderma spore powder, adjusting water content of Ganoderma spore powder to 75-85% with deionized water, and culturing at 25-30 deg.C under shading and heat preservation for 30-48 h.
High-pressure puffing: freezing 5.5Kg of Ganoderma spore powder subjected to germination culture at-15 deg.C for 12 hr, puffing at 85 deg.C under 11MPa in a puffing machine, and cooling to room temperature to obtain puffed Ganoderma spore powder;
and (3) pulse discharge plasma treatment: stirring and mixing 5Kg of puffed ganoderma spore powder and 5Kg of composite particles uniformly, performing pulse discharge plasma treatment for 6min by using argon as working gas under the conditions that the pulse discharge voltage is 35kV and the pulse frequency is 550Hz, and separating the composite particles by magnetic separation after the treatment is finished to obtain pre-wall-broken ganoderma spore powder;
mechanical wall breaking: and (3) placing the pre-wall-broken ganoderma lucidum spore powder into a wall breaking machine to carry out mechanical wall breaking to obtain the wall-broken ganoderma lucidum spore powder traditional Chinese medicine decoction pieces.
The wall breaking rate of the ganoderma lucidum spore powder after wall breaking by microscopic examination is 99.85%.
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims. The techniques, shapes, and configurations not described in detail in the present invention are all known techniques.
Claims (9)
1. The preparation method of the traditional Chinese medicine decoction pieces is characterized by comprising the following steps:
high-pressure puffing: freezing the selected traditional Chinese medicinal materials at low temperature, then putting the traditional Chinese medicinal materials into a bulking machine, bulking at low temperature and high pressure, and cooling to room temperature after the bulking is completed to obtain bulked traditional Chinese medicinal materials;
and (3) pulse discharge plasma treatment: mixing the puffed traditional Chinese medicinal materials and the composite particles, performing pulse discharge plasma treatment, and separating the composite particles by magnetic separation after the treatment is finished to obtain the traditional Chinese medicinal materials with the wall broken in advance;
mechanical wall breaking: mechanically breaking the wall of the Chinese medicinal materials to obtain Chinese medicinal decoction pieces.
2. The method for preparing decoction pieces of Chinese medicinal herbs in accordance with claim 1, wherein the temperature of said low-temperature freezing treatment is-20 to-5 ℃ and the treatment time is 10 to 12 hours.
3. The method for preparing herbal pieces prepared for decoction as claimed in claim 1, wherein the puffing at low temperature and high pressure is carried out under the pressure of 10-12MPa at 85-90 deg.C for 1-2min with nitrogen as the pressurizing gas.
4. The method as claimed in claim 3, wherein the pulsed discharge plasma treatment comprises argon as working gas, the pulsed discharge voltage is 25-35kV, the pulse frequency is 500-550Hz, and the treatment time is 5-8 min.
5. The method for preparing herbal pieces-for-decoction as set forth in claim 4, further comprising a germination culturing step before the high-pressure puffing step, wherein the germination culturing step is specifically: adjusting water content of the Chinese medicinal materials to 75-85% with deionized water, and culturing at 25-30 deg.C under shading and heat preservation for 30-48 h.
6. The method for preparing decoction pieces of Chinese medicinal herbs according to claim 5, wherein said Chinese medicinal herbs are Ganoderma lucidum spore powder or pollen.
7. The method for preparing decoction pieces of Chinese medicinal materials according to any one of claims 1 to 6, wherein the composite particles are prepared by coating nano ferroferric oxide with titanium nitride, and mixing with porous zirconia and rod-like nano alumina.
8. The method for preparing herbal pieces-according to claim 7, wherein the method for preparing said composite particles comprises the steps of:
s1: adding nano ferroferric oxide and cyanamide into absolute ethyl alcohol, magnetically stirring for 2 hours, drying in an oven at 60-80 ℃ for 20-24 hours, putting into a tubular furnace after drying, introducing titanium tetrachloride preheated to 60 ℃ into the tubular furnace by taking nitrogen as a carrier, simultaneously introducing ammonia for deposition reaction for 45-60 minutes, stopping introducing ammonia and nitrogen carrying titanium tetrachloride after the reaction is finished, introducing inert gas, and calcining at 900 ℃ for 5-8 hours to obtain nano ferroferric oxide particles coated with titanium nitride;
s2: placing the product prepared in the step S1 in a ball mill, adding rodlike nano alumina and porous zirconia, adding deionized water, performing ball milling and mixing, adding a PVA (polyvinyl alcohol) adhesive, continuing ball milling and mixing, and performing spray granulation to obtain a composite particle blank;
s3: and (3) placing the prepared composite particle blank in a muffle furnace, heating to 400-ion-doped 500 ℃ at the speed of 10-12 ℃/min, preserving heat for 2-3h, heating to 1450-ion-doped 1550 ℃ at the speed of 5-8 ℃/min, preserving heat, calcining for 2-3h, cooling to room temperature after calcining is finished, and taking out to obtain the composite particle.
9. The method for preparing decoction pieces of traditional Chinese medicine according to claim 8, wherein in the step S2, the mass ratio of the nano ferroferric oxide, the rodlike nano alumina and the porous zirconia coated with the titanium nitride is as follows: 0.2:0.01:1.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111840347A (en) * | 2020-09-01 | 2020-10-30 | 江西纳弗堂制药有限公司 | Preparation method of nano traditional Chinese medicine decoction pieces |
| CN115380977A (en) * | 2022-08-08 | 2022-11-25 | 广东润源中天生物科技有限公司 | Preparation method of ganoderma lucidum, wolfberry fruit and jujube tea and ganoderma lucidum, wolfberry fruit and jujube tea |
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