CN114504608B - Anti-cold granules and preparation method thereof - Google Patents
Anti-cold granules and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of traditional Chinese medicine preparations, and provides anti-cold granules and a preparation method thereof. The preparation method comprises the following steps: (1) Preparing a honeysuckle extract, preparing a red paeony root extract and preparing a rhizoma dryopteris crassirhizomae extract; (2) Mixing flos Lonicerae extract, radix Paeoniae Rubra extract and rhizoma Dryopteris Crassirhizomatis extract, concentrating under reduced pressure to obtain fluid extract, adding adjuvants, and making into anti-cold granule. The preparation method can obviously improve the content of 15 effective components in the anti-influenza particles, has simple preparation process, and is suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of traditional Chinese medicine preparations, and particularly relates to anti-cold granules and a preparation method thereof.
Background
The anti-cold granules serving as one of the medicines for treating the cold are popular because the anti-cold granules have smaller toxic and side effects and better and obvious effects compared with western medicines and can improve the body resistance.
The anti-cold granule comprises flos Lonicerae, radix Paeoniae Rubra and rhizoma Dryopteris Crassirhizomatis as main ingredients. The traditional preparation method adopts a water extraction and alcohol precipitation method. The anti-cold granules prepared by the traditional method have low content of active ingredients of the medicine and large waste of raw material medicines.
Patent No. CN 105079135B provides a Chinese medicinal composition for treating common cold and its preparation method, wherein the preparation method comprises extracting effective components from raw materials under ultrahigh pressure, and mixing with natural clarifier to prevent moisture absorption and agglomeration of the granule. According to the experimental data of the patent, the content of paeoniflorin and aspidin is mainly improved, and the improvement degree is limited.
The anti-influenza granule mainly comprises 15 effective components: chlorogenic acid, neochlorogenic acid, cryptochlorogenic acid, swertiamarin, rutin, isochlorogenic acid B, isochlorogenic acid A and isochlorogenic acid C from flos Lonicerae; paeoniflorin, oxypaeoniflorin, albiflorin, gallic acid, and pentagalloylglucose from radix Paeoniae Rubra; and protocatechuic acid and p-hydroxybenzoic acid from rhizoma Dryopteris Crassirhizomatis.
How to simultaneously increase the content of the effective components in the anti-influenza particles is a problem to be solved urgently.
Disclosure of Invention
In view of the above-mentioned disadvantages in the prior art, the first objective of the present invention is to provide a method for preparing anti-influenza granules, which can significantly increase the content of 15 effective ingredients in the anti-influenza granules, and the preparation process is simple and suitable for industrial production.
In view of the above-mentioned disadvantages of the prior art, a second object of the present invention is to provide an anti-influenza particle having a high content of active ingredients.
In order to achieve the above purpose, the solution adopted by the invention is as follows:
a method of preparing anti-influenza particles comprising: (1) preparation of honeysuckle extract: soaking honeysuckle in distilled water, mixing the honeysuckle with the first aqueous solution according to a mass ratio of 1 to 12-15, carrying out ultrasonic extraction for 25-35min at a power of 80-120W, keeping the pH value of the first aqueous solution at 3.8-4.2, filtering, and concentrating under reduced pressure to obtain a honeysuckle extract; preparing a red peony root extract: soaking radix Paeoniae Rubra in distilled water, mixing radix Paeoniae Rubra and second aqueous solution at a mass ratio of 1-18-22, ultrasonically extracting at a power of 80-120W for 25-35min, wherein the pH of the second aqueous solution is 4.5-5.0, filtering, concentrating under reduced pressure to obtain radix Paeoniae Rubra water extract, adding natural clarifier into the radix Paeoniae Rubra water extract, and collecting supernatant to obtain radix Paeoniae Rubra extract; preparation of rhizoma dryopteris crassirhizomae extract: soaking rhizoma Dryopteris Crassirhizomatis in distilled water, mixing the rhizoma Dryopteris Crassirhizomatis and a third aqueous solution at a mass ratio of 1-12, ultrasonically extracting at a power of 80-120W for 25-35min, wherein the pH of the third aqueous solution is 5.5-6, filtering, and concentrating under reduced pressure to obtain rhizoma Dryopteris Crassirhizomatis extract; the mass ratio of the honeysuckle to the red peony root to the male fern rhizome is 3; (2) Mixing flos Lonicerae extract, radix Paeoniae Rubra extract and rhizoma Dryopteris Crassirhizomatis extract, and concentrating under reduced pressure to obtain fluid extract with relative density of 1.3; adding adjuvants into the fluid extract to obtain anti-cold granule.
An anti-influenza granule prepared by the above preparation method.
The anti-influenza particle and the preparation method thereof provided by the invention have the beneficial effects that:
(1) The preparation method of the anti-cold particle provided by the invention is different from the traditional method in which the active ingredients are extracted after the three raw material medicines are mixed, but the three raw material medicines are extracted separately, so that the problem that the active ingredients of other raw material medicines are easily decomposed due to different pH values of water extracts of the raw material medicines is solved, and the extraction rate of each active ingredient is further improved;
(2) In the application, the pH values of different aqueous solutions are set according to the pH values of different raw material medicine aqueous extracts, so that the stability of the effective components during extraction can be greatly improved, and the leaching rate of the effective components is further improved;
(3) Ultrasonic extraction is adopted, the energy of the ultrasonic extraction is concentrated, higher temperature can be generated, and violent vibration is generated to cause cavitation in a wave body; in the application, the process conditions of ultrasonic extraction are limited aiming at extracting different active ingredients of different raw material medicines, and all process parameters are matched with each other, so that the leaching rate of the active ingredients can be greatly improved, the extraction time can be shortened, the environmental pollution caused by adopting ethanol can be avoided, and the characteristics and the quality of the extract can be well maintained under the condition that the extraction times are only 1 time and the solvent only adopts water;
(4) Secondly, the natural clarifying agent is added in the preparation step of the red paeony root extract to precipitate the starch in the red paeony root, and compared with the patent documents in the background art, the influence of the starch in the red paeony root on the honeysuckle water extract and the rhizoma dryopteris crassirhizomae water extract can be almost completely avoided, so that the leaching rate of each effective component is further improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are conventional products which are not indicated by manufacturers and are commercially available.
The anti-influenza particles and the preparation method thereof provided by the embodiments of the present invention are specifically described below.
The invention provides a preparation method of anti-influenza particles, which comprises the following steps: pretreatment: honeysuckle, red peony root and rhizoma dryopteris crassirhizomae are all plant crude drugs, the cell tissues are compact, the cell walls are thick, and the solvent is not easy to permeate, so that the effective components are difficult to leach. The surface area of the traditional Chinese medicinal materials can be increased after the traditional Chinese medicinal materials are crushed, so that the effective components are easier to leach, and the leaching speed can be increased. In the application, considering that the powder is easy to fly due to too small crushed particle size and the effect cannot be achieved due to too large crushed particle size, the honeysuckle, the red paeony root and the male fern rhizome are all crushed and sieved by a 20-mesh sieve.
During leaching, the temperature is higher under most conditions, so that the traditional Chinese medicine raw materials are directly contacted with a thermal solvent, a surface protein layer is heated and solidified, and the subsequent permeation of the solvent to cell tissues is hindered. In the application, before formal leaching, honeysuckle and distilled water are respectively mixed according to a weight ratio of 1.
(1) Preparing a honeysuckle extract: soaking flos Lonicerae in distilled water, mixing flos Lonicerae and the first aqueous solution at a mass ratio of 1-12-15, ultrasonically extracting at power of 80-120W for 25-35min, keeping pH of the first aqueous solution at 3.8-4.2, filtering, and concentrating under reduced pressure to obtain flos Lonicerae extract.
In the preparation process of the honeysuckle extract, the process parameters can be matched with each other in a synergistic manner, particularly, the temperature of the solvent can be naturally raised during ultrasonic extraction, so that the leaching rate is increased, the extraction time can be shortened during ultrasonic extraction, and the extraction frequency is reduced.
Preparing a red peony root extract: soaking radix Paeoniae Rubra in distilled water, mixing radix Paeoniae Rubra and second aqueous solution at a mass ratio of 1-18-22, ultrasonic extracting at power of 80-120W for 25-35min, wherein the pH of the second aqueous solution is 4.5-5.0, filtering, and concentrating under reduced pressure to obtain radix Paeoniae Rubra water extract; adding ZTC1+1 natural clarifier pretreatment agent A with the mass of 0.2% of that of red peony root into red peony root aqueous extract, stirring, boiling for 20min, cooling the liquid medicine to 60 ℃, adding an equivalent amount of ZTC1+1 natural clarifier pretreatment agent B, stirring, keeping the temperature at 60 ℃ for 6h, boiling for 30min, adding 6 percent ZTC1+1 natural clarifier IIB when the liquid medicine temperature is reduced to 70 ℃, stirring, keeping the temperature for 20min, adding 2 percent ZTC1+1 natural clarifier IIA, stirring, boiling for 1h; cooling, standing at room temperature for 10 hr, filtering, and concentrating under reduced pressure to obtain radix Paeoniae Rubra extract.
The red paeony root extract can greatly increase the leaching rate according to the mutual matching of the extraction process parameters, and the natural clarification method is adopted to precipitate the starch in the red paeony root when the red paeony root aqueous extract is preliminarily obtained, so that on one hand, the leaching rate of the red paeony root extract can be improved, on the other hand, the subsequent influence on the honeysuckle extract and the cyrtomium fortunei extract can be avoided, and the product quality is prevented from being influenced by the viscosity generated in the filtering process.
Preparing the rhizoma dryopteris crassirhizomae extract: soaking rhizoma Dryopteris Crassirhizomatis in distilled water, mixing rhizoma Dryopteris Crassirhizomatis and the third aqueous solution at a mass ratio of 1-12, ultrasonically extracting at a power of 80-120W for 25-35min, wherein the pH of the third aqueous solution is 5.5-6, filtering, and concentrating under reduced pressure to obtain rhizoma Dryopteris Crassirhizomatis extract. In the present embodiment, the mass ratio of honeysuckle, red peony root and male fern rhizome is 3.
(2) Mixing flos Lonicerae extract, radix Paeoniae Rubra extract and rhizoma Dryopteris Crassirhizomatis extract, and concentrating under reduced pressure at 70-75 deg.C to obtain fluid extract with relative density of 1.3; adding adjuvants into the fluid extract to obtain anti-cold granule.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment provides a preparation method of anti-influenza particles, which comprises the following steps: (1) preparation of honeysuckle extract: crushing honeysuckle, sieving with a 20-mesh sieve, adding 20 times of distilled water by weight, stirring and soaking at a rotating speed of 80r/min for 2 hours, mixing the honeysuckle with a first aqueous solution according to a mass ratio of 1 to 12, performing ultrasonic extraction at a power of 80W for 35 minutes, keeping the pH of the first aqueous solution at 3.8, filtering, and performing reduced pressure concentration to obtain a honeysuckle extract; preparing a red peony root extract: crushing the red paeony root, sieving the crushed red paeony root with a 20-mesh sieve, adding 20 times of distilled water by weight, stirring and soaking the mixture for 2 hours at the rotating speed of 80r/min, mixing the red paeony root and a second aqueous solution according to the mass ratio of 1; adding ZTC1+1 natural clarifier pretreatment agent A with the mass of 0.2% of that of red peony root into red peony root aqueous extract, stirring, boiling for 20min, cooling the liquid medicine to 60 ℃, adding an equivalent amount of ZTC1+1 natural clarifier pretreatment agent B, stirring, keeping the temperature at 60 ℃ for 6h, boiling for 30min, adding 6 percent ZTC1+1 natural clarifier IIB when the liquid medicine temperature is reduced to 70 ℃, stirring, keeping the temperature for 20min, adding 2 percent ZTC1+1 natural clarifier IIA, stirring, boiling for 1h; cooling, standing at room temperature for 10 hr, filtering, and concentrating under reduced pressure to obtain radix Paeoniae Rubra extract; preparing the rhizoma dryopteris crassirhizomae extract: crushing rhizoma dryopteris crassirhizomae, sieving with a 20-mesh sieve, adding 20 times of distilled water by weight, stirring and soaking at a rotating speed of 80r/min for 2h, mixing the rhizoma dryopteris crassirhizomae and a third aqueous solution according to a mass ratio of 1; the mass ratio of the honeysuckle to the red peony root to the male fern rhizome is 3; (2) Mixing flos Lonicerae extract, radix Paeoniae Rubra extract and rhizoma Dryopteris Crassirhizomatis extract, and concentrating under reduced pressure at 70 deg.C to obtain fluid extract with relative density of 1.3; adding adjuvants into the fluid extract to obtain anti-cold granule.
Example 2
The embodiment provides a preparation method of anti-influenza particles, which comprises the following steps: (1) preparation of honeysuckle extract: crushing honeysuckle, sieving with a 20-mesh sieve, adding 20 times of distilled water by weight, stirring and soaking at a rotating speed of 100r/min for 2 hours, mixing the honeysuckle with a first aqueous solution according to a mass ratio of 1; preparing a red peony root extract: crushing the red paeony root, sieving the crushed red paeony root with a 20-mesh sieve, adding 20 times of distilled water by weight, stirring and soaking the mixture for 2 hours at the rotating speed of 100r/min, mixing the red paeony root and a second aqueous solution according to the mass ratio of 1; adding ZTC1+1 natural clarifier pretreatment agent A with the mass of 0.2% of that of the red peony root into the red peony root aqueous extract, stirring, boiling for 20min, cooling the liquid medicine to 60 ℃, adding an equivalent amount of ZTC1+1 natural clarifier pretreatment agent B, stirring, preserving heat for 6h at 60 ℃, boiling for 30min, adding 6% ZTC1+1 natural clarifier IIB when the liquid medicine temperature is reduced to 70 ℃, stirring, preserving heat for 20min, adding 2% ZTC1+1 natural clarifier IIA, stirring, boiling for 1h; cooling, standing at room temperature for 10 hr, filtering, and concentrating under reduced pressure to obtain radix Paeoniae Rubra extract; preparing the rhizoma dryopteris crassirhizomae extract: crushing rhizoma dryopteris crassirhizomae, sieving with a 20-mesh sieve, adding 20 times of distilled water by weight, stirring and soaking at a rotating speed of 100r/min for 2h, mixing the rhizoma dryopteris crassirhizomae and a third aqueous solution according to a mass ratio of 1; the mass ratio of the honeysuckle to the red peony root to the male fern rhizome is 3; (2) Mixing flos Lonicerae extract, radix Paeoniae Rubra extract and rhizoma Dryopteris Crassirhizomatis extract, and concentrating under reduced pressure at 75 deg.C to obtain fluid extract with relative density of 1.3; adding adjuvants into the fluid extract to obtain anti-cold granule.
Example 3
The embodiment provides a preparation method of anti-influenza particles, which comprises the following steps: (1) preparation of honeysuckle extract: pulverizing flos Lonicerae, sieving with a 20-mesh sieve, adding 20 times of distilled water, stirring and soaking at 90r/min for 2h, mixing flos Lonicerae and the first aqueous solution according to a mass ratio of 1:13, performing ultrasonic extraction at a power of 100W for 30min, keeping pH of the first aqueous solution at 4.0, filtering, and concentrating under reduced pressure to obtain flos Lonicerae extract; preparing a red peony root extract: crushing the red paeony root, sieving the crushed red paeony root by a sieve of 20 meshes, adding distilled water with the weight of 20 times of the crushed red paeony root, stirring and soaking the mixture for 2 hours at the rotating speed of 90r/min, mixing the red paeony root and a second aqueous solution according to the mass ratio of 1 to 20, carrying out ultrasonic extraction at the power of 100W for 30 minutes, and carrying out filtration and reduced pressure concentration to obtain a red paeony root aqueous extract, wherein the pH value of the second aqueous solution is 4.8; adding ZTC1+1 natural clarifier pretreatment agent A with the mass of 0.2% of that of red peony root into red peony root aqueous extract, stirring, boiling for 20min, cooling the liquid medicine to 60 ℃, adding an equivalent amount of ZTC1+1 natural clarifier pretreatment agent B, stirring, keeping the temperature at 60 ℃ for 6h, boiling for 30min, adding 6 percent ZTC1+1 natural clarifier IIB when the liquid medicine temperature is reduced to 70 ℃, stirring, keeping the temperature for 20min, adding 2 percent ZTC1+1 natural clarifier IIA, stirring, boiling for 1h; cooling, standing at room temperature for 10 hr, filtering, and concentrating under reduced pressure to obtain radix Paeoniae Rubra extract; preparing the rhizoma dryopteris crassirhizomae extract: crushing rhizoma dryopteris crassirhizomae, sieving with a 20-mesh sieve, adding 20 times of distilled water by weight, stirring and soaking at a rotation speed of 90r/min for 2h, mixing the rhizoma dryopteris crassirhizomae and a third aqueous solution according to a mass ratio of 1; the mass ratio of the honeysuckle to the red peony root to the male fern rhizome is 3; (2) Mixing flos Lonicerae extract, radix Paeoniae Rubra extract and rhizoma Dryopteris Crassirhizomatis extract, and concentrating under reduced pressure at 72 deg.C to obtain fluid extract with relative density of 1.3; adding adjuvants into the fluid extract to obtain anti-cold granule.
Comparative example 1
The present comparative example provides a method of preparing an anti-influenza particle comprising: (1) preparing a honeysuckle extract: crushing honeysuckle, sieving with a 20-mesh sieve, adding 20 times of distilled water by weight, stirring and soaking at a rotating speed of 90r/min for 2 hours, mixing the honeysuckle with the first aqueous solution according to a mass ratio of 1; preparing a red peony root extract: crushing red paeony root, sieving with a 20-mesh sieve, adding 20 times of distilled water by weight, stirring and soaking for 2 hours at the rotating speed of 90r/min, mixing the red paeony root with a second aqueous solution according to the mass ratio of 1; adding ZTC1+1 natural clarifier pretreatment agent A with the mass of 0.2% of that of red peony root into red peony root aqueous extract, stirring, boiling for 20min, cooling the liquid medicine to 60 ℃, adding an equivalent amount of ZTC1+1 natural clarifier pretreatment agent B, stirring, keeping the temperature at 60 ℃ for 6h, boiling for 30min, adding 6 percent ZTC1+1 natural clarifier IIB when the liquid medicine temperature is reduced to 70 ℃, stirring, keeping the temperature for 20min, adding 2 percent ZTC1+1 natural clarifier IIA, stirring, boiling for 1h; cooling, standing at room temperature for 10 hr, filtering, and concentrating under reduced pressure to obtain radix Paeoniae Rubra extract; preparing the rhizoma dryopteris crassirhizomae extract: crushing rhizoma dryopteris crassirhizomae, sieving with a 20-mesh sieve, adding 20 times of distilled water by weight, stirring and soaking at a rotating speed of 90r/min for 2h, mixing the rhizoma dryopteris crassirhizomae and a third aqueous solution according to a mass ratio of 1; the mass ratio of the honeysuckle to the red peony root to the male fern rhizome is 3; (2) Mixing flos Lonicerae extract, radix Paeoniae Rubra extract and rhizoma Dryopteris Crassirhizomatis extract, and concentrating under reduced pressure at 72 deg.C to obtain fluid extract with relative density of 1.3; adding adjuvants into the fluid extract to obtain anti-cold granule.
Comparative example 2
The present comparative example provides a method of preparing an anti-influenza particle comprising: (1) preparation of honeysuckle extract: pulverizing flos Lonicerae, sieving with a 20-mesh sieve, adding 20 times of distilled water, stirring and soaking at 90r/min for 2h, mixing flos Lonicerae and the first aqueous solution according to a mass ratio of 1:13, performing ultrasonic extraction at a power of 100W for 30min, keeping pH of the first aqueous solution at 4.0, filtering, and concentrating under reduced pressure to obtain flos Lonicerae extract; preparing a red peony root extract: crushing the red paeony root, sieving the crushed red paeony root with a 20-mesh sieve, adding 20 times of distilled water by weight, stirring and soaking the mixture for 2 hours at the rotating speed of 90r/min, mixing the red paeony root and a second aqueous solution according to the mass ratio of 1; preparation of rhizoma dryopteris crassirhizomae extract: crushing rhizoma dryopteris crassirhizomae, sieving with a 20-mesh sieve, adding 20 times of distilled water by weight, stirring and soaking at a rotating speed of 90r/min for 2h, mixing the rhizoma dryopteris crassirhizomae and a third aqueous solution according to a mass ratio of 1; the mass ratio of the honeysuckle to the red peony root to the male fern rhizome is 3; (2) Mixing the honeysuckle extract, the red paeony root extract and the male fern rhizome extract, adding a ZTC1+1 natural clarifying agent pretreating agent A with the mass of 0.2 percent of that of the red paeony root into the mixture, stirring, boiling for 20min, cooling the liquid medicine to 60 ℃, adding an equivalent amount of the ZTC1+1 natural clarifying agent pretreating agent B into the mixture, stirring, preserving the heat for 6h at 60 ℃, boiling for 30min, adding 6 percent ZTC1+1 natural clarifying agent IIB into the mixture after the liquid medicine is cooled to 70 ℃, stirring, preserving the heat for 20min, adding 2 percent ZTC1+1 natural clarifying agent IIA into the mixture, stirring, and boiling for 1h; cooling, standing at room temperature for 10 hr, filtering, and concentrating under reduced pressure to obtain fluid extract with relative density of 1.3 at 72 deg.C; adding adjuvants into the fluid extract to obtain anti-cold granule.
Comparative example 3
The present comparative example provides a method of preparing an anti-influenza particle comprising: (1) preparation of honeysuckle extract: adding 20 times of distilled water by weight into honeysuckle, stirring and soaking for 2 hours at the rotating speed of 90r/min, mixing the honeysuckle with the first aqueous solution according to the mass ratio of 1; preparing a red peony root extract: adding 20 times of distilled water by weight into red paeony root, stirring and soaking for 2 hours at the rotating speed of 90r/min, mixing the red paeony root and the second aqueous solution according to the mass ratio of 1; adding ZTC1+1 natural clarifier pretreatment agent A with the mass of 0.2% of that of the red peony root into the red peony root aqueous extract, stirring, boiling for 20min, cooling the liquid medicine to 60 ℃, adding an equivalent amount of ZTC1+1 natural clarifier pretreatment agent B, stirring, preserving heat for 6h at 60 ℃, boiling for 30min, adding 6% ZTC1+1 natural clarifier IIB when the liquid medicine temperature is reduced to 70 ℃, stirring, preserving heat for 20min, adding 2% ZTC1+1 natural clarifier IIA, stirring, boiling for 1h; cooling, standing at room temperature for 10 hr, filtering, and concentrating under reduced pressure to obtain radix Paeoniae Rubra extract; preparing the rhizoma dryopteris crassirhizomae extract: adding 20 times of distilled water by weight into rhizoma Dryopteris Crassirhizomatis, stirring and soaking for 2h at the rotating speed of 90r/min, mixing the rhizoma Dryopteris Crassirhizomatis and a third aqueous solution according to the mass ratio of 1 to 14, performing ultrasonic extraction at the power of 100W for 30min, filtering, and concentrating under reduced pressure to obtain the rhizoma Dryopteris Crassirhizomatis extract; the mass ratio of the honeysuckle to the red peony root to the male fern rhizome is 3; (2) Mixing flos Lonicerae extract, radix Paeoniae Rubra extract and rhizoma Dryopteris Crassirhizomatis extract, and concentrating under reduced pressure at 72 deg.C to obtain fluid extract with relative density of 1.3; adding adjuvants into the fluid extract to obtain anti-cold granule.
Comparative example 4
The present comparative example provides a method of preparing an anti-influenza particle comprising: (1) preparation of honeysuckle extract: pulverizing flos Lonicerae, sieving with 20 mesh sieve, mixing flos Lonicerae with the first aqueous solution at a mass ratio of 1; preparing a red peony root extract: crushing the red paeony root, sieving the crushed red paeony root with a 20-mesh sieve, mixing the red paeony root with a second aqueous solution according to the mass ratio of 1; adding ZTC1+1 natural clarifier pretreatment agent A with the mass of 0.2% of that of the red peony root into the red peony root aqueous extract, stirring, boiling for 20min, cooling the liquid medicine to 60 ℃, adding an equivalent amount of ZTC1+1 natural clarifier pretreatment agent B, stirring, preserving heat for 6h at 60 ℃, boiling for 30min, adding 6% ZTC1+1 natural clarifier IIB when the liquid medicine temperature is reduced to 70 ℃, stirring, preserving heat for 20min, adding 2% ZTC1+1 natural clarifier IIA, stirring, boiling for 1h; cooling, standing at room temperature for 10 hr, filtering, and concentrating under reduced pressure to obtain radix Paeoniae Rubra extract; preparing the rhizoma dryopteris crassirhizomae extract: crushing rhizoma dryopteris crassirhizomae, sieving with a 20-mesh sieve, mixing the rhizoma dryopteris crassirhizomae and a third aqueous solution according to the mass ratio of 1; the mass ratio of the honeysuckle to the red peony root to the male fern rhizome is 3; (2) Mixing flos Lonicerae extract, radix Paeoniae Rubra extract and rhizoma Dryopteris Crassirhizomatis extract, and concentrating under reduced pressure at 72 deg.C to obtain fluid extract with relative density of 1.3; adding adjuvants into the fluid extract to obtain anti-cold granule.
Comparative example 5
The present comparative example provides a method of preparing an anti-influenza particle comprising: (1) preparation of honeysuckle extract: crushing honeysuckle, sieving with a 20-mesh sieve, adding 20 times of distilled water by weight, stirring and soaking at a rotation speed of 90r/min for 2 hours, mixing the honeysuckle with a first aqueous solution according to a mass ratio of 1 to 10, performing ultrasonic extraction at a power of 130W for 30 minutes, keeping the pH of the first aqueous solution at 5.0, filtering, and performing reduced pressure concentration to obtain a honeysuckle extract; preparing a red peony root extract: crushing the red paeony root, sieving the crushed red paeony root with a 20-mesh sieve, adding 20 times of distilled water by weight, stirring and soaking the mixture for 2 hours at the rotating speed of 90r/min, mixing the red paeony root and a second aqueous solution according to the mass ratio of 1; adding ZTC1+1 natural clarifier pretreatment agent A with the mass of 0.2% of that of red peony root into red peony root aqueous extract, stirring, boiling for 20min, cooling the liquid medicine to 60 ℃, adding an equivalent amount of ZTC1+1 natural clarifier pretreatment agent B, stirring, keeping the temperature at 60 ℃ for 6h, boiling for 30min, adding 6 percent ZTC1+1 natural clarifier IIB when the liquid medicine temperature is reduced to 70 ℃, stirring, keeping the temperature for 20min, adding 2 percent ZTC1+1 natural clarifier IIA, stirring, boiling for 1h; cooling, standing at room temperature for 10 hr, filtering, and concentrating under reduced pressure to obtain radix Paeoniae Rubra extract; preparing the rhizoma dryopteris crassirhizomae extract: crushing rhizoma dryopteris crassirhizomae, sieving with a 20-mesh sieve, adding 20 times of distilled water by weight, stirring and soaking at a rotation speed of 90r/min for 2h, mixing the rhizoma dryopteris crassirhizomae and a third aqueous solution according to a mass ratio of 1; the mass ratio of the honeysuckle to the red peony root to the male fern rhizome is 3; (2) Mixing flos Lonicerae extract, radix Paeoniae Rubra extract and rhizoma Dryopteris Crassirhizomatis extract, and concentrating under reduced pressure at 72 deg.C to obtain fluid extract with relative density of 1.3; adding adjuvants into the fluid extract to obtain anti-cold granule.
Comparative example 6
The present comparative example provides a method of preparing an anti-influenza particle comprising: (1) pretreatment: weighing the honeysuckle, the red paeony root and the rhizoma dryopteris crassirhizomae according to the mass ratio of 3; (2) Mixing the pretreated honeysuckle, the pretreated red peony root and the pretreated male fern rhizome to obtain a mixture, wherein the mass ratio of the mixture to the aqueous solution is 3:47 mixing, performing ultrasonic extraction at power of 100W for 90min, filtering, and concentrating under reduced pressure to obtain water extract; adding ZTC1+1 natural clarifier pretreatment agent A with 0.2% of radix Paeoniae Rubra into the water extract, stirring, boiling for 20min, cooling the liquid medicine to 60 deg.C, adding the same amount of ZTC1+1 natural clarifier pretreatment agent B, stirring, maintaining the temperature at 60 deg.C for 6h, boiling for 30min, adding 6% ZTC1+1 natural clarifier IIB when the liquid medicine temperature is reduced to 70 deg.C, stirring, maintaining the temperature for 20min, adding 2% ZTC1+1 natural clarifier IIA, stirring, boiling for 1h; cooling, standing at room temperature for 10 hr, filtering, and concentrating under reduced pressure to obtain extract; (2) Concentrating the extract at 72 deg.C under reduced pressure to obtain fluid extract with relative density of 1.3; adding adjuvants into the fluid extract to obtain anti-cold granule.
Comparative example 7
The comparative example (China pharmacopoeia 2000 edition I-474) provides a preparation method of anti-influenza particles, which comprises the following steps: preparing 210g of honeysuckle, 210g of red paeony root and 70g of rhizoma dryopteris crassirhizomae; decocting the three medicines twice by adding water, each time for 1.5h, mixing decoctions, filtering, concentrating the filtrate to 250ml, adding ethanol until the ethanol content reaches 50%, stirring, standing overnight, filtering, recovering ethanol from the filtrate, and concentrating to obtain fluid extract with the relative density of 1.28-1.30 (50 ℃); adding adjuvants into the fluid extract to obtain anti-cold granule.
Experimental example 1
The experimental method comprises the following steps: the anti-influenza particles prepared in examples 1 to 3 and comparative examples 1 to 7 were set as experimental groups 1 to 10, and the contents of 15 active ingredients in the anti-influenza particles were simultaneously determined by the HPLC-DAD method [ J ]. Online refined article of chinese scientific article, 2016,9 (11): the method of '2.3.7 sample assay' in 1081-1089, which measures the content of 15 active ingredients in anti-influenza granules (5 g/bag) in experimental groups 1-10, is shown in Table 1:
TABLE 1
As can be seen from the data in table 1, the anti-influenza granules prepared by the method for preparing anti-influenza granules provided in examples 1 to 3 of the present application have significantly increased contents of active ingredients.
The preparation method of comparative example 1 does not limit the pH of the aqueous solution for extracting each of the three crude drugs, and the content of each active ingredient of the anti-influenza granules prepared by the preparation method is lower than that of the anti-influenza granules prepared by the preparation method of the present application.
The preparation method of the comparative example 2 is different from the preparation method of the application examples 1-3 in the using sequence of the natural clarifying agent, the comparative example 2 is to clarify after mixing the extracts of the three raw material medicines, the effective substances in the extracts are still influenced, and the content of the effective components of the prepared anti-influenza particles is lower than that of the application.
In the preparation method of comparative example 3, the three raw materials are not crushed, and the content of each active ingredient of the anti-influenza particles prepared is lower than that of the particles prepared by the method, which indicates that the crushing particle size of the particles is beneficial to extraction of the active ingredients.
In the preparation method of the comparative example 4, the raw material medicines are not stirred and soaked, and the content of each effective component of the anti-influenza particle prepared is lower than that of the anti-influenza particle prepared by adopting the method, which shows that the stirring and soaking method is favorable for full swelling of the effective component and is more favorable for subsequent extraction.
The technological parameters for leaching of the raw material extracts in the preparation method of the comparative example 5 are out of the range of the application, and the content of each effective component in the prepared anti-influenza particles is lower than that of the anti-influenza particles prepared by adopting the application, so that the technological parameters are in synergistic cooperation in the preparation process of the raw material medicines, the leaching of the effective components can be promoted together, and the content of the effective components in the finished product is improved.
In the preparation method of the comparative example 6, the three raw material medicines are mixed together for ultrasonic extraction, and the comparative example 6 is obviously lower than that in the application from the aspect of the content of the active ingredients, so that the raw material medicines are extracted separately, the mutual influence can be avoided, and the leaching of the active ingredients of the raw material medicines is better promoted.
Comparative example 7 is the prior art for preparing anti-influenza particles provided in the chinese pharmacopoeia, the content of each active ingredient of the anti-influenza particles prepared by the preparation method provided by the present application is significantly better than that of comparative example 7, and compared with comparative example 7, the present application has the advantages of high content of active ingredients in the finished product, environmental protection and shorter extraction time.
In conclusion, by adopting the preparation method of the anti-influenza particles provided by the invention, the content of 15 effective components in the anti-influenza particles can be obviously improved, and the preparation process is simple and is suitable for industrial production.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A preparation method of anti-influenza particles is characterized by comprising the following steps: the method comprises the following steps:
(1) Preparing a honeysuckle extract: soaking honeysuckle in distilled water, mixing the honeysuckle with a first aqueous solution according to a mass ratio of 1-12-15, carrying out ultrasonic extraction for 25-35min at a power of 80-120W, keeping the pH value of the first aqueous solution at 3.8-4.2, filtering, and concentrating under reduced pressure to obtain a honeysuckle extract;
preparing a red peony root extract: soaking radix Paeoniae Rubra in distilled water, mixing radix Paeoniae Rubra and a second aqueous solution at a mass ratio of 1-18-22, ultrasonically extracting at a power of 80-120W for 25-35min, wherein the pH of the second aqueous solution is 4.5-5.0, filtering, and concentrating under reduced pressure to obtain radix Paeoniae Rubra water extract; adding ZTC1+1 natural clarifier pretreatment agent A with the mass of 0.2% of the red peony root into the red peony root aqueous extract for stirring, boiling for 20min, cooling the liquid medicine to 60 ℃, adding an equal amount of ZTC1+1 natural clarifier pretreatment agent B for stirring, preserving heat for 6h at 60 ℃, boiling for 30min, adding 6% ZTC1+1 natural clarifier IIB when the liquid medicine temperature is reduced to 70 ℃, stirring, preserving heat for 20min, then adding 2% ZTC1+1 natural clarifier IIA for stirring, boiling for 1h; cooling, standing at room temperature for 10h, filtering, and concentrating under reduced pressure to obtain radix Paeoniae Rubra extract;
preparing the rhizoma dryopteris crassirhizomae extract: soaking rhizoma Dryopteris Crassirhizomatis in distilled water, mixing the rhizoma Dryopteris Crassirhizomatis with a third aqueous solution at a mass ratio of 1-12-15, ultrasonically extracting at a power of 80-120W for 25-35min, wherein the pH of the third aqueous solution is 5.5-6, filtering, and concentrating under reduced pressure to obtain rhizoma Dryopteris Crassirhizomatis extract;
the mass ratio of the honeysuckle to the red peony root to the male fern rhizome is 3;
(2) Mixing the honeysuckle extract, the red paeony root extract and the rhizoma dryopteris crassirhizomae extract, and concentrating under reduced pressure to obtain clear paste with the relative density of 1.3; and adding auxiliary materials into the clear paste to prepare the anti-cold granules.
2. The method for producing antiinfective particles of claim 1, wherein: before the honeysuckle is soaked in distilled water, the honeysuckle is crushed and sieved by a 20-mesh sieve.
3. The method for producing antiinfective particles of claim 2, wherein: in the preparation of the honeysuckle extract, the weight ratio of the honeysuckle to the distilled water is 1.
4. The method for producing antiinfective particles of claim 1, wherein: before the red paeony root is soaked in distilled water, the red paeony root is crushed and sieved by a 20-mesh sieve.
5. The method for producing antiinfective particles of claim 4, wherein: in the preparation of the red peony root extract, the weight ratio of the red peony root to the distilled water is 1.
6. The method for producing a susceptor particle according to claim 1, wherein: before soaking the rhizoma dryopteris crassirhizomae in distilled water, crushing the rhizoma dryopteris crassirhizomae and sieving the powder with a 20-mesh sieve.
7. The method for producing antiinfective particles of claim 6, wherein: in the preparation of the rhizoma dryopteris crassirhizomae extract, the weight ratio of the rhizoma dryopteris crassirhizomae to the distilled water is 1.
8. The method for producing antiinfective particles of claim 1, wherein: in the step (2), the honeysuckle extract, the red peony root extract and the rhizoma dryopteris crassirhizomae extract are mixed and then are concentrated under reduced pressure at 70-75 ℃.
9. An anti-influenza particle produced by the production method according to any one of claims 1 to 8.
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| CN101152267A (en) * | 2006-09-28 | 2008-04-02 | 浙江大学宁波理工学院 | Method of preparing anticold grain based on ultrasound wave auxiliary extraction technology |
| CN105079135A (en) * | 2014-05-16 | 2015-11-25 | 四川好医生攀西药业有限责任公司 | Traditional Chinese medicine combination used for treating cold and preparation method thereof |
| CN105079134A (en) * | 2014-05-16 | 2015-11-25 | 四川好医生攀西药业有限责任公司 | Preparation process of traditional Chinese medicine preparation used for treating cold and application of traditional Chinese medicine preparation |
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| CN101152267A (en) * | 2006-09-28 | 2008-04-02 | 浙江大学宁波理工学院 | Method of preparing anticold grain based on ultrasound wave auxiliary extraction technology |
| CN105079135A (en) * | 2014-05-16 | 2015-11-25 | 四川好医生攀西药业有限责任公司 | Traditional Chinese medicine combination used for treating cold and preparation method thereof |
| CN105079134A (en) * | 2014-05-16 | 2015-11-25 | 四川好医生攀西药业有限责任公司 | Preparation process of traditional Chinese medicine preparation used for treating cold and application of traditional Chinese medicine preparation |
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