CN111317784A

CN111317784A - Preparation method of concentrated Chinese angelica and Niantong pills

Info

Publication number: CN111317784A
Application number: CN202010124228.7A
Authority: CN
Inventors: 姚金龙; 李荣苗
Original assignee: JIANGXI XINGLIN BAIMA PHARMACEUTICAL CO Ltd
Current assignee: JIANGXI XINGLIN BAIMA PHARMACEUTICAL CO Ltd
Priority date: 2020-02-27
Filing date: 2020-02-27
Publication date: 2020-06-23

Abstract

The invention relates to a preparation method of a concentrated Chinese angelica Niantong pill. The method comprises extracting part A of raw materials including Notopterygii rhizoma, radix Angelicae sinensis, radix Saposhnikoviae, rhizoma Atractylodis (parched), Atractylodis rhizoma (parched), herba Artemisiae Scopariae and radix Puerariae with supercritical CO2 fluid to obtain extract A; decocting part of raw material B, radix Codonopsis, Scutellariae radix, cimicifugae rhizoma, radix Sophorae Flavescentis, Alismatis rhizoma, rhizoma anemarrhenae, Polyporus, and Glycyrrhrizae radix with water twice, filtering, and concentrating the filtrate to obtain soft extract B; and preparing the extract A, the thick paste B and auxiliary materials into concentrated angelica sinensis Niantong pills. The concentrated Chinese angelica Niantong pill prepared by the invention has definite curative effect, and solves the problems of poor compliance and influence on curative effect caused by a large number of medicines taken by patients.

Description

Preparation method of concentrated Chinese angelica and Niantong pills

Technical Field

The invention belongs to the field of traditional Chinese medicines, and particularly relates to a preparation method of a concentrated Chinese angelica and Niantong pill.

Background

The Chinese angelica and Niantong pill has the functions of clearing away heat, promoting diuresis, dispelling wind and relieving pain. Can be used for treating arthromyodynia caused by damp-heat obstruction, with symptoms of red swelling and pain of joint or red swelling and pain of foot shin; it can also be used for treating sore . The Dang Gui Niantong pill is a grayish brown watered pill with bitter taste. The preparation process in the prior art comprises the following steps: 40g of angelica, 40g of radix puerariae, 40g of codonopsis pilosula, 40g of rhizoma atractylodis (fried), 40g of rhizoma cimicifugae, 40g of radix sophorae flavescentis, 60g of rhizoma alismatis, 60g of fried rhizoma atractylodis macrocephalae, 60g of rhizoma anemarrhenae, 60g of radix sileris, 100g of notopterygium root, 100g of scutellaria baicalensis, 100g of polyporus umbellatus, 100g of oriental wormwood and 100g of liquorice, and the fifteen medicines are crushed into fine powder, sieved, mixed uniformly, made into pills with water and dried to obtain the traditional. Each 18 pills weight lg. Is administered orally. 9g once and 2 times a day.

From the above, the existing Chinese angelica Niantong pill has the dosage up to 162 pills each time, which not only has a large dosage and a large disposable dosage, but also makes the patient have trouble taking the medicine and have errors easily, and the patient has very poor compliance of taking the medicine, thereby affecting the curative effect. Therefore, it is very necessary to provide a concentrated Dang Gui Niantong pill with definite curative effect, convenient administration and small dosage.

Disclosure of Invention

The invention provides a preparation method of concentrated angelica sinensis Niantong pills on the basis of overcoming the defects that the angelica sinensis Niantong pills in the prior art are taken as many as 162 pills each time, the number of the pills is large, and the one-time dosage is large.

In order to achieve the purpose, the invention adopts the following technical scheme:

on the one hand, the preparation method of the concentrated Chinese angelica Niantong pill is provided, which comprises the following steps:

(1) weighing the following raw medicinal materials in parts by weight: 40 parts of angelica, 40 parts of radix puerariae, 40 parts of codonopsis pilosula, 40 parts of rhizoma atractylodis (fried), 40 parts of rhizoma cimicifugae, 40 parts of radix sophorae flavescentis, 60 parts of rhizoma alismatis, 60 parts of rhizoma atractylodis macrocephalae (fried), 60 parts of rhizoma anemarrhenae, 60 parts of radix sileris, 100 parts of notopterygium root, 100 parts of scutellaria baicalensis, 100 parts of grifola, 100 parts of oriental wormwood and 100 parts of liquorice;

(2) cleaning and pulverizing part A of raw materials, Notopterygii rhizoma, radix Angelicae sinensis, radix Saposhnikoviae, rhizoma Atractylodis (parched), Atractylodis rhizoma (parched), herba Artemisiae Scopariae and radix Puerariae, and extracting with supercritical CO2 fluid to obtain extract A;

(3) decocting part of the raw medicinal material B, radix codonopsis pilosulae, scutellaria baicalensis, cimicifuga foetida, radix sophorae flavescentis, rhizoma alismatis, rhizoma anemarrhenae, grifola and liquorice with water twice, adding 8-12 times of water by weight each time, decocting for 1-2 hours each time, filtering decoction, combining filtrates, and concentrating to obtain thick paste B;

(4) adding sucrose, micro-powder silica gel and a disintegrating agent into the extract A and the thick paste B obtained in the steps (2) and (3) to prepare wet pills, drying and polishing to obtain the concentrated Chinese angelica Niantong pills.

Further, the supercritical CO2 fluid extraction method in the step (2) comprises the following specific steps: the raw medicinal materials after being cleaned and crushed are extracted for 2 to 4 hours at constant temperature and pressure under the conditions of extraction pressure of 20 to 30Mpa, extraction temperature of 40 to 50 ℃, resolution pressure of 6 to 7Mpa, resolution temperature of 40 to 50 ℃ and CO2 flow rate of 250 to 350kg/h, and extract A is obtained.

Further, the relative density of the thick paste B in the step (3) is 1.2-1.4.

Further, the disintegrating agent in the step (4) is at least one of starch, sodium carboxymethyl starch or low-substituted hydroxypropyl cellulose.

Further, the drying in the step (4) is carried out under the conditions that the steam pressure is 0.40-0.60 Mpa, the drying temperature is 50-80 ℃, and the moisture is less than or equal to 8.0%.

On the other hand, the concentrated Chinese angelica Niantong pill prepared by the method is provided.

The invention has the following positive effects:

the concentrated Chinese angelica Niantong pills prepared by the invention are orally taken 2g at a time, namely 20 concentrated pills, per 10 pills are heavy, the existing pills are twisted, as many as 162 Chinese angelica Niantong pills need to be taken each time, the taking quantity is large, the patient is troublesome to take and easy to have errors, and the medicine taking compliance of the patient is improved, so that the curative effect is ensured.

The preparation method provided by the invention selects notopterygium root, angelica, radix sileris, rhizoma atractylodis (fried), rhizoma atractylodis macrocephalae (fried), oriental wormwood and radix puerariae, and the seven traditional Chinese medicinal materials are extracted by adopting a supercritical fluid technology, so that the loss of volatile components can be prevented, and the dissolution of fat-soluble components can be improved; the preparation method is characterized in that codonopsis pilosula, scutellaria baicalensis, rhizoma cimicifugae, radix sophorae flavescentis, rhizoma alismatis, rhizoma anemarrhenae, grifola, liquorice and the other eight traditional Chinese medicinal materials are decocted into a medicine, and an optimal extraction process is adopted in combination with screening of extraction times, extraction time and water adding times, so that the purposes of reducing energy consumption, shortening the preparation process time and improving the dissolution efficiency of effective components are achieved under the condition of meeting the preparation requirement.

Detailed Description

The present invention is further described in the following examples, which should not be construed as limiting the scope of the invention, but rather as providing the following examples which are set forth to illustrate and not limit the scope of the invention.

Example 1

A preparation method of a concentrated Chinese angelica Niantong pill comprises the following steps:

(1) weighing the following raw medicinal materials in parts by weight: 40g of angelica, 40g of radix puerariae, 40g of codonopsis pilosula, 40g of rhizoma atractylodis (fried), 40g of rhizoma cimicifugae, 40g of radix sophorae flavescentis, 60g of rhizoma alismatis, 60g of rhizoma atractylodis macrocephalae (fried), 60g of rhizoma anemarrhenae, 60g of radix sileris, 100g of notopterygium root, 100g of scutellaria baicalensis, 100g of grifola, 100g of oriental wormwood and 100g of liquorice;

(2) cleaning and crushing a part A of a raw medicinal material, namely notopterygium root, Chinese angelica, divaricate saposhnikovia root, rhizoma atractylodis (fried), bighead atractylodes rhizome (fried), oriental wormwood and radix puerariae, extracting by using supercritical CO2 fluid, and extracting for 3 hours at constant temperature and pressure under the conditions that the extraction pressure is 25MPa, the extraction temperature is 45 ℃, the resolution pressure is 6MPa, the resolution temperature is 45 ℃ and the CO2 flow rate is 300kg/h to obtain an extract A;

(3) decocting part B of the raw medicinal material, radix Codonopsis, Scutellariae radix, cimicifugae rhizoma, radix Sophorae Flavescentis, Alismatis rhizoma, rhizoma anemarrhenae, Polyporus, and Glycyrrhrizae radix with 12 times of water for two times, each time for 1 hr, filtering decoctions, mixing filtrates, and concentrating to obtain soft extract B with relative density of 1.24;

(4) adding sucrose, silica gel micropowder and starch into the extract A and the thick paste B obtained in the steps (2) and (3) to prepare wet pills, and drying and polishing under the conditions that the steam pressure is 0.50Mpa, the drying temperature is 60 ℃ and the moisture is 6.0 percent to obtain the concentrated Chinese angelica Niantong pills.

Example 2

(2) cleaning and crushing a part A of a raw medicinal material, namely notopterygium root, Chinese angelica, divaricate saposhnikovia root, rhizoma atractylodis (fried), bighead atractylodes rhizome (fried), oriental wormwood and radix puerariae, extracting by using supercritical CO2 fluid, and extracting for 3 hours at constant temperature and pressure under the conditions that the extraction pressure is 20Mpa, the extraction temperature is 45 ℃, the resolution pressure is 7Mpa, the resolution temperature is 48 ℃ and the CO2 flow rate is 320kg/h to obtain an extract A;

(3) decocting part B of the raw medicinal material, radix Codonopsis, Scutellariae radix, cimicifugae rhizoma, radix Sophorae Flavescentis, Alismatis rhizoma, rhizoma anemarrhenae, Polyporus, and Glycyrrhrizae radix with 12 times of water for two times, each time for 1 hr, filtering decoctions, mixing filtrates, and concentrating to obtain soft extract B with relative density of 1.27;

(4) adding sucrose, silica gel micropowder and starch into the extract A and the thick paste B obtained in the steps (2) and (3) to prepare wet pills, and drying and polishing under the conditions that the steam pressure is 0.60Mpa, the drying temperature is 70 ℃ and the moisture is 6.0 percent to obtain the concentrated Chinese angelica Niantong pills.

Example 3

(2) cleaning raw material A, Notopterygii rhizoma, radix Angelicae sinensis, radix Saposhnikoviae, rhizoma Atractylodis (parched), Atractylodis rhizoma (parched), herba Artemisiae Scopariae and radix Puerariae, pulverizing, and extracting with supercritical CO₂Fluid extraction, namely extracting for 3 hours at constant temperature and pressure under the conditions that the extraction pressure is 30MPa, the extraction temperature is 45 ℃, the desorption pressure is 6MPa, the desorption temperature is 42 ℃ and the CO2 flow rate is 280kg/h to obtain an extract A;

(3) decocting part B of the raw medicinal material, radix Codonopsis, Scutellariae radix, cimicifugae rhizoma, radix Sophorae Flavescentis, Alismatis rhizoma, rhizoma anemarrhenae, Polyporus, and Glycyrrhrizae radix with 12 times of water for two times, each time for 1 hr, filtering decoctions, mixing filtrates, and concentrating to obtain soft extract B with relative density of 1.32;

(4) adding sucrose, silica gel micropowder and starch into the extract A and the thick paste B obtained in the steps (2) and (3) to prepare wet pills, and drying and polishing under the conditions that the steam pressure is 0.40Mpa, the drying temperature is 55 ℃ and the moisture is 6.0 percent to obtain the concentrated Chinese angelica Niantong pills.

Example 4

Investigation of extraction Process

The invention researches the Chinese angelica Niantong pill into the concentrated Chinese angelica Niantong pill with simple process and definite curative effect on the basis of the Chinese angelica Niantong pill, reduces the dosage and is beneficial to better serving patients. According to the existing research data of chemistry, pharmacology and the like of the traditional Chinese medicinal materials, the eight traditional Chinese medicines such as the codonopsis pilosula, the scutellaria baicalensis and the like in the prescription are extracted by water and concentrated, and the purpose is to keep the chemical composition of the original prescription, improve the medicine content and reduce the dosage. The invention adopts an orthogonal test method to research the extraction process, so as to comprehensively compare various influencing factors in the extraction process, determine the primary and secondary and interaction of the factors, obtain the optimal collocation of the factors at each level and facilitate the optimal process optimization in production. The process optimization is carried out by adopting orthogonal experimental design, so that on one hand, the time for researching the extraction process can be obviously shortened, and the research cost is reduced; on the other hand, the effective components of the original prescription can be extracted to a greater extent, thereby providing a foundation for fully exerting the clinical curative effect. In addition, in consideration of the factors of keeping volatile components, simplifying process flow and the like, the preparation process of the product selects the other seven medicinal materials of notopterygium root, oriental wormwood and the like to be extracted into the medicine by supercritical fluid. Preliminary experiments show that when the aqueous extract is concentrated to a relative density of about 1.20, it is mixed with the extract to facilitate the formation of pills, including the plasticity of the wet material, the extrusion of strips, and the complete homogeneity of the formed pills. Further prompts the reasonability and feasibility of the water extraction process.

1 Material

Agilent1200 high performance liquid chromatograph;

baicalin reference (China institute for food and drug assay, lot number 110821-201313); acetonitrile is chromatographically pure, water is ultrapure water, and other reagents are analytically pure.

2 methods and results

The research adopts an orthogonal test method, the baicalin content and the water-soluble solid substance content in the scutellaria baicalensis are taken as evaluation indexes, the water adding amount, the extraction time and the extraction frequency influencing the extraction are optimized, and the factor level design is shown in table 1.

TABLE 1 factor level table

Level of	A water addition amount/time	Number of times of extraction	C extraction time/h
				1	8	1	1
2	10	2	1.5
				3	12	3	2

2.1 preparation of samples

Taking 9 parts of medicinal materials, each part of which contains 40g of codonopsis pilosula, 100g of scutellaria baicalensis, 40g of rhizoma cimicifugae, 40g of sophora flavescens, 60g of rhizoma alismatis, 60g of rhizoma anemarrhenae, 100g of polyporus umbellatus and 100g of liquorice, extracting according to a method of orthogonal test arrangement shown in table 1, filtering, combining filtrates, measuring the volume for later use. Respectively measuring the mass of water-soluble solid and the content of baicalin in the extracting solution.

2.2 determination of the amount of Water-soluble solid substance

Precisely measuring 50.00g of each sample solution, measuring according to a drying weight loss measuring method (0831 in the four ministry of communications in the national pharmacopoeia 2015 edition) to obtain a dry extract, and calculating the quality of a water-soluble solid, wherein the formula is as follows:

the mass of water-soluble solid substance/g (the mass of dry extract in 50g of extracting solution/g × extracting solution/g)/50

2.3 method for measuring baicalin

The measurement is carried out by high performance liquid chromatography (0512 in the four-department general regulation of the 2015 edition in China pharmacopoeia).

Chromatographic conditions

Chromatographic Column Symmetry Column C18(4.6 × 250mm, 5 μm), mobile phase of methanol-0.2% phosphoric acid solution (45:55), detection wavelength of 278nm, and theoretical plate number not less than 2500 calculated according to baicalin peak.

Preparation of control solutions: taking appropriate amount of baicalin reference substance, precisely weighing, and adding diluted ethanol to obtain solution containing 60 μ g per lml.

Preparation of a test solution: weighing about 0.8g of the dry extract in 2.2, precisely weighing, placing in a conical flask with a plug, precisely adding 50mL of dilute ethanol, sealing the plug, weighing, performing ultrasonic treatment (power 500W and frequency 40kHz) for 1 hour, cooling, weighing again, supplementing the lost weight with dilute ethanol, filtering with a 0.45-micron microporous membrane, and taking the subsequent filtrate to obtain the final product.

The determination method comprises the following steps: precisely sucking 10 μ L of each of the reference solution and the sample solution, injecting into liquid chromatograph, and measuring.

2.4 data processing and extraction Process optimization

And (3) adopting a comprehensive weighting and scoring method, taking the maximum value of 9 tests of the water-soluble solid matter quantity and the baicalin content as 100, respectively converting the total quantity of each index component into a scoring value, carrying out comprehensive evaluation, and screening the optimal process. The results are shown in tables 2 and 3.

TABLE 2 orthogonal experimental design and results

TABLE 3 analysis of variance of orthogonal test results

Source of variation	SS	f	S	F	P
						A	91.12	2	46.14	3.26	＞0.10
B	1510.00	2	757.00	53.45	＜0.05
						C	60.85	2	29.42	2.08	＞0.10
D	27.33	2	14.16	/	/

F_0.10(2,2)＝99.00，F_0.05(2,2)＝19.00

As can be seen from the visual analysis of the data in the table above, the extraction conditions are preferably A3B2C1 conditions. In order to verify the visual analysis result, the experimental data is subjected to variance analysis, and the variance analysis result shows that: the factor B of the factors to be examined, namely the significant difference of the extraction times on the baicalin content and the water-soluble solid matter measuring amount. The influence level of all factors is integrated, namely extraction times (B) > water adding amount (A) > extraction time (C). From the viewpoint of saving solvent and time, the optimal extraction process is determined as follows: decocting radix Codonopsis, Scutellariae radix, etc. with 12 times of water twice for 1 hr.

2.5 validation test three validation tests were performed, each weighing 40g of radix Codonopsis, 100g of Scutellariae radix, 40g of cimicifugae rhizoma, 40g of radix Sophorae Flavescentis, 60g of Alismatis rhizoma, 60g of rhizoma anemarrhenae, 100g of Polyporus, and 100g of Glycyrrhrizae radix, extracting according to the optimal extraction process conditions of orthogonal test, determining the quality of water-soluble solid and baicalin content in the water extract, and calculating the comprehensive score. The results are shown in Table 4.

TABLE 4 verification of the optimal extraction Process

The results show that the average value of the solid yield of the three parallel tests is 32.50%, the average value of the comprehensive score value is 95.8, and the difference from the maximum value of the comprehensive score of the orthogonal test is not large, which indicates that the screened extraction process conditions are basically stable.

Example 5

Animal pharmacodynamic experiment

1 materials and instruments

1.1 animals

60 healthy SD rats, body weight (180. + -. 20) g, male and female halves.

1.2 arthritis rat model

Fixing the supine position on an anatomical plate, disinfecting the ankle joint of the calf of the right hind limb of the rat conventionally, selecting the outer side of the ankle joint by adopting a puncture point of a No. 6 injection needle, enabling a needle opening to incline upwards and penetrate into an ankle joint cavity at an included angle of 45 degrees with the tibia, injecting 0.2ml of sodium urate solution with the dosage of 250mg/ml, and ensuring that the opposite side of the ankle joint bulges successfully.

1.3 Experimental groups and dosing

Taking 10 normal-fed SD rats as a blank control group; the molded 50 rats were randomly divided into 5 groups, including: the model group comprises high, middle and low dose groups of concentrated Dang Gui Niantong pills, and a control drug group (Dang Gui Niantong pills), wherein each group comprises 10 rats. Each group of rats was gavaged 1 time a day for 7 days

Perfusing the blank control group and the model group with normal saline;

concentrated angelica sinensis Niantong pill: the concentrated Chinese angelica Niantong pill prepared in the embodiment 1 is taken, dissolved by double distilled water and then is perfused into the stomach, and the low dose group is 0.02g/kg, the middle dose group is 0.05g/kg, and the high dose group is 0.08 g/kg;

the contrast medicine group (Chinese angelica Niantong pill): pulverizing NIANTONG pill, dissolving in double distilled water, and intragastric administering at a dose of 0.21 g/kg.

2 method of experiment

1.1 Observation index

The acute inflammatory status of rats was observed at 1 and 7 days of administration, according to the Coderre dysfunction index and inflammatory index evaluation criteria.

Evaluation side

Dysfunction: the left hind foot is completely lifted off the ground, the gait of the three feet is grade 3, the left hind group bends up, the toes are on the back, the lameness is remarkably grade 2, the left hind foot lands and is lightened, the toes are not unfolded, and the lameness is slightly grade 1; the four feet are uniformly landed, and the gait is normally 0 grade;

inflammation index: swelling of limbs around the joint of the left hind paw is grade 3, obvious red swelling appears at the joint part of the left hind paw, the bony sign disappears is grade 2, the joint of the left hind paw is slightly swollen, erythema on the skin is grade 1, and the normal grade is grade 0; meanwhile, the toe swelling degree condition is detected by using a foot volume measuring instrument.

1.2 determination of serum inflammatory factor content

Fixing the rat in a dissecting plate after the last administration, injecting 10% chloral hydrate into abdominal cavity for anesthesia, collecting 5ml of abdominal cavity main venous blood, detecting the content of neutrophilic granulocyte, lymphocyte and leukocyte in serum by a full-automatic biochemical analyzer, placing the residual serum for 1 hour at room temperature, centrifuging by a centrifuge 2500rmp for 15 minutes, and taking supernatant, and detecting the content of NO and uric acid.

1.3 determination of inflammatory factor content in ankle Joint tissue

The method comprises the steps of taking blood, killing a rat quickly, separating soft tissues around an ankle joint quickly, centrifuging, taking supernate, detecting the content of TNF- α, IL-1 β and NO and the content of NO and uric acid in serum by an ELISA method, diluting a standard substance, adding the diluted standard substance into standard substance holes of an ELISA plate, adding a sample into each sample hole, 10 mu L of each sample hole, sealing a reaction hole by adhesive paper, incubating for 2 hours at 37 ℃, washing the plate for five times, adding 10 mu L of biotinylated antibody working solution, incubating for 1 hour at 37 ℃, washing the plate for five times, adding 10 mu L of enzyme conjugate working solution, incubating for 30 minutes in a dark place at 37 ℃, washing the plate for five times, adding 10 mu L of developing solution into each hole, incubating for 20 minutes in a dark place at 37 ℃, finally adding stop solution, detecting an OD450 value after mixing uniformly, taking the concentration of the standard substance as an abscissa, taking the OD value as an ordinate, drawing a standard curve, and checking the concentration of the sample in the standard curve according to the OD.

3 results of the experiment

3.1 the results of swelling, dysfunction and inflammation index of the toes of rats 1 and 7 days after administration are shown in tables 5 and 6 below.

TABLE 5 toe swelling, dysfunction and inflammation index results in rats 1 day after dosing

TABLE 6 toe swelling, dysfunction and inflammation index results in rats 7 days after dosing

Note # indicates P < 0.05 compared to blank control; expression vs model, P < 0.05

As can be seen from Table 5, 1 day after administration, the results of the swelling degree, dysfunction and inflammation index of the toes of the rats were significantly different compared with the blank control group, indicating that the model was successfully made. Compared with the model group, the results of the toe swelling degree, the dysfunction and the inflammation index of the rat are all lower than those of the model group, but the significant difference is not generated.

As can be seen from table 6, no significant difference was observed in the dysfunction of each group 7 days after the administration. Compared with a blank control group, the results of the toe swelling degree and the inflammation index of the rat are reduced and have significant difference. Each administration group to model group ratio: the swelling degree and inflammation index results of the toes of the rats are lower than those of the model group, the low-dose group has no significant difference, and the medium-dose group, the high-dose group and the angelica Niantong pill group have significant difference. The ratio of the concentrated angelica sinensis Niantong pill to the contrast medicine angelica sinensis Niantong pill is as follows: the low dose group is different from the angelica pick pain pill group, the middle dose group is equivalent to the angelica pick pain pill group, and the high dose group is better than the angelica pick pain pill group and has significant difference.

3.2 measurement of inflammatory factors in serum

After 7 days of administration, the rat serum neutrophil, leukocyte, lymphocyte, NO and uric acid contents were determined, and the results are shown in table 7 below.

TABLE 7 determination of inflammatory factors in serum

As can be seen from Table 7, 7 days after administration, the contents of neutrophils, leukocytes, lymphocytes, NO and uric acid in the model group and the blank control group were significantly different, indicating that the molding was successful. Each administration group to model group ratio: the content of neutrophilic granulocyte, lymphocyte and uric acid is reduced, the content of NO is increased, the middle dose group, the high dose group and the Chinese angelica Niantong pill group have significant difference, and the low dose group has NO significant difference; the content of leucocytes is reduced, and the administration groups have significant difference. The ratio of the concentrated angelica sinensis Niantong pill to the contrast medicine angelica sinensis Niantong pill is as follows: the neutral granulocyte, the leucocyte and NO, the medium dose group is equivalent to the Chinese angelica Niantong pill; lymphocytes and uric acid, the high dose group is equivalent to the Dang Gui Niantong pill. The results show that the angelica Niantong pill has obvious regulation effect on anti-inflammatory factors in serum, the effect of a high-dose group in the concentrated angelica Niantong pill is better, and the curative effect of the concentrated angelica Niantong pill is stronger.

3.3 measurement results of inflammatory factors in ankle Joint tissues

The levels of inflammatory factors NO, IL-1 β and TNF- α in rat ankle tissues 7 days after administration are shown in Table 8 below.

TABLE 8 determination of inflammatory factors in ankle tissue

As can be seen from Table 8, the contents of IL-1 β, TNF- α and NO are increased and have significant difference compared with a blank control group 7 days after administration, which indicates that the molding is successful, the contents of IL-1 β, TNF- α and NO are reduced in each administration group and each model group, the contents of IL-1 β, TNF- α and NO are significantly different in a medium dose group, a high dose group and a Chinese angelica Nippon pill group, and the contents of IL-1 β, TNF- α and NO are not significantly different in a low dose group, and the contents of the concentrated Chinese angelica Nippon pill and the control Chinese angelica Nippon pill group are equal to those of the Chinese angelica Nippon pill, and the high dose group is better than the Chinese angelica Nippon pill.

Claims

1. A preparation method of a concentrated Chinese angelica Niantong pill is characterized by comprising the following steps:

2. The preparation method of the concentrated angelica pick up pill according to claim 1, wherein the supercritical CO2 fluid extraction method in the step (2) comprises the following specific steps: the raw medicinal materials after being cleaned and crushed are extracted for 2 to 4 hours at constant temperature and pressure under the conditions of extraction pressure of 20 to 30Mpa, extraction temperature of 40 to 50 ℃, resolution pressure of 6 to 7Mpa, resolution temperature of 40 to 50 ℃ and CO2 flow rate of 250 to 350kg/h, and extract A is obtained.

3. The preparation method of the concentrated Chinese angelica and Niantong pill according to claim 1, wherein the relative density of the thick paste B in the step (3) is 1.20-1.40.

4. The method for preparing the concentrated Dang Gui Niantong pill according to claim 1, wherein the disintegrant in the step (4) is any one of starch, sodium carboxymethyl starch or low-substituted hydroxypropyl cellulose.

5. The method for preparing the concentrated Dang Gui Niantong pill according to claim 1, wherein the drying in the step (4) is performed under the conditions of a steam pressure of 0.40 to 0.60Mpa, a drying temperature of 50 to 80 ℃, and a moisture content of 8.0% or less.

6. A concentrated Dang Gui Niantong pill, characterized in that it is prepared by the preparation method of any one of claims 1 to 5.