阅读说明：本技术 一种冻干粉的制备方法 (Preparation method of freeze-dried powder ) 是由 张志强 刘香云 姚杭琦 张美玲 周永康 程立伟 于 2021-05-27 设计创作，主要内容包括：本发明属于冻干粉制备技术领域,具体涉及一种冻干粉的制备方法。该方法包括将中药提取液置于预冻结温度下,然后升温至25-35℃,得到中药冻干粉；所述预冻结温度低于中药提取液共晶点5～14℃；所述预冻结温度升温至25-35℃的过程中至少包括8个保温过程。该方法得到的冻干粉能够保持原体积,没有出现塌陷、表面光洁,可整块脱落且不散碎,色泽均匀,无花斑,质地细腻。另外,本发明提供的方法制备得到的冻干粉的含水量低、复溶时间短,比表面积和孔隙率均有所增加,有效降低冻干粉的复溶时间。(The invention belongs to the technical field of freeze-dried powder preparation, and particularly relates to a preparation method of freeze-dried powder. The method comprises placing the Chinese medicinal extractive solution at pre-freezing temperature, and heating to 25-35 deg.C to obtain Chinese medicinal lyophilized powder; the pre-freezing temperature is 5-14 ℃ lower than the eutectic point of the traditional Chinese medicine extracting solution; the process of raising the pre-freezing temperature to 25-35 ℃ at least comprises 8 heat preservation processes. The obtained lyophilized powder can maintain original volume, has no collapse, smooth surface, uniform color, no mottle, and fine texture, and can be dropped off in one piece without breaking. In addition, the freeze-dried powder prepared by the method provided by the invention has low water content, short redissolution time, increased specific surface area and porosity and effectively reduced redissolution time.)

1. A method for preparing freeze-dried powder is characterized by comprising the following steps,

placing the traditional Chinese medicine extracting solution at a pre-freezing temperature, and then heating to 25-35 ℃ to obtain traditional Chinese medicine freeze-dried powder;

the pre-freezing temperature is 5-14 ℃ lower than the eutectic point of the traditional Chinese medicine extracting solution;

the process of raising the pre-freezing temperature to 25-35 ℃ at least comprises 8 heat preservation processes;

the heat preservation time of each heat preservation process is not less than 3 h.

2. The production method according to claim 1, wherein the heat-retaining process includes a first heat-retaining process, a second heat-retaining process, a third heat-retaining process, a fourth heat-retaining process, a fifth heat-retaining process, a sixth heat-retaining process, a seventh heat-retaining process, and an eighth heat-retaining process;

the first heat preservation process is carried out at a pre-freezing temperature;

and the heat preservation temperature of the eighth heat preservation process is 25-35 ℃.

3. The method according to claim 2, wherein the difference between the holding temperature of the second holding process and the holding temperature of the first holding process is not more than 10 ℃;

the difference of the heat preservation temperature of the third heat preservation process and the second heat preservation process is not more than 15 ℃;

the difference of the heat preservation temperature of the fourth heat preservation process and the third heat preservation process is not more than 15 ℃;

the difference of the heat preservation temperature of the fifth heat preservation process and the fourth heat preservation process is not more than 15 ℃;

the difference of the heat preservation temperature of the sixth heat preservation process and the fifth heat preservation process is not more than 20 ℃;

the temperature of the seventh heat preservation process is not lower than 0 ℃.

4. The preparation method according to any one of claims 1 to 3, wherein the holding time of the first holding process is not less than 3 hours;

the heat preservation time of the second heat preservation process and the third heat preservation process is not less than 5 hours;

the heat preservation time of the fourth heat preservation process, the fifth heat preservation process, the sixth heat preservation process and the seventh heat preservation process is not less than 3 hours;

and the heat preservation time of the eighth heat preservation process is not less than 7 h.

5. The preparation method according to claim 4, wherein the first heat preservation process is carried out for 3-4 hours;

the heat preservation time of the second heat preservation process is 5-6 hours;

the heat preservation time of the third heat preservation process is 5-6 hours;

the heat preservation time of the fourth heat preservation process is 3-4 hours;

the heat preservation time of the fifth heat preservation process is 3-4 hours;

the heat preservation time of the sixth heat preservation process is 3-4 hours;

the heat preservation time of the seventh heat preservation process is 3-4 hours;

and the heat preservation time of the eighth heat preservation process is 7-8 h.

6. The method according to any one of claims 1 to 5, wherein the herbal extract is a herbal concentrate having a density of 1.00 to 1.05 g/ml.

7. The method for preparing the Chinese medicinal extract as claimed in any one of claims 1 to 6, wherein the extraction method comprises decocting the decoction pieces in water for 1 to 3 times, and concentrating under reduced pressure until the concentration density is 1.00 to 1.05 g/ml.

8. The preparation method of any one of claims 1 to 7, wherein the difference between the highest liquid level and the lowest liquid level of the Chinese medicinal extract is not more than 1cm when the freeze-dried powder is prepared.

9. The method according to any one of claims 1 to 8, wherein the source of the Chinese medicinal extract is a medicinal material rich in sugar, oil and volatile oil and a general medicinal material.

10. Lyophilized powder prepared by the method of any one of claims 1 to 9.

Technical Field

The invention belongs to the technical field of freeze-dried powder preparation, and particularly relates to a preparation method of freeze-dried powder.

Background

At present, most of traditional Chinese medicine products are divided into decoction pieces, Chinese patent medicines and traditional Chinese medicine formula granules, and for modern urban life, the granules have the advantages of convenient carrying and storage, no need of decoction and preparation by warm water, and have gradually gained the recognition of more doctors and patients. The Chinese medicinal components comprise effective components, auxiliary components and ineffective components. The extraction process involves the processes of extraction, separation, concentration, purification, refining, drying and the like, and the types of the extracted traditional Chinese medicine components have close relation with the quality of the product. Wherein, the operation of selecting proper temperature and method to dry the traditional Chinese medicine extracting solution is one of the important steps for producing most preparations of the traditional Chinese medicine.

The vacuum freeze drying technology is a technology combining vacuum, freezing and drying, and is a process of freezing a dried substance at a low temperature and then directly sublimating frozen water molecules into water vapor to escape in a proper vacuum environment. The vacuum freeze drying technology is developed rapidly in the field of food and medicine in recent years, the technology not only has various advantages of the traditional drying technology, but also realizes the preservation of material structure, shape and the like under the influence of the development of the technology and keeps the living activity of effective components at normal temperature; compared with vacuum reduced pressure drying and spray drying, the vacuum freeze drying has the advantages of no deterioration of samples, easy long-term storage, thorough dehydration, easy redissolution, easy aseptic operation, contribution to keeping the activity of thermosensitive medicaments, less loss of volatile components and the like. Aiming at the vacuum freeze drying process of the traditional Chinese medicine extracting solution, a process for preparing high-quality freeze-dried powder is also lacked.

In the prior art, the problems of collapse, bubbling, uneven texture and difficult powder collection are easy to occur in the process of preparing the freeze-dried powder. In addition, the time of the freeze-drying process is generally more than 50h, the freeze-drying time is long, and the production energy consumption is relatively large.

Disclosure of Invention

Therefore, the technical problem to be solved by the invention is to overcome the defects of easy collapse, bubbling, uneven texture, difficult powder collection and the like in the preparation process of the freeze-dried powder in the prior art. Therefore, a method for preparing freeze-dried powder is provided.

Therefore, the invention provides the following technical scheme.

The invention provides a preparation method of freeze-dried powder, which comprises the following steps,

placing the traditional Chinese medicine extracting solution at a pre-freezing temperature, and then heating to 25-35 ℃ to obtain traditional Chinese medicine freeze-dried powder;

the pre-freezing temperature is 5-14 ℃ lower than the eutectic point of the traditional Chinese medicine extracting solution;

the process of raising the pre-freezing temperature to 25-35 ℃ at least comprises 8 heat preservation processes;

the heat preservation time of each heat preservation process is not less than 3 h.

The heat preservation process comprises a first heat preservation process, a second heat preservation process, a third heat preservation process, a fourth heat preservation process, a fifth heat preservation process, a sixth heat preservation process, a seventh heat preservation process and an eighth heat preservation process;

the first heat preservation process is carried out at a pre-freezing temperature;

the heat preservation temperature in the eighth heat preservation process is 25-35 ℃.

Further, the difference of the heat preservation temperature of the second heat preservation process and the first heat preservation process is not more than 10 ℃;

the difference of the heat preservation temperature of the third heat preservation process and the second heat preservation process is not more than 15 ℃;

the difference of the heat preservation temperature of the fourth heat preservation process and the third heat preservation process is not more than 15 ℃;

the difference of the heat preservation temperature of the fifth heat preservation process and the fourth heat preservation process is not more than 15 ℃;

the difference of the heat preservation temperature of the sixth heat preservation process and the fifth heat preservation process is not more than 20 ℃;

the temperature of the seventh heat preservation process is not lower than 0 ℃.

Further, the heat preservation time of the first heat preservation process is not less than 3 hours;

the heat preservation time of the second heat preservation process and the third heat preservation process is not less than 5 hours;

the heat preservation time of the fourth heat preservation process, the fifth heat preservation process, the sixth heat preservation process and the seventh heat preservation process is not less than 3 hours;

and the heat preservation time of the eighth heat preservation process is not less than 7 h.

Further, the heat preservation time of the first heat preservation process is 3-4 h;

the heat preservation time of the second heat preservation process is 5-6 hours;

the heat preservation time of the third heat preservation process is 5-6 hours;

the heat preservation time of the fourth heat preservation process is 3-4 hours;

the heat preservation time of the fifth heat preservation process is 3-4 hours;

the heat preservation time of the sixth heat preservation process is 3-4 hours;

the heat preservation time of the seventh heat preservation process is 3-4 hours;

and the heat preservation time of the eighth heat preservation process is 7-8 h.

The traditional Chinese medicine extracting solution is a traditional Chinese medicine concentrated solution with the density of 1.00-1.05 g/ml.

The extraction method of the traditional Chinese medicine extracting solution comprises the steps of adding water into decoction pieces, decocting for 1-3 times, and concentrating under reduced pressure until the density of a concentrated solution is 1.00-1.05 g/ml; preferably, the drinking tablets are decocted by adding water, filtered by filter cloth of 130-150 meshes and combined, the liquid medicine is decompressed and concentrated under the conditions that the rotating speed is 50-60 r/min and the temperature is 50-60 ℃, and then the liquid medicine is placed in a vacuum freeze dryer for drying to obtain freeze-dried powder.

The freeze-dried powder can be prepared by the method, can also be prepared by other methods in the prior art, and can also be purchased.

Further, when the freeze-dried powder is prepared, the difference value between the highest liquid level and the lowest liquid level of the traditional Chinese medicine extracting solution is not more than 1 cm.

The traditional Chinese medicine extracting solution is prepared from medicinal materials rich in sugar, grease and volatile oil and common medicinal materials; wherein, the general medicinal materials refer to medicinal materials without sugar, oil and volatile oil.

The Chinese medicinal extract can be from single Chinese medicinal material or compound Chinese medicinal material.

The Chinese medicinal extractive solution can be derived from, but not limited to, Hypericum perforatum, parched fructus Vitics Simplicifoliae, fructus Leonuri, fructus Vitics Simplicifoliae, herba Cynomorii, herba Artemisiae Anomalae, rhizoma Wenyujin Concisa, fructus Akebiae or rhizoma Zingiberis and rhizoma Atractylodis decoction.

Taking hypericum perforatum as an example, the heat preservation process comprises a first heat preservation process, a second heat preservation process, a third heat preservation process, a fourth heat preservation process, a fifth heat preservation process, a sixth heat preservation process, a seventh heat preservation process and an eighth heat preservation process, and the temperature of each heat preservation process is as follows:

the temperature of the first heat preservation process is-35 ℃ to-30 ℃; the temperature of the second heat preservation process is-29 ℃ to-25 ℃; the temperature of the third heat preservation process is-20 ℃ to-15 ℃; the temperature of the fourth heat preservation process is-14 ℃ to-10 ℃; the temperature of the fifth heat preservation process is-9 ℃ to-5 ℃; the temperature of the sixth heat preservation process is 0-4 ℃; the temperature of the seventh heat preservation process is 10-15 ℃; the temperature of the eighth heat preservation process is 25-30 ℃.

Taking fried chastetree fruit as an example, the heat preservation process comprises a first heat preservation process, a second heat preservation process, a third heat preservation process, a fourth heat preservation process, a fifth heat preservation process, a sixth heat preservation process, a seventh heat preservation process and an eighth heat preservation process, and the temperature of each heat preservation process is as follows:

the temperature of the first heat preservation process is-35 ℃ to-30 ℃; the temperature of the second heat preservation process is-29 ℃ to-25 ℃; the temperature of the third heat preservation process is-20 ℃ to-15 ℃; the temperature of the fourth heat preservation process is-14 ℃ to-10 ℃; the temperature of the fifth heat preservation process is-9 ℃ to-5 ℃; the temperature of the sixth heat preservation process is 0-4 ℃; the temperature of the seventh heat preservation process is 10-15 ℃; the temperature of the eighth heat preservation process is 25-30 ℃.

Taking motherwort fruit as an example, the heat preservation process comprises a first heat preservation process, a second heat preservation process, a third heat preservation process, a fourth heat preservation process, a fifth heat preservation process, a sixth heat preservation process, a seventh heat preservation process and an eighth heat preservation process, wherein the temperature of each heat preservation process is respectively as follows:

the temperature of the first heat preservation process is-50 ℃ to-45 ℃; the temperature of the second heat preservation process is-44 ℃ to-40 ℃; the temperature of the third heat preservation process is-35 ℃ to-30 ℃; the temperature of the fourth heat preservation process is-25 ℃ to-20 ℃; the temperature of the fifth heat preservation process is-15 ℃ to-10 ℃; the temperature of the sixth heat preservation process is 0-4 ℃; the temperature of the seventh heat preservation process is 10-15 ℃; the temperature of the eighth heat preservation process is 20-25 ℃.

Taking fructus viticis as an example, the heat preservation process comprises a first heat preservation process, a second heat preservation process, a third heat preservation process, a fourth heat preservation process, a fifth heat preservation process, a sixth heat preservation process, a seventh heat preservation process and an eighth heat preservation process, and the temperature of each heat preservation process is respectively as follows:

the temperature of the first heat preservation process is-35 ℃ to-30 ℃; the temperature of the second heat preservation process is-29 ℃ to-25 ℃; the temperature of the third heat preservation process is-20 ℃ to-15 ℃; the temperature of the fourth heat preservation process is-14 ℃ to-10 ℃; the temperature of the fifth heat preservation process is-9 ℃ to-5 ℃; the temperature of the sixth heat preservation process is 0-4 ℃; the temperature of the seventh heat preservation process is 10-15 ℃; the temperature of the eighth heat preservation process is 25-30 ℃.

Taking the cynomorium as an example, the heat preservation process comprises a first heat preservation process, a second heat preservation process, a third heat preservation process, a fourth heat preservation process, a fifth heat preservation process, a sixth heat preservation process, a seventh heat preservation process and an eighth heat preservation process, and the temperature of each heat preservation process is respectively as follows:

the temperature of the first heat preservation process is-45 ℃ to-40 ℃; the temperature of the second heat preservation process is-39 ℃ to-35 ℃; the temperature of the third heat preservation process is-29 ℃ to-25 ℃; the temperature of the fourth heat preservation process is-19 ℃ to-15 ℃; the temperature of the fifth heat preservation process is-9 ℃ to-5 ℃; the temperature of the sixth heat preservation process is 0-4 ℃; the temperature of the seventh heat preservation process is 10-15 ℃; the temperature of the eighth heat preservation process is 25-30 ℃.

Taking artemisia anomala as an example, the heat preservation process comprises a first heat preservation process, a second heat preservation process, a third heat preservation process, a fourth heat preservation process, a fifth heat preservation process, a sixth heat preservation process, a seventh heat preservation process and an eighth heat preservation process, and the temperature of each heat preservation process is as follows:

the temperature of the first heat preservation process is-40 ℃ to-35 ℃; the temperature of the second heat preservation process is-35 ℃ to-30 ℃; the temperature of the third heat preservation process is-30 ℃ to-25 ℃; the temperature of the fourth heat preservation process is-25 ℃ to-20 ℃; the temperature of the fifth heat preservation process is-20 ℃ to-15 ℃; the temperature of the sixth heat preservation process is-15 ℃ to 0 ℃; the temperature of the seventh heat preservation process is 0-15 ℃; the temperature of the eighth heat preservation process is 25-35 ℃.

Taking rhizoma curcumae longae as an example, the heat preservation process comprises a first heat preservation process, a second heat preservation process, a third heat preservation process, a fourth heat preservation process, a fifth heat preservation process, a sixth heat preservation process, a seventh heat preservation process and an eighth heat preservation process, and the temperature of each heat preservation process is respectively as follows:

the temperature of the first heat preservation process is-45 ℃ to-40 ℃; the temperature of the second heat preservation process is-40 ℃ to-35 ℃; the temperature of the third heat preservation process is-35 ℃ to-30 ℃; the temperature of the fourth heat preservation process is-30 ℃ to-20 ℃; the temperature of the fifth heat preservation process is-20 ℃ to-15 ℃; the temperature of the sixth heat preservation process is-15 ℃ to 0 ℃; the temperature of the seventh heat preservation process is 0-15 ℃; the temperature of the eighth heat preservation process is 25-35 ℃.

Taking a predictor as an example, the heat preservation process comprises a first heat preservation process, a second heat preservation process, a third heat preservation process, a fourth heat preservation process, a fifth heat preservation process, a sixth heat preservation process, a seventh heat preservation process and an eighth heat preservation process, and the temperature of each heat preservation process is as follows:

the temperature of the first heat preservation process is-40 ℃ to-35 ℃; the temperature of the second heat preservation process is-35 ℃ to-30 ℃; the temperature of the third heat preservation process is-30 ℃ to-25 ℃; the temperature of the fourth heat preservation process is-25 ℃ to-20 ℃; the temperature of the fifth heat preservation process is-20 ℃ to-15 ℃; the temperature of the sixth heat preservation process is-15 ℃ to 0 ℃; the temperature of the seventh heat preservation process is 0-15 ℃; the temperature of the eighth heat preservation process is 25-35 ℃.

The invention also provides the freeze-dried powder prepared by the preparation method.

The freeze-dried powder is redissolved in water at the temperature of 80-100 ℃, and the mass concentration of the redissolved solution is 0.01-0.1 g/ml.

The freeze-dried powder obtained by the invention has no suspended matters and no precipitate after redissolution.

The technical scheme of the invention has the following advantages:

1. the preparation method of the freeze-dried powder provided by the invention comprises the steps of placing a traditional Chinese medicine extracting solution at a pre-freezing temperature, and then heating to 25-35 ℃ to obtain the traditional Chinese medicine freeze-dried powder; the pre-freezing temperature is 5-14 ℃ lower than the eutectic point of the traditional Chinese medicine extracting solution; the process of raising the pre-freezing temperature to 25-35 ℃ at least comprises 8 heat preservation processes; the heat preservation time of each heat preservation process is not less than 3 h. The obtained lyophilized powder can maintain original volume, has no collapse, smooth surface, uniform color, no mottle, and fine texture, and can be dropped off in one piece without breaking. In addition, the freeze-dried powder prepared by the method provided by the invention has low water content, short redissolution time, increased specific surface area and porosity and effectively reduced redissolution time.

According to the preparation method of the freeze-dried powder, the gradient of the temperature of the Chinese medicine extract is improved and maintained, so that the damage of a material structure and the influence of effective components caused by large-scale temperature change are avoided, the phenomena of insufficient drying and material collapse frequently encountered in the process of slow temperature rise are solved, and the quality of the freeze-dried powder is effectively improved.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.

FIG. 1 is a graph showing the resistance and temperature changes of Hypericum perforatum measured in example 1 of the present invention;

FIG. 2 is the appearance diagram of the freeze-dried powder of Hypericum perforatum of example 1 of the present invention;

FIG. 3 is a graph showing the measured resistance and temperature changes of parched fructus Vitics Simplicifoliae in example 2 of the present invention;

FIG. 4 is a diagram showing the appearance of lyophilized powder of Chastetree fruit according to example 2 of the present invention;

FIG. 5 is a graph showing the variation of the resistance and temperature of the motherwort fruit tested in example 3 of the present invention;

FIG. 6 is an appearance diagram of the motherwort fruit lyophilized powder of embodiment 3 of the present invention;

FIG. 7 is a graph showing the resistance and temperature changes of Vitex rotundifolia according to example 4 of the invention;

FIG. 8 is a diagram showing the appearance of lyophilized powder of Vitex rotundifolia according to example 4 of the invention;

FIG. 9 is a graph showing the resistance and temperature change of the cynomorium songaricum measured in example 5 of the present invention;

FIG. 10 is an appearance diagram of lyophilized powder of Cynomorium songaricum of example 5 of the present invention;

FIG. 11 is a graph of the resistance and temperature changes of Siphonostegia chinensis measured in example 6 of the present invention;

fig. 12 is a diagram of the appearance of lyophilized north artemisia anomala powder in example 6 of the present invention;

FIG. 13 is a graph showing the resistance and temperature changes of turmeric pieces measured in example 7 of the present invention;

FIG. 14 is a diagram showing the appearance of lyophilized powder of Wenyujin Concisa of example 7 of the present invention;

FIG. 15 is a graph showing the measured predicted subesistance and temperature changes in example 8 of the present invention;

FIG. 16 is a diagram showing the appearance of lyophilized powder of example 8 of the present invention;

FIG. 17 is a graph showing the resistance and temperature changes of Ganjiangyu decoction measured in example 9 of the present invention;

FIG. 18 is a diagram of measuring the appearance of the lyophilized powder of Ganjing Lingzhu decoction in example 9 of the present invention;

FIG. 19 is a diagram showing the appearance of the freeze-dried powder of Hypericum perforatum of comparative example 1;

FIG. 20 is a diagram showing the appearance of the freeze-dried powder of Hypericum perforatum of comparative example 2 of the present invention.

Detailed Description

The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.

The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.

The freeze dryer used in the following examples and comparative examples was of the type VFD-2000A.

Example 1

The embodiment provides a preparation method of hypericum perforatum freeze-dried powder, which comprises the following steps,

preparing a hypericum perforatum extract: taking 100g of herba Hyperici perforati decoction pieces, adding 12 times of water for decocting one time, soaking for 30min, and decocting for 20 min; adding water 10 times the amount of decoction pieces into the second decoction, decocting for 15min, filtering the two decoctions with 150 mesh filter cloth, mixing filtrates, and concentrating the filtrate at 55r/min under reduced pressure at 55 deg.C until the concentration density is 1.05g/ml to obtain herba Hyperici perforati Chinese medicinal extractive solution.

Determining the eutectic point of hypericum perforatum: placing appropriate amount of herba Hyperici perforati extract in a material tray, inserting platinum resistance temperature probe and electrode into the extract (the two electrodes and temperature probe are spaced at a certain distance and do not touch the bottom of the sample tray), placing in a freeze drying chamber of a freeze dryer, and refrigerating. And in the temperature change process, synchronously reading the resistance omega at the two ends of the resistor and the temperature value T of the material to be detected through a digital multimeter and a temperature measurement system of the freeze dryer. The temperature (DEG C) is taken as an abscissa, the resistance omega is taken as an ordinate to make a change curve of the resistance omega along with the temperature T, and the resistance sudden change value in the cooling process is the temperature of the eutectic point, and the result is shown in figure 1. With the graph of fig. 1, the mobile ions are gradually reduced and the resistance is gradually increased to infinity along with the continuous freezing of the free moisture in the freezing process of the hypericum perforatum extract, when the temperature is reduced to minus 26 to minus 24 ℃, the resistance of the material is suddenly increased, and the corresponding temperature is the eutectic point temperature of the hypericum perforatum, wherein the eutectic point is minus 26 to minus 24 ℃.

Preparing freeze-dried powder: placing herba Hyperici perforati traditional Chinese medicine extract in a material tray of a freeze dryer, and adjusting the liquid level height of the extract to 1 cm. Putting the mixture into a freeze dryer at normal temperature. Adjusting the temperature of the freeze dryer to a pre-freezing temperature, setting the pre-freezing temperature to be-30 ℃, and then heating to 30 ℃, wherein the heating process comprises 8 heat preservation processes, and the specific heating process comprises the following steps:

(1) preserving the heat for 4 hours at the pre-freezing temperature; (2) heating to-27 deg.C, and keeping the temperature for 6 h; (3) heating to-18 ℃ and then preserving heat for 6 h; (4) heating to-12 deg.C, and maintaining for 3 hr; (5) heating to-8 ℃ and then preserving heat for 3 h; (6) heating to 3 ℃ and then preserving heat for 3 h; (7) heating to 12 ℃, and then preserving heat for 3 h; (8) heating to 30 ℃ and then preserving heat for 8 h;

and after the heat preservation is finished, obtaining the hypericum perforatum freeze-dried powder.

The appearance state of the freeze-dried powder of hypericum perforatum obtained in this example is shown in fig. 2: can keep the original volume, does not collapse, has smooth surface, can fall off in a whole block without scattering, has uniform color, no mottle and fine texture.

Taking 10g of the hypericum perforatum freeze-dried powder obtained in the embodiment, adding 200ml of hot water with the temperature of 82 +/-2 ℃, redissolving, stirring for 5min, immediately observing that the freeze-dried powder is completely dissolved, wherein the redissolved solution has no suspended matters and no precipitate.

Measuring the water content of the freeze-dried powder, placing the freeze-dried powder in an evaporation vessel, weighing and recording again after drying, repeating twice, and taking an average value, namely the water content of the freeze-dried powder, wherein the data is as follows:

TABLE 1 moisture content of Hypericum perforatum freeze-dried powder

The water content of the hypericum perforatum freeze-dried powder obtained in the embodiment is less than 4%.

Example 2

The embodiment provides a preparation method of lyophilized powder of parched fructus viticis, which comprises the following steps,

preparing a fried chastetree fruit extracting solution: taking 200g of fried fructus viticis medicinal material decoction pieces, adding water with the amount being 12 times of that of the decoction pieces for one decoction, soaking for 30min, and then decocting for 20 min; adding water 10 times the amount of decoction pieces, decocting for 15min, filtering the two decoctions with 150 mesh filter cloth, mixing filtrates, and concentrating under reduced pressure at 55 deg.C at rotation speed of 55r/min until the concentration density is 1.05g/ml to obtain parched fructus Vitics Simplicifoliae Chinese medicinal extractive solution.

The eutectic point of parched fructus Vitics Simplicifoliae was determined according to the method for determining eutectic point of Hypericum perforatum in example 1, see FIG. 3. As can be seen from FIG. 3, the eutectic point temperature of the parched fructus viticis is-26 to-24 ℃.

Preparing freeze-dried powder: placing the parched fructus Vitics Simplicifoliae traditional Chinese medicine extract in a material tray of a freeze dryer, and adjusting the liquid level height of the extract to 1 cm. Putting the mixture into a freeze dryer at normal temperature. Adjusting the temperature of the freeze dryer to a pre-freezing temperature, setting the pre-freezing temperature to be-30 ℃, and then heating to 30 ℃, wherein the heating process comprises 8 heat preservation processes, and the specific heating process comprises the following steps:

(1) preserving the heat for 4 hours at the pre-freezing temperature; (2) heating to-27 deg.C, and keeping the temperature for 6 h; (3) heating to-18 ℃ and then preserving heat for 6 h; (4) heating to-12 deg.C, and maintaining for 3 hr; (5) heating to-8 ℃ and then preserving heat for 3 h; (6) heating to 3 ℃ and then preserving heat for 3 h; (7) heating to 12 ℃, and then preserving heat for 3 h; (8) heating to 30 ℃ and then preserving heat for 8 h;

and after the heat preservation is finished, obtaining the parched fructus viticis lyophilized powder.

The appearance state of the lyophilized powder of fructus viticis obtained in this example is shown in fig. 4: can keep the original volume, does not collapse, has smooth surface, can fall off in a whole block without scattering, has uniform color, no mottle and fine texture.

10g of the lyophilized powder of the parched fructus viticis negundo obtained in the embodiment is added with 200ml of hot water with the temperature of 82 +/-2 ℃, redissolved and stirred for 5 minutes, and the lyophilized powder is completely dissolved by immediate observation, and the redissolved solution has no suspended matters and no precipitate.

Measuring the water content of the freeze-dried powder, placing the freeze-dried powder in an evaporation vessel, weighing and recording again after drying, repeating twice, and taking an average value, namely the water content of the freeze-dried powder, wherein the data is as follows:

TABLE 2 Water content of lyophilized powder of parched fructus Vitics Simplicifoliae

The water content of the lyophilized powder of fructus viticis preparata prepared in this example is less than 5%.

Example 3

The embodiment provides a preparation method of motherwort fruit freeze-dried powder, which comprises the following steps,

preparing a motherwort fruit extracting solution: taking 100g of decoction pieces of motherwort fruit medicinal materials, adding water with the amount being 10 times of that of the decoction pieces in one decoction, soaking for 30min, and then decocting for 30 min; adding water with the amount of 8 times of the decoction pieces into the second decoction, decocting for 20min, filtering the two decoctions with 150 mesh filter cloth respectively, mixing filtrates, and concentrating the filtrate at 55r/min under reduced pressure at 55 deg.C until the concentration density is 1.05g/ml to obtain fructus Leonuri Chinese medicinal extractive solution.

The eutectic point of motherwort fruit was determined according to the method of example 1 for determining the eutectic point of hypericum perforatum, as shown in FIG. 5. As can be seen from FIG. 5, the eutectic point temperature of fructus Leonuri is-40 to-42 ℃.

Preparing freeze-dried powder: placing the Chinese medicinal extractive solution of fructus Leonuri in a material tray of a freeze dryer, and adjusting the liquid level height of the extractive solution to 1 cm. Putting the mixture into a freeze dryer at normal temperature. Adjusting the temperature of the freeze dryer to a pre-freezing temperature, setting the pre-freezing temperature to-47 ℃, and then heating to 25 ℃, wherein the heating process comprises 8 heat preservation processes, and the specific heating process comprises the following steps:

(1) preserving the heat for 4 hours at the pre-freezing temperature; (2) heating to-42 deg.C, and keeping the temperature for 6 h; (3) heating to-35 deg.C, and keeping the temperature for 6 h; (4) heating to-22 deg.C, and maintaining for 3 hr; (5) heating to-12 deg.C, and maintaining for 3 hr; (6) heating to 2 ℃ and then preserving heat for 3 h; (7) heating to 12 ℃, and then preserving heat for 3 h; (8) heating to 25 ℃, and then preserving heat for 7.5 h;

after the heat preservation is finished, the motherwort fruit freeze-dried powder is obtained.

The appearance state of the motherwort fruit freeze-dried powder obtained in this example is shown in fig. 6: can keep the original volume, does not collapse, has smooth surface, can fall off in a whole block without scattering, has uniform color, no mottle and fine texture.

10g of motherwort fruit freeze-dried powder obtained in the embodiment is taken, 200ml of hot water with the temperature of 82 +/-2 ℃ is added, redissolution is carried out, stirring is carried out for 5 minutes, and the freeze-dried powder is immediately observed to be completely dissolved, so that the redissolved solution has no suspended matters and no precipitate.

Measuring the water content of the freeze-dried powder, placing the freeze-dried powder in an evaporation vessel, weighing and recording again after drying, repeating twice, and taking an average value, namely the water content of the freeze-dried powder, wherein the data is as follows:

TABLE 3 Water content of fructus Leonuri lyophilized powder

The motherwort fruit freeze-dried powder prepared by the embodiment has the water content of less than 6%.

Example 4

The embodiment provides a method for preparing fructus viticis lyophilized powder, which comprises the following steps,

preparing a fructus viticis extracting solution: taking 100g of fructus viticis medicinal material decoction pieces, adding water with the amount being 10 times of the decoction pieces for one decoction, soaking for 30min, and then decocting for 30 min; adding water with the amount 8 times of the decoction pieces into the second decoction, decocting for 20min, filtering the two decoctions with 150 mesh filter cloth, respectively, mixing filtrates, and concentrating the filtrate at 55r/min under reduced pressure at 55 deg.C until the concentration density is 1.05g/ml to obtain fructus Vitics Simplicifoliae Chinese medicinal extractive solution.

The eutectic point of chastetree fruit was determined according to the method of example 1 for determining the eutectic point of hypericum perforatum, see fig. 7. As can be seen from FIG. 7, the eutectic point temperature of fructus Vitics Simplicifoliae is-26 to-24 ℃.

Preparing freeze-dried powder: placing the fructus Vitics Simplicifoliae traditional Chinese medicine extract in a material tray of a freeze dryer, and adjusting the liquid level height of the extract to 1 cm. Putting the mixture into a freeze dryer at normal temperature. Adjusting the temperature of the freeze dryer to a pre-freezing temperature, setting the pre-freezing temperature to be-30 ℃, and then heating to 30 ℃, wherein the heating process comprises 8 heat preservation processes, and the specific heating process comprises the following steps:

(1) preserving the heat for 4 hours at the pre-freezing temperature; (2) heating to-25 deg.C, and keeping the temperature for 5.5 h; (3) heating to-15 ℃ and then preserving heat for 6 h; (4) heating to-10 deg.C, and maintaining for 3 hr; (5) heating to-8 ℃ and then preserving heat for 3 h; (6) heating to 4 ℃ and then preserving heat for 3 h; (7) heating to 10 ℃ and then preserving heat for 3 h; (8) heating to 30 ℃ and then preserving heat for 8 h;

and after the heat preservation is finished, obtaining the fructus viticis freeze-dried powder.

The appearance state of the lyophilized powder of fructus viticis obtained in this example is shown in fig. 8: can keep the original volume, does not collapse, has smooth surface, can fall off in a whole block without scattering, has uniform color, no mottle and fine texture.

Taking 10g of the lyophilized vitex rotundifolia powder obtained in the embodiment, adding 200ml of 82 +/-2 ℃ hot water, redissolving, stirring for 5 minutes, immediately observing, and completely dissolving the lyophilized vitex rotundifolia powder, wherein the redissolved solution has no suspended matters or precipitates.

Measuring the water content of the freeze-dried powder, placing the freeze-dried powder in an evaporation vessel, weighing and recording again after drying, repeating twice, and taking an average value, namely the water content of the freeze-dried powder, wherein the data is as follows:

TABLE 4 moisture content of lyophilized powder of fructus Vitics Simplicifoliae

The water content of the lyophilized powder of fructus viticis prepared in this example is less than 6%.

Example 5

The embodiment provides a preparation method of cynomorium songaricum freeze-dried powder, which comprises the following steps,

preparing a cynomorium songaricum extracting solution: taking 100g of cynomorium songaricum medicinal decoction pieces, adding water with the amount being 10 times of that of the decoction pieces in one decoction, soaking for 30min, and then decocting for 30 min; adding water with the amount 8 times of the decoction pieces into the second decoction, decocting for 20min, filtering the two decoctions with 150 mesh filter cloth, respectively, mixing filtrates, and concentrating the filtrate at 55r/min under reduced pressure at 55 deg.C until the concentration density is 1.05g/ml to obtain herba Cynomorii Chinese medicinal extractive solution.

The eutectic point of cynomorium songaricum was measured according to the method for measuring the eutectic point of hypericum perforatum in example 1, as shown in fig. 9. As can be seen from FIG. 9, the eutectic point temperature of the cynomorium songaricum is-40 to-36 ℃.

Preparing freeze-dried powder: placing herba Cynomorii traditional Chinese medicine extractive solution in material tray of freeze dryer, and adjusting liquid level height of the extractive solution to 1 cm. Putting the mixture into a freeze dryer at normal temperature. Adjusting the temperature of the freeze dryer to a pre-freezing temperature, setting the pre-freezing temperature to be-45 ℃, and then heating to 25 ℃, wherein the heating process comprises 8 heat preservation processes, and the specific heating process comprises the following steps:

(1) preserving the heat for 4 hours at the pre-freezing temperature; (2) heating to-35 deg.C, and keeping the temperature for 5 h; (3) heating to-29 ℃ and then preserving heat for 5.5 h; (4) heating to-17 deg.C, and maintaining for 3 hr; (5) heating to-7 ℃ and then preserving heat for 3 h; (6) heating to 0 deg.C, and keeping the temperature for 3 h; (7) heating to 10 ℃ and then preserving heat for 3 h; (8) heating to 25 ℃, and then preserving heat for 8 hours;

and after the heat preservation is finished, obtaining the cynomorium songaricum freeze-dried powder.

The appearance state of the cynomorium songaricum lyophilized powder obtained in this example is shown in fig. 10: can keep the original volume, does not collapse, has smooth surface, can fall off in a whole block without scattering, has uniform color, no mottle and fine texture.

10g of the cynomorium songaricum freeze-dried powder obtained in the embodiment is added with 200ml of hot water with the temperature of 82 +/-2 ℃, redissolved and stirred for 5 minutes, and the freeze-dried powder is immediately observed to be totally dissolved, and the redissolved solution has no suspended matters and no precipitate.

Measuring the water content of the freeze-dried powder, placing the freeze-dried powder in an evaporation vessel, weighing and recording again after drying, repeating twice, and taking an average value, namely the water content of the freeze-dried powder, wherein the data is as follows:

TABLE 5 moisture content of lyophilized powder of Cynomorium songaricum

The water content of the cynomorium songaricum freeze-dried powder prepared by the embodiment is less than 4%.

Example 6

This embodiment provides a method for preparing lyophilized powder of artemisia anomala, which comprises the following steps,

preparing a artemisia anomala extracting solution: taking 100g of decoction pieces of the medicinal material of the artemisia anomala, adding water with the amount being 10 times of that of the decoction pieces in one decoction, soaking for 30min, and then decocting for 30 min; adding water with the amount of 8 times of the decoction pieces into the second decoction, decocting for 20min, filtering the two decoctions with 150 mesh filter cloth, respectively, mixing filtrates, and concentrating the filtrate at 55r/min under reduced pressure at 55 deg.C until the concentration density is 1.05g/ml to obtain herba Artemisiae Anomalae Chinese medicinal extractive solution.

The eutectic point of diverse wormwood herb was determined according to the method for determining the eutectic point of hypericum perforatum in example 1, as shown in fig. 11. As can be seen from FIG. 11, the eutectic point temperature of Siphonostegia chinensis is-32 to-29 ℃.

Preparing freeze-dried powder: placing the herba Artemisiae Anomalae traditional Chinese medicine extract in a material tray of a freeze dryer, and adjusting the liquid level height of the extract to 1 cm. Putting the mixture into a freeze dryer at normal temperature. Adjusting the temperature of the freeze dryer to a pre-freezing temperature, setting the pre-freezing temperature to-40 ℃, and then heating to 35 ℃, wherein the heating process comprises 8 heat preservation processes, and the specific heating process comprises the following steps:

(1) preserving the heat for 4 hours at the pre-freezing temperature; (2) heating to-32 ℃ and then preserving heat for 6 h; (3) heating to-30 deg.C, and keeping the temperature for 5.5 h; (4) heating to-23 deg.C, and maintaining for 3 hr; (5) heating to-18 ℃ and then preserving heat for 3 h; (6) heating to-12 deg.C, and maintaining for 3 hr; (7) heating to 10 ℃ and then preserving heat for 3 h; (8) heating to 35 ℃ and then preserving heat for 8 h;

and after the heat preservation is finished, obtaining the lyophilized powder of the artemisia anomala.

The appearance state of the lyophilized powder of artemisia anomala obtained in this example is shown in fig. 12: can keep the original volume, does not collapse, has smooth surface, can fall off in a whole block without scattering, has uniform color, no mottle and fine texture.

Taking 10g of the lyophilized powder of artemisia anomala obtained in the embodiment, adding 200ml of hot water with the temperature of 82 +/-2 ℃, redissolving, stirring for 5 minutes, immediately observing, and completely dissolving the lyophilized powder, wherein the redissolved solution has no suspended matters or precipitates.

Measuring the water content of the freeze-dried powder, placing the freeze-dried powder in an evaporation vessel, weighing and recording again after drying, repeating twice, and taking an average value, namely the water content of the freeze-dried powder, wherein the data is as follows:

TABLE 6 moisture content of lyophilized powder of Siphonostegia chinensis

The lyophilized powder of artemisia anomala prepared in this example has a water content of less than 5%.

Example 7

The embodiment provides a preparation method of turmeric tablet freeze-dried powder, which comprises the following steps,

preparing a rhizoma wenyujin concinnatae extracting solution: taking 100g of rhizoma curcumae longae decoction pieces, adding water with the amount being 10 times of that of the decoction pieces in one decoction, soaking for 30min, and then decocting for 30 min; adding water with the amount 8 times of that of decoction pieces into the second decoction, decocting for 20min, filtering the two decoctions with 150 mesh filter cloth respectively, mixing filtrates, and concentrating the filtrate at 55r/min under reduced pressure at 55 deg.C until the concentration density is 1.05g/ml to obtain rhizoma Wenyujin Concisa Chinese medicinal extract.

The co-crystal point of turmeric root-leaf was determined according to the method of example 1 for determining the co-crystal point of hypericum perforatum, see fig. 13. As can be seen from FIG. 13, the eutectic point temperature of turmeric root tuber is-36 to-33 ℃.

Preparing freeze-dried powder: placing rhizoma Wenyujin Concisa traditional Chinese medicine extract in a material tray of a freeze dryer, and adjusting the liquid level height of the extract to 1 cm. Putting the mixture into a freeze dryer at normal temperature. Adjusting the temperature of the freeze dryer to a pre-freezing temperature which is set to be-42 ℃, and then heating to 30 ℃, wherein the heating process comprises 8 heat preservation processes, and the specific heating process comprises the following steps:

(1) preserving the heat for 4 hours at the pre-freezing temperature; (2) heating to-37 deg.C, and keeping the temperature for 6 h; (3) heating to-33 ℃ and then preserving heat for 5.5 h; (4) heating to-25 ℃ and then preserving heat for 3 h; (5) heating to-18 ℃ and then preserving heat for 3 h; (6) heating to-12 deg.C, and maintaining for 3 hr; (7) heating to 15 ℃, and then preserving heat for 3 h; (8) heating to 30 ℃ and then preserving heat for 8 h;

and after the heat preservation is finished, obtaining the rhizoma wenyujin concinnatae freeze-dried powder.

The appearance state of the turmeric root tuber freeze-dried powder obtained in this example is shown in fig. 14: can keep the original volume, does not collapse, has smooth surface, can fall off in a whole block without scattering, has uniform color, no mottle and fine texture.

10g of the turmeric powder obtained in the embodiment is added with 200ml of hot water with the temperature of 82 +/-2 ℃, redissolved and stirred for 5 minutes, and the lyophilized powder is completely dissolved by immediate observation, and the redissolved solution has no suspended matters and no precipitate.

Measuring the water content of the freeze-dried powder, placing the freeze-dried powder in an evaporation vessel, weighing and recording again after drying, repeating twice, and taking an average value, namely the water content of the freeze-dried powder, wherein the data is as follows:

TABLE 7 moisture content of Wenyujin Concisa lyophilized powder

The water content of the turmeric tablet freeze-dried powder prepared by the embodiment is less than 5.5%.

Example 8

The embodiment provides a preparation method of a fructus akebiae freeze-dried powder, which comprises the following steps,

preparing a fructus akebiae extract: taking 100g of decoction pieces of fructus akebiae, adding water with the amount being 10 times of the decoction pieces for one decoction, soaking for 30min, and then decocting for 30 min; adding water with the amount 8 times of the decoction pieces into the second decoction, decocting for 20min, filtering the two decoctions with 150 mesh filter cloth, respectively, mixing filtrates, and concentrating the filtrate at 55r/min under reduced pressure at 55 deg.C until the concentration density is 1.05g/ml to obtain fructus Akebiae Chinese medicinal extractive solution.

The eutectic point of the propagules was determined according to the method of example 1 for the eutectic point of hypericum perforatum, see fig. 15. As can be seen from FIG. 15, the sub-eutectic temperature is predicted to be-30 to-26 ℃.

Preparing freeze-dried powder: placing fructus Akebiae extractive solution in material tray of freeze dryer, and adjusting liquid level height of the extractive solution to 1 cm. Putting the mixture into a freeze dryer at normal temperature. Adjusting the temperature of the freeze dryer to a pre-freezing temperature, setting the pre-freezing temperature to-38 ℃, and then heating to 28 ℃, wherein the heating process comprises 8 heat preservation processes, and the specific heating process comprises the following steps:

(1) preserving the heat for 4 hours at the pre-freezing temperature; (2) heating to-35 deg.C, and keeping the temperature for 6 h; (3) heating to-28 deg.C, and maintaining for 5.5 h; (4) heating to-23 deg.C, and maintaining for 3 hr; (5) heating to-18 ℃ and then preserving heat for 3 h; (6) heating to-8 ℃ and then preserving heat for 3 h; (7) heating to 8 ℃, and then preserving heat for 3 h; (8) heating to 28 ℃, and then preserving heat for 8 hours;

and after the heat preservation is finished, obtaining the fructus akebiae freeze-dried powder.

The appearance state of the lyophilized powder of preignition obtained in this example is shown in fig. 16: can keep the original volume, does not collapse, has smooth surface, can fall off in a whole block without scattering, has uniform color, no mottle and fine texture.

10g of the lyophilized powder of akebia fruit obtained in the example is added with 200ml of hot water with the temperature of 82 +/-2 ℃, redissolved and stirred for 5 minutes, and the lyophilized powder is completely dissolved by immediate observation, and the redissolved solution has no suspended matters and no precipitate.

Measuring the water content of the freeze-dried powder, placing the freeze-dried powder in an evaporation vessel, weighing and recording again after drying, repeating twice, and taking an average value, namely the water content of the freeze-dried powder, wherein the data is as follows:

TABLE 8 Preset Water content of lyophilized powder

The water content of the lyophilized powder of fructus akebiae prepared in this example is less than 5.2%.

Example 9

The embodiment provides a preparation method of gan Jiang Ling Zhu Tang freeze-dried powder, which comprises the following steps,

preparing an extracting solution of the gan ginger, poria and rhizoma atractylodis decoction: taking 100g of the prescription medicine of the gan Jiang Ling Shu decoction, adding water with the amount being 10 times of that of decoction pieces for one decoction, soaking for 30min, and then decocting for 90 min; filtering with 150 mesh filter cloth to obtain filtrate, cooling to room temperature, concentrating the filtrate at 55 deg.C at 55r/min under reduced pressure until the concentration is 1.04g/ml to obtain rhizoma Zingiberis recens rhizoma Atractylodis decoction Chinese medicinal extractive solution. Wherein, the prescription of the decoction of the rhizoma zingiberis, poria and rhizoma atractylodis: 6g of liquorice decoction pieces, 6g of largehead atractylodes rhizome decoction pieces, 12g of dried ginger decoction pieces and 12g of tuckahoe decoction pieces, which meet the relevant regulations under the terms of liquorice (concoction), largehead atractylodes rhizome (concoction), dried ginger (concoction) and tuckahoe (concoction) in the 2020 edition of pharmacopoeia of the people's republic of China.

The eutectic point of the gan Jiang Ling Zhu Tang was determined according to the method of determining the eutectic point of Hypericum perforatum in example 1, as shown in FIG. 17. As can be seen from FIG. 17, the eutectic point temperature of gan Jiang Ling Shu Tang is-10 to-5 ℃.

Preparing freeze-dried powder: placing the traditional Chinese medicine extract of rhizoma Zingiberis recens rhizoma Atractylodis decoction in a material tray of a freeze dryer, and adjusting the liquid level height of the extract to 1 cm. Putting the mixture into a freeze dryer at normal temperature. Adjusting the temperature of the freeze dryer to a pre-freezing temperature which is set to be-20 ℃, and then heating to 30 ℃, wherein the heating process comprises 11 heat preservation processes, and the specific heating process comprises the following steps:

(1) preserving the heat for 4 hours at the pre-freezing temperature; (2) heating to-15 ℃ and then preserving heat for 5 h; (3) heating to-10 deg.C, and keeping the temperature for 5 h; (4) heating to 0 deg.C, and keeping the temperature for 3 h; (5) heating to 5 ℃ and then preserving heat for 3 h; (6) heating to 10 ℃ and then preserving heat for 3 h; (7) heating to 15 ℃, and then preserving heat for 3 h; (8) heating to 20 ℃, and then preserving heat for 7 hours; (9) heating to 25 ℃, and then preserving heat for 3 h; (10) heating to 30 ℃ and then preserving heat for 8 h.

And after the heat preservation is finished, the gan Jiang Ling Shu Tang freeze-dried powder is obtained.

The appearance state of the gan jiang ling shu tang lyophilized powder obtained in this example is shown in fig. 18: can keep the original volume, has smooth surface, can fall off in a whole block without scattering, has uniform color, no mottle and fine texture.

10g of the freeze-dried powder of the decoction of gan Jiang Ling Zhu Tang obtained in the embodiment is added with 200ml of hot water with the temperature of 82 +/-2 ℃, redissolved and stirred for 5 minutes, and the freeze-dried powder is completely dissolved by immediate observation, and the redissolved solution has no suspended matters and no sediment.

Measuring the water content of the freeze-dried powder, placing the freeze-dried powder in an evaporation vessel, weighing and recording again after drying, repeating for three times, and taking an average value, namely the water content of the freeze-dried powder, wherein the data is as follows:

TABLE 9 Water content of gan Jiang Ling Zhu Tang Freeze-dried powder

The water content of the gan ginger ling shu decoction freeze-dried powder prepared by the embodiment is less than 6.79%.

The specific surface area and the void ratio of the freeze-dried powder provided by the embodiments 1 to 9 are increased, so that the reconstitution effect of the freeze-dried powder can be improved, and the reconstitution time can be reduced.

Comparative example 1

The comparative example provides a preparation method of hypericum perforatum freeze-dried powder, and the difference from the example 1 is that: the preparation method of the comparative example comprises 7 heat preservation processes from the pre-freezing temperature to 30 ℃, and comprises the following steps,

preparing a hypericum perforatum extract: taking 100g of herba Hyperici perforati decoction pieces, adding 12 times of water for decocting one time, soaking for 30min, and decocting for 20 min; adding water 10 times the amount of decoction pieces, decocting for 15min, filtering the two decoctions with 150 mesh filter cloth, mixing filtrates, and concentrating the filtrate at 55r under reduced pressure at 55 deg.C until the concentration density is 1.05g/ml to obtain herba Hyperici perforati Chinese medicinal extractive solution.

Determining the eutectic point of hypericum perforatum: the eutectic point of the hypericum perforatum is-26 to-24 ℃.

Preparing freeze-dried powder: placing herba Hyperici perforati traditional Chinese medicine extract in a material tray of a freeze dryer, and adjusting the liquid level height of the extract to 1 cm. Putting the mixture into a freeze dryer at normal temperature. Adjusting the temperature of the freeze dryer to a pre-freezing temperature, setting the pre-freezing temperature to be-30 ℃, and then heating to 30 ℃, wherein the heating process comprises 7 heat preservation processes, and the specific heating process comprises the following steps:

(1) preserving the heat for 4 hours at the pre-freezing temperature; (2) heating to-27 deg.C, and keeping the temperature for 8 h; (3) heating to-18 ℃ and then preserving heat for 8 h; (4) heating to-12 deg.C, and keeping the temperature for 5 h; (5) heating to-8 ℃ and then preserving heat for 5 h; (6) heating to 3 ℃ and then preserving heat for 3 h; (7) heating to 12 ℃, and then preserving heat for 3 h;

and after the heat preservation is finished, obtaining the hypericum perforatum freeze-dried powder.

The appearance state of the hypericum perforatum freeze-dried powder obtained in the comparative example is shown in figure 19: the problems of collapse, uneven texture, incomplete freeze-drying, difficult powder collection and the like of the sample occur.

The freeze-dried hypericum perforatum powder obtained in the embodiment is re-dissolved in water with the temperature of 82 +/-2 ℃, and the re-dissolving time is longer.

Measuring the water content of the freeze-dried powder, placing the freeze-dried powder in an evaporation vessel, weighing and recording again after drying, repeating twice, and taking an average value, namely the water content of the freeze-dried powder, wherein the data is as follows:

TABLE 10 moisture content of Hypericum perforatum freeze-dried powder

The water content of the freeze-dried powder obtained by the comparative example is higher.

Comparative example 2

The comparative example provides a preparation method of hypericum perforatum freeze-dried powder, which is different from the example 1 in that the preparation method of the comparative example adopts a slow temperature rise process from the pre-freezing temperature to 30 ℃, does not include a heat preservation process, and comprises the following steps,

preparing a hypericum perforatum extract: taking 100g of herba Hyperici perforati decoction pieces, adding 12 times of water for decocting one time, soaking for 30min, and decocting for 20 min; adding water 10 times the amount of decoction pieces, decocting for 15min, filtering the two decoctions with 150 mesh filter cloth, mixing filtrates, and concentrating the filtrate at 55r under reduced pressure at 55 deg.C until the concentration density is 1.05g/ml to obtain herba Hyperici perforati Chinese medicinal extractive solution.

Determining the eutectic point of hypericum perforatum: the eutectic point of the hypericum perforatum is-26 to-24 ℃.

Preparing freeze-dried powder: placing herba Hyperici perforati traditional Chinese medicine extract in a material tray of a freeze dryer, and adjusting the liquid level height of the extract to 1 cm. Putting the mixture into a freeze dryer at normal temperature. Adjusting the temperature of the freeze dryer to a pre-freezing temperature, setting the pre-freezing temperature to be-30 ℃, then heating to 30 ℃, wherein the heating process is a slow heating process, the heating time from the pre-freezing temperature to 30 ℃ is 36 hours, and the temperature is increased to 30 ℃ to obtain the hypericum perforatum freeze-dried powder.

The appearance state of the hypericum perforatum freeze-dried powder obtained in the comparative example is shown in figure 20: the sample was not lyophilized, not formed, and no lyophilized powder was obtained.

It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the spirit or scope of the invention.