阅读说明：本技术 一种芍药甘草汤制剂及其制备方法 (Peony and liquorice soup preparation and preparation method thereof ) 是由 宋纹 刘志东 于 2021-02-09 设计创作，主要内容包括：本发明提供了一种芍药甘草汤制剂及其制备方法,将白芍和炙甘草通过加热煎煮、提取、过滤、浓缩、喷雾干燥得到干膏粉,再将干膏粉与辅料混合进行干法制粒,得到颗粒剂。本发明的制备方法制粒成功率高,便于大规模工业生产,且在制备过程中最大程度保留了药物活性成分,药效良好。(The invention provides a peony and licorice decoction preparation and a preparation method thereof, which comprises the steps of heating and decocting radix paeoniae alba and honey-fried licorice root, extracting, filtering, concentrating, spray-drying to obtain dry extract powder, mixing the dry extract powder with auxiliary materials, and carrying out dry granulation to obtain granules. The preparation method has high granulation success rate, is convenient for large-scale industrial production, reserves the active ingredients of the medicine to the maximum extent in the preparation process, and has good medicine effect.)

1. A peony and licorice root decoction preparation is characterized in that: the preparation is granules, the raw materials of the preparation are radix paeoniae alba and radix glycyrrhizae preparata, and the auxiliary materials comprise one or two of corn starch and dextrin.

2. A method for preparing the peony and licorice decoction preparation of claim 1, comprising the steps of:

s1: adding radix paeoniae alba and radix glycyrrhizae preparata into an extraction tank, adding water, soaking for 0.5-2 h, and then heating to boil;

s2: keeping boiling, extracting to obtain an extracting solution, boiling for 1-3 h, and stopping heating;

s3: filtering the extracting solution obtained in the step S2 while the extracting solution is hot to obtain filtrate;

s4: concentrating the filtrate obtained in S3 under reduced pressure to obtain a final concentrated solution with the relative density of 1.05-1.22 g/mL (60 ℃);

s5: spray drying the final concentrated solution obtained by S4 to obtain radix Paeoniae and Glycyrrhrizae radix decoction spray dried dry extract powder;

s6: mixing the spray-dried dry extract powder of the peony and licorice decoction with auxiliary materials, and then feeding the mixture into a dry granulating machine for granulation to obtain the peony and licorice decoction granules.

3. The method of claim 2, wherein: in the step S1, the ratio of the white paeony root to the honey-fried licorice root is 1: 1.

4. The method of claim 2, wherein: in the step S3, 2 layers of gauze or 200 mesh filter cloth are used for filtering.

5. The method of claim 2, wherein: in step S4, the filtrate is concentrated under reduced pressure at 60 ℃.

6. The method of claim 2, wherein: in the step S5, the inlet temperature of spray drying is 170 ℃, and the outlet temperature is 90 +/-2 ℃.

7. The method of claim 2, wherein: in the step S6, the ratio of the auxiliary material to the spray-dried dry extract powder of the peony and licorice decoction is 1:1, 1.5:1 or 2: 1.

8. The method of claim 2, wherein: in the granulation in the step S6, the material is fed and granulated for 1-3 times according to the feeding speed of 20-30 rpm, the rolling wheel speed of 15-30 rpm, the granulation speed of 5-15 rpm and the finishing aperture of 1.5 mm.

Technical Field

The invention belongs to the technical field of traditional Chinese medicines, and particularly relates to a peony and licorice decoction preparation and a preparation method thereof.

Background

Paeonia lactiflora and licorice decoction was first recorded in Shang Han Lun of Zhang Zhongjing, and is commonly used for relieving contracture pains caused by yin blood deficiency and malnutrition of tendons and vessels, including stomach pain, intestinal spastic pain, dysmenorrhea, other visceral colic, muscle pain, headache, eye pain, neuralgia, bronchospasm and the like.

The traditional Chinese medicine decoction usually has the defects of time-consuming decoction, inconvenient administration, extensive process, lack of quality control and the like, and the traditional Chinese medicine formula granules are granules prepared by taking the traditional Chinese medicine decoction pieces processed by standard processing as raw materials and adopting the process technologies of extraction, low-temperature concentration, instant drying and the like under the guidance of the traditional Chinese medicine theory, so that the defects of the traditional Chinese medicine decoction are overcome, and the large-scale production is facilitated. However, the traditional Chinese medicine extract is generally easy to absorb moisture, the nature of the soft material is greatly changed no matter the traditional Chinese medicine extract has high viscosity in ethanol or water, the dosage of the wetting agent or the adhesive is slightly changed, and the types, dosage range of the wetting agent and the like of the auxiliary materials for granulation are strictly controlled. In addition, the preparation process is limited, and the drug effects of the traditional Chinese medicine formula granules and the traditional Chinese medicine decoction are generally different.

Disclosure of Invention

In view of the above, the invention aims to provide a peony and licorice decoction preparation and a preparation method thereof, so as to solve the problems of difficult granulation, low granulation success rate, complex process, unsuitability for large-scale production and the like of the existing peony and licorice decoction preparation, ensure the content of active ingredients and keep good drug effect.

In order to achieve the purpose, the technical scheme of the invention is realized as follows:

a Chinese herbaceous peony and licorice root decoction preparation is a granule preparation, the raw materials of the preparation are radix paeoniae alba and radix glycyrrhizae preparata, and the auxiliary materials comprise one or two of corn starch and dextrin.

A preparation method of the peony and licorice decoction preparation comprises the following steps:

s1: adding radix paeoniae alba and radix glycyrrhizae preparata into an extraction tank, adding water, soaking for 0.5-2 h, and then heating to boil;

s2: keeping boiling, extracting to obtain an extracting solution, boiling for 1-3 h, and stopping heating;

s3: filtering the extracting solution obtained in the step S2 while the extracting solution is hot to obtain filtrate;

s4: concentrating the filtrate obtained in S3 under reduced pressure to obtain a final concentrated solution with the relative density of 1.05-1.22 g/mL (60 ℃);

s5: spray drying the final concentrated solution obtained by S4 to obtain radix Paeoniae and Glycyrrhrizae radix decoction spray dried dry extract powder;

s6: mixing the spray-dried dry extract powder of the peony and licorice decoction with auxiliary materials, and then feeding the mixture into a dry granulating machine for granulation to obtain the peony and licorice decoction granules.

Further, in the step S1, the ratio of white peony root to honey-fried licorice root is 1: 1.

Further, in step S3, filtering is performed by using 2 layers of gauze or 200 mesh filter cloth.

Further, in step S4, the filtrate was concentrated under reduced pressure at 60 ℃.

Further, in the step S5, the inlet temperature of the spray drying is 170 ℃, and the outlet temperature is 90 ± 2 ℃.

Further, in the step S6, the ratio of the auxiliary material to the spray-dried dry extract powder of the peony and licorice decoction is 1:1, 1.5:1 or 2: 1.

Further, in the granulation in the step S6, the material is fed and granulated for 1-3 times at a feeding speed of 20-30 rpm, a rolling wheel speed of 15-30 rpm, a granulation speed of 5-15 rpm and a finishing aperture of 1.5 mm.

The preparation method of the peony and licorice decoction preparation has the following advantages:

(1) according to the method, corn starch and dextrin are innovatively selected as auxiliary materials to prepare the peony and licorice decoction particles, and the granulation method is matched, so that the granulation success rate is favorably improved, and the large-scale industrial production is easily realized;

(2) the preparation method of the peony and licorice decoction provided by the invention furthest reserves active ingredients similar to the peony and licorice decoction through the steps of decoction, extraction, filtration, concentration, spray drying, granulation and the like, and has good drug effect.

Detailed Description

The invention will be described in detail with reference to specific embodiments. The examples are intended to illustrate the invention, but are not intended to limit the scope of applicability of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Example 1

The embodiment of the invention relates to a peony and licorice decoction preparation and a preparation method thereof, and the preparation method comprises the following specific steps:

(1) adding radix paeoniae alba and radix glycyrrhizae preparata into an extraction tank, wherein the ratio of the radix paeoniae alba to the radix glycyrrhizae preparata is 1:1, adding water, soaking for 0.5-2 h, and then heating to boil;

(2) keeping boiling, extracting to obtain an extracting solution, boiling for 1-3 h, and stopping heating;

(3) filtering the extracting solution obtained in the step (2) with 2 layers of gauze or 200-mesh filter cloth while the extracting solution is hot to obtain filtrate;

(4) concentrating the filtrate obtained in the step (3) at 60 ℃ under reduced pressure to obtain a final concentrated solution with the relative density of 1.05-1.22 g/mL (60 ℃);

(5) spray drying the final concentrated solution obtained in the step (4) at the inlet temperature of 170 ℃ and the outlet temperature of 90 +/-2 ℃ to obtain the peony and licorice decoction spray-dried dry paste powder;

(6) mixing the powder with auxiliary materials according to the medicine-auxiliary ratio (auxiliary materials/spray-dried dry extract powder of the peony and licorice decoction) of 1:1, 1.5:1 or 2:1, then feeding the mixture into a dry granulating machine for granulation, wherein the feeding speed is 20-30 rpm, the rolling wheel speed is 15-30 rpm, the granulating speed is 5-15 rpm, the finishing aperture is 1.5mm, and feeding and granulating the mixture for 1-3 times to finally obtain the peony and licorice decoction granules.

Example 2

The embodiment of the invention relates to a peony and licorice decoction preparation and a preparation method thereof, and the preparation method comprises the following specific steps:

(1) the following decoction pieces were put into an extraction pot: 20kg of white paeony root and 20kg of honey-fried licorice root, 560L (14 times of water) of water is added, the mixture is soaked for 1 hour (the soaking and the beating are circulated at the same time), and the mixture is heated to be boiled;

(2) boiling, respectively taking 500mL of decoction when boiling for 10min, 20min, 30min, 40min, 50min, 60min, 70min, 80min, 90min, 100min, 110min and 120min, filtering with 2 layers of gauze while hot for use, and stopping heating when boiling for 120 min; filtering the rest extractive solution with 200 mesh filter cloth;

the extracting solutions extracted in different time periods can be tested or applied according to actual requirements, and if no special application exists, the extracting solutions in specific time periods can be selected or mixed and then decompressed and compressed.

(3) Mixing the filtered extract, concentrating at 60 ℃ under reduced pressure to obtain a final concentrated solution with the relative density of 1.05-1.22 g/mL (60 ℃);

(4) spray drying the final concentrated solution at inlet temperature of 170 deg.C and outlet temperature of 90 + -2 deg.C to obtain spray dried powder of radix Paeoniae and Glycyrrhrizae radix decoction;

(5) humidifying the spray-dried dry extract powder of the peony and licorice decoction until the water content is 6%, mixing the spray-dried dry extract powder of the peony and licorice decoction with auxiliary materials according to the medicine-auxiliary ratio (auxiliary material/spray-dried dry extract powder of the peony and licorice decoction) of 1:1, 1.5:1 or 2:1, and then feeding the mixture into a dry granulating machine for granulation, wherein the feeding speed is 20-30 rpm, the rolling wheel speed is 15-30 rpm, the granulating speed is 5-15 rpm, the finishing aperture is 1.5mm, and the feeding granulation is carried out for 1-3 times, so that the peony and licorice.

Example 3

In this example, the feeding speed of a dry granulation machine was compared and the preparation method of the peony and licorice decoction preparation used was substantially the same as that of example 1 except that dextrin was selected as an auxiliary material, the drug-adjuvant ratio was 1:1, the rolling wheel speed was 23, the granulation speed was 11, and the finishing aperture was 1.5mm, and the properties of the granules obtained at feeding speeds of 21, 23, 25, 27 and 29 were examined, respectively, and the test results are detailed in table 1.

It should be noted that the present example uses the primary forming rate and the particle size as the index, and the optimum feeding speed of the granulator is preferred. The calculation method of the one-time forming rate is shown in formula (1).

The prepared granules are weighed according to a double-screening method of 'Chinese pharmacopoeia' 2020 edition, placed in a screen mesh with a first screen on the upper layer and a fifth screen on the lower layer, screened in a horizontal state, reciprocated left and right, and flapped for 3 minutes while moving the screen. Weighing the particles and powder which can not pass through the first sieve and can pass through the fifth sieve, calculating the proportion (%) of the particles and powder, and determining that the particles and powder are qualified if the proportion is less than 15%. The calculation method is shown in formula (2).

TABLE 1 Paeonia lactiflora and licorice root decoction dry granulator feeding speed investigation

The granulator appeared jammed at feed rates of 21 and 29. When the feed rate was 27, the primary molding rate was 65.3% and the particle size was 4.0%. When the feeding speeds are 23 and 25, the one-shot forming rate is less than 60%, so that the feeding speed is preferably 27.

Example 4

In this example, the rolling speed of the dry granulation machine is compared and studied, and the preparation method of the peony and licorice decoction preparation is basically the same as that of example 1, except that dextrin is selected as an auxiliary material, and the ratio of the components is 1: 1. The feeding speed was set to 27, the granulation speed was set to 11, and the finishing hole diameter was 1.5mm, and the properties of the granules obtained at the respective roller speeds of 19, 21, 25 and 27 were examined, with the primary molding ratio and the particle size as the index of examination, and the optimum roller speed of the granulator was preferred. The calculation method of the one-time forming rate and the granularity is shown in a formula (1) and a formula (2), and the test result is shown in a table 2 in detail.

TABLE 2 Paeonia lactiflora and licorice root decoction dry granulator rolling wheel speed investigation

At a wheel speed of 19, the granulator experienced jamming. When the feeding speed is 25 and 27, the one-time forming rate is less than 60 percent. When the feeding speed is 21, the one-shot forming rate is 64.6% < 65.3%, so the rolling wheel speed is preferably 23.

Example 5

In this example, the comparative study on the granulation speed of the dry granulation machine was performed, and the preparation method of the peony and licorice decoction preparation used is basically the same as that of example 1, except that dextrin was selected as an auxiliary material, and the ratio of the components to the auxiliary material was 1: 1. The feeding speed was set to 27, the rolling wheel speed was set to 23, and the finishing hole diameter was 1.5mm, and the properties of the granules obtained at the granulation speeds of 9, 10, 12 and 13 were examined, respectively, with the primary molding rate and the particle size as the index of examination, and the optimum granulation speed of the granulator was preferred. The calculation method of the one-time forming rate and the granularity is shown in formula (1) and formula (2). The test results are detailed in table 3.

TABLE 3 Paeonia lactiflora and licorice root decoction dry granulation speed investigation

The primary forming rate was < 60% at granulation speeds of 9, 10 and 12. When the granulation speed is 13, the primary molding ratio is 65.9% which is not much different from 65.3% in the case of the granulation speed 11, but the particle size at the granulation speed 13 is 6.7% which is larger than 4.0% in the case of 11, so that the granulation speed is preferably 11.

From the comprehensive examples 3-5, it can be seen that the parameters of the dry granulation-granulator for the peony and licorice root decoction are 27rmp of feeding speed, 23rmp of rolling wheel speed and 11rmp of granulation speed, the one-time forming rate of the obtained granules is 65.3%, and the granules have good shape.

Example 6

In this example, a comparative study is performed on the dry granulation auxiliary materials of the peony and licorice root decoction, and the preparation method of the adopted peony and licorice root decoction preparation is basically the same as that in example 1, except that two auxiliary materials of corn starch and dextrin are respectively selected for dry granulation of the peony and licorice root decoction, and the corn starch and the dextrin and the spray-dried dry extract powder of the peony and licorice root decoction are respectively prepared at a ratio of 1: 1; 1.5: 1; feeding and granulating the mixed powder with the ratio of 2:1 for three times according to the feeding speed of 27rpm, the rolling wheel speed of 23rpm, the granulating speed of 11rpm and the finishing aperture of 1.5mm, collecting granules and recording each index parameter. Respectively investigating the drug-adjuvant ratio of 1: 1; 1.5:1 and 2:1, and the optimal auxiliary material proportion is preferably selected by taking the one-time forming rate, the three-time forming rate, the dissolubility and the moisture as evaluation indexes. The results are detailed in Table 4.

The calculation method of the one-time forming rate is shown in formula (1).

The third forming rate is that the same powder put into the dry type granulator is sieved after being prepared into granules, the powder is fed again, the third forming is repeated for three times, and the granules prepared by the third forming accounts for the proportion of the fed material. The calculation method is shown in formula (3).

Solubility: according to 2020 < Chinese pharmacopoeia > taking 10g of the granules, adding 200ml of hot water, stirring for 5 minutes, immediately observing, and observing the dissolution state of the granules. The Chinese medicine granules are qualified if the Chinese medicine granules are completely dissolved or slightly turbid and have no coke breeze.

Moisture content: the moisture content of the granules was measured directly by MJ33 moisture meter (manufacturer: Mettler-Torledo, temperature range 50-160 deg.C).

TABLE 4 radix Paeoniae and radix Glycyrrhizae decoction Dry granulation adjuvant investigation

The auxiliary materials are dextrin: the granulator is stuck when the medicine-assistant ratio is 2: 1. When the medicine-assistant ratio is 1:1, the one-time forming rate is 67.2%, the three-time forming rate is 89.3%, the granularity is 2.7%, and the water content of the granules is 3.02%. The dissolution time is about 200s, and the granules are brown yellow suspension after dissolution, and all indexes are better. When the ratio of the drug to the adjuvant is 1.5:1, the tertiary molding rate is high, but the particle size is too large, so that the particles are easy to loosen. Therefore, when dextrin is selected as the auxiliary material, the optimal medicine-auxiliary ratio is 1: 1.

The auxiliary materials are corn starch: when the medicine-assistant ratio is 1:1 and 2:1, the one-time forming rate is less than 60 percent, and the three-time forming rate is less than 80 percent. When the medicine-assistant ratio is 1.5:1, the one-time forming rate is 61.5%, the three-time forming rate is 85.8%, the granularity is 2.8%, the water content of the granules is 3.32%, the dissolving time is 150s, and the granules are in brown yellow suspension after being dissolved, so that the indexes are all better. Therefore, when starch is selected as the auxiliary material, the optimal medicine-auxiliary ratio is 1.5: 1.

The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.