CN102688272B - Preparation method for medicine for treating anaemia - Google Patents

Preparation method for medicine for treating anaemia Download PDF

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CN102688272B
CN102688272B CN201210196507XA CN201210196507A CN102688272B CN 102688272 B CN102688272 B CN 102688272B CN 201210196507X A CN201210196507X A CN 201210196507XA CN 201210196507 A CN201210196507 A CN 201210196507A CN 102688272 B CN102688272 B CN 102688272B
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rhizoma atractylodis
melanteritum
medicine
fine powder
vinegar
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CN102688272A (en
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贾茹
韩小平
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Han Xiaoping
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Abstract

The invention discloses a preparation method for a medicine for treating anaemia. The preparation method comprises the following steps of: slicing rhizoma atractylodis, removing fuzz from cartialgenous, processing tortoise shell with vinegar, calcining copperas and performing plain frying on medicated leaven, wherein the weight ratio of the rhizoma atractylodis to the cartialgenous to the tortoise shell to the copperas to the medicated leaven is 6:1:3:5:5. The copperas calcining step comprises the following process flows of: crushing into a fine powder capable of passing through a sieve of 200 meshes; heating for 20 minutes at the temperature of 160 DEG C; heating to 400 DEG C; calcining for 1 hour; quenching with 0.2 time of rice vinegar; calcining for 1 hour at the temperature of 200 DEG C; extracting the rhizoma atractylodis in eight times weight of water; performing reflux for 2 hours at the steam pressure which is not higher than 0.2MPa; filtering a decoction; adding 5 times weight of water to dregs of the decoction and performing reflux for 2 hours and filtering to obtain filtrate; merging the decorations and filtering; concentrating the filtrate under the conditions that the vacuum degree is 0.05-0.08MPa, the temperature is 70-80 DEG C, and the steam pressure is 0.1-0.2MPa to obtain a paste; crushing the cartialgenous, the tortoise shell, the copperas and the medicated leaven and evenly mixing with the paste; and drying, crushing and pelletizing to obtain the medicine for treating the anaemia. According to the preparation method for the medicine for treating the anaemia, the energy consumption is reduced, the extraction efficiency of effective components of the rhizoma atractylodis is increased, and the controllability of the quality of the medicine is ensured.

Description

A kind of preparation method for the treatment of the medicine of anemia
Technical field
The present invention relates to treat the medicine of anemia, particularly relating to a kind of is the preparation method of the Chinese patent medicine of raw material treatment anemia with Chinese medicine.
Background technology
The kind of anemia is a lot, and cause of disease complexity, the traditional Chinese medical science think that the source of blood and generation mainly depend on the function of taste and kidney.The medicine of existing treatment anemia is a lot, but the western medicine anemia exists specific aim single, and the state of an illness be difficult for the shortcoming of radical cure, and the Chinese medicine of existing treatment anemia exists onset slow, the problem that curative effect is low easily repeatedly.
The patent No. 95102249.0, denomination of invention is a kind of Chinese medicine for the treatment of anemia, disclose with Rhizoma Atractylodis, Cornu Cervi Pantotrichum, Carapax et Plastrum Testudinis(processed with vinegar), forged Melanteritum, the stir-fry Massa Medicata Fermentata is raw material, produce capsule according to conventional method, wherein the Rhizoma Atractylodis water extraction is got volatile oil and decocting liquid concentrated extract three times, all the other four Chinese medicines are ground into powder and add extractum and make behind the granule dryly, and it is encapsulated to spray Rhizoma Atractylodis oil then.Prior art has two: 1, with Rhizoma Atractylodis water extraction three times volatile oil and decocting liquid concentrated extract, all the other four Chinese medicines are ground into powder and add extractum and make behind the granule dryly, it is encapsulated to spray Rhizoma Atractylodis oil then; 2, the above five tastes, Rhizoma Atractylodis add 8 times of amounts of water and extracted volatile oil 2 hours, and the aqueous solution after distillation device is in addition collected; Medicinal residues add 5 times of amounts of water, decoct 2 hours, merge distillate and decocting liquid, filter, and it is 1.2~1.25(70 ℃ that filtrate is concentrated into relative density) clear paste, standby; Four flavors such as all the other Massa Medicata Fermentatas are ground into fine powder, add in the clear paste, and it are an amount of to add starch, stirs, and makes granule, and drying is evenly sprayed Rhzoma Atractylodis Lanceae volatile oil in granule, encapsulated (seeing drug standard WS-5528(B-0528)-2002); The production process that relates in the background technology document exists processing step loaded down with trivial details, and technical parameter is indeterminate, the bigger grade of energy consumption problem more or less.And in preparation Chinese medicine process, different because of the difference of processing step and technical parameter, its ingredient of medicine of preparation gained and the drug effect of generation all can have very big difference, that is to say: its quality controllability of Chinese medicine of the treatment anemia of producing according to above production technology is poor, can't effectively guarantee product quality aborning, and then pharmaceutical effectiveness can not get guaranteeing.Imitate and can not get guaranteeing.
Summary of the invention
The purpose of this invention is to provide a kind of is the preparation method of the Chinese patent medicine of raw material treatment anemia with Chinese medicine.
The present invention is achieved by the following technical solutions:
A kind of preparation method for the treatment of the medicine of anemia may further comprise the steps:
(1) medical material pre-treatment: with Rhizoma Atractylodis sections, Cornu Cervi Pantotrichum unhairing, Carapax Et Plastrum Testudinis vinegar system, the Melanteritum calcine, Massa Medicata Fermentata is fried, and the Rhizoma Atractylodis of wherein cutting into slices, unhairing Cornu Cervi Pantotrichum, Carapax et Plastrum Testudinis(processed with vinegar), calcine Melanteritum, the weight ratio of frying Massa Medicata Fermentata are 6:1:3:5:5; Wherein, Melanteritum calcine step is: clean Melanteritum is ground into the fine powder that can cross 200 mesh sieves, fine powder is warming up to 400 ℃ in heating under 160 ℃ of temperature after 20 minutes again, calcined 1 hour, with the refining of quenching while hot of the rice vinegar of 0.2 times of Melanteritum weight, then 200 ℃ of calcinings 1 hour down, cool and get final product;
(2) water extraction: get Rhizoma Atractylodis with 8 times of weight floodings after 1 hour under the condition of steam pressure≤0.2Mpa reflux, extract, 2 hours, collect volatile oil, filter decocting liquid, medicinal residues are added 5 times of weight water, 2 hours after-filtration of reflux, extract, get decocting liquid again, twice decocting liquid merged after-filtration, filtrate is 0.05~0.08Mpa in vacuum, temperature is 70~80 ℃, and steam pressure is to carry out vacuum decompression with spherical concentration tank under the condition of 0.1~0.2Mpa to be concentrated into 70 ℃ time relative density be that 1.2~1.25 Rhizoma Atractylodis clear paste is standby;
(3) pulverize: will be through unhairing Cornu Cervi Pantotrichum, Carapax et Plastrum Testudinis(processed with vinegar), the calcine Melanteritum of step (1) pre-treatment, fry Massa Medicata Fermentata and mix, be ground into the fine powder that can cross 100 mesh sieves, it is even that the fine powder range estimation does not have caking, no foreign body, color and luster;
(4) granulation is encapsulated: step (3) gained fine powder is added in the Rhizoma Atractylodis clear paste of step (2) gained; behind the mix homogeneously; drying and crushing is made granule; granulation order number is 20 orders; granule carries out granulate with pelletizing machine; granulate order number is 20 orders, evenly sprays Rhzoma Atractylodis Lanceae volatile oil and mix with granule in three-dimensional motion mixer, and the granule that mixes is encapsulated by the specification of 0.3g/ grain.
Preparation method of the present invention has been improved the Melanteritum technology for calcining, improve effective ingredient---the activity of ferrous iron (Fe2+) in human body of iron supplement in the preparation, and solubility strengthens, and has improved to the present invention relates to the curative effect of preparation aspect the low diseases of bone marrow hematogenesis such as treatment iron deficiency anemia, aplastic anemia; The process conditions that the present invention carries by accurate control Rhizoma Atractylodis water, and then improve extraction ratio, the quality of strict control medicine improves curative effect.
For a better understanding of the present invention, below by the further raising of the quality controllable and curative effect of the medicine of elaboration preparation method system of the present invention of test example.
1, get 3 batch samples that this law makes and carry out the quality standard check, assay is as follows:
Figure 955883DEST_PATH_IMAGE001
2, get the sample that this law makes and treat the iron deficiency anemia clinical evaluation, process and result are as follows:
(1) case standard:
Include standard in---meet the diagnosis of doctor trained in Western medicine iron deficiency anemia; Meeting Chinese medical discrimination is the syndrome of yang deficiency of spleen and kidney patient; Age is at 18-70 between year; Tried voluntarily and the person that signs the Informed Consent Form.
Exclusion standard---merge serious primary disease such as liver (1.5 times of liver function>normal values), kidney, hemopoietic system, the psychotic; Gestation or preparation gestation, women breast-feeding their children; To this medicine composition allergy sufferers and serious allergic constitution person; Participate in the patient of other clinical medicine tests in nearly 3 months.
(2) test method
This test is followed at random, double blinding, parallel control, multiple center clinical study method, the capsule of selecting method for making of the present invention to make is trial drug, 95102249.0 patent of invention in the capsule that makes of the preparation process that provides be control drug 1, drug standard WS-5528(B-0528)-the 2002[method for making] capsule that makes is control drug 2.
(3) observation index
Demography data---name, sex, age, occupation, nationality, body weight, height, marriage situation (record once before the treatment).
Safety observation---symptom, sign that vital sign (temperature pulse respiration, blood pressure, heart rate), routine blood test, routine urinalysis, stool routine examination+occult blood laboratory examination, Electrocardioscopy, liver function (ALT, AST, TBIL, DBIL), renal function (BUN, Cr) inspection, adverse events, untoward reaction occur are observed.
Health giving quality observation---1) serum ferritin, serum levels of iron, transferrins, total iron binding capacity; 2) tcm syndrome curative effect; 3) variation of traditional Chinese medical science related symptoms, picture of the tongue and pulse condition.
(4) observation time point
Relevant S﹠S: record before the medication and after the medication.
Safety indexes observation: each does once (should check in 1 week in 1 week and after the drug withdrawal, and answer the appearance of close observation untoward reaction, and carry out record) before and after the treatment before medication.
(5) efficacy assessment standard
Standard formulation with reference to " new Chinese medicine clinical research guideline " " new Chinese medicine treatment iron deficiency anemia clinical research guideline ".
Total mark before therapeutic index (n)=treatment-treatment back total mark * 100%
Total mark before the treatment
Clinical recovery: therapeutic index (integrated value reduction) 〉=90%.
Produce effects: therapeutic index (integrated value reduction) 〉=70%,<90%.
Effectively: therapeutic index (integrated value reduction) 〉=30%,<70%.
Invalid: therapeutic index (integrated value reduction)<30%.
(6) result
According to case inclusion criteria and the exclusion standard in the clinical trial protocol, have 180 routine subject enrollments and enter this test, test group is 60 examples, and matched group 1 is 60 examples, and matched group 2 is 60 examples.The data blind review determines after all 4 weeks of case treatment: data of safety collection (SS) 180 examples, and wherein test group is 60 examples, and matched group 1 is 60 examples, and matched group 2 is 60 examples; Complete analysis collection (FAS) 180 examples, wherein test group is 60 examples, and matched group 1 is 60 examples, and matched group 2 is 60 examples; Meet scheme collection (PPS) 180 examples 24 weeks, wherein test group is 60 examples, and matched group 1 is 60 examples, and matched group 2 is 60 examples.
Demographic characteristics: average 33.88 years old of 1 age of matched group before the treatment, male's 25 examples, women's 35 examples, the average 168.5cm of height, weight average 63.66kg; Average 34.38 years old of 2 ages of matched group, male's 26 examples, women's 34 examples, the average 168.7cm of height, weight average 65.36kg; Average 35.56 years old of test group age, male's 28 examples, women's 32 examples, the average 169.52cm of height, weight average 66.28kg; The equal not statistically significants of data set differences such as age, sex, height, body weight, nationality, occupation, marital status between test group and matched group (P〉0.05), have comparability.
Three groups of medical histories, the course of disease, state of an illness classification, primary disease treatment history, drug allergy histories and merge the equal not statistically significant of disease group differences (P〉0.05) have comparability.
Vital sign: matched group 1 is breathed the average 118.11mmHg of systolic pressure, the average 74.85mmHg of diastolic pressure, average 36.51 ℃ of body temperature average 18.66 times before the treatment; Matched group 2 is breathed the average 117.91mmHg of systolic pressure, the average 75.14mmHg of diastolic pressure, average 36.47 ℃ of body temperature average 18.54 times; Test group is breathed average 18.39 times, the average 119.41mmHg of systolic pressure, the average 74.76mmHg of diastolic pressure, average 36.49 ℃ of body temperature;Blood pressure between matched group and test group in the vital sign, breathing, heart rate,, the equal not statistically significant of body temperature group difference (P〉0.05), have comparability.
Effectiveness is observed:
Serum ferritin: after treating for 4 weeks, effective percentage matched group 1 is 44.07%, and matched group 2 is 44.67%, and test group is 64.82%; Through rank test, matched group and test group treatment 4 all backs group differences have statistical significance (P<0.05).
Serum levels of iron: after treating for 4 weeks, effective percentage matched group 1 is 42.16%, and matched group 2 is 41.98%, and test group is 58.5%; Through rank test, matched group and test group treatment 4 all backs group differences have statistical significance (P<0.05).
Transferrins: after treating for 4 weeks, effective percentage matched group 1 is 43.92%, and matched group 2 is 44.07%, and test group is 59.00%; Through rank test, matched group and test group treatment 4 all backs group differences have statistical significance (P<0.05).
Total iron binding capacity: after treating for 4 weeks, effective percentage matched group 1 is 45.78%, and matched group 2 is 46.27%, and test group is 65.14%; Through rank test, matched group and test group treatment 4 all backs group differences have statistical significance (P<0.05).
The tcm syndrome curative effect: after treating for 4 weeks, cure-remarkable-effectiveness rate matched group 1 is 44.44%, and matched group 2 is 46.35%, and test group is 64.86%; Total effective rate matched group 1 is 65.63%, and matched group 2 is 69.35%, and test group is 84.79%; Through rank test, matched group and test group treatment 4 all back cure-remarkable-effectiveness rates and total effective rate group difference have statistical significance (P<0.05).
Safety is observed:
Matched group and test group all do not have bad event and take place.
Medicine of the present invention is formed with natural Chinese medicines, has no side effect, and preparation method has reduced power consumption; Improve the extraction effect of Rhizoma Atractylodis effective ingredient, guaranteed to produce the quality controllable of medicine; Improved the curative effect of the low disease of bone marrow hematogenesis aspects such as treatment iron deficiency anemia, aplastic anemia.
The specific embodiment
Embodiment 1
A kind of preparation method for the treatment of the medicine of anemia may further comprise the steps:
(1) medical material pre-treatment: take by weighing the section of 6.3kg Rhizoma Atractylodis, unhairing Cornu Cervi Pantotrichum 1.05kg, Carapax et Plastrum Testudinis(processed with vinegar) 3.15kg, calcine Melanteritum 5.25kg fries Massa Medicata Fermentata 5.25kg;
Wherein, Melanteritum calcine step is: clean Melanteritum is ground into the fine powder that can cross 200 mesh sieves, fine powder is warming up to 400 ℃ in heating under 160 ℃ of temperature after 20 minutes again, calcined 1 hour, with the refining of quenching while hot of the rice vinegar of 0.2 times of Melanteritum weight, then 200 ℃ of calcinings 1 hour down;
(2) water extraction: get Rhizoma Atractylodis sections with the purified water lixiviate of 50.4kg after 1 hour under the condition of steam pressure 0.2Mpa reflux, extract, 2 hours, collect volatile oil, filter decocting liquid device collection in addition, medicinal residues are added 31.5kg water, 2 hours after-filtration of reflux, extract, get decocting liquid again, twice decocting liquid merged after-filtration get filtrate 79.9kg, filtrate is 0.06Mpa in vacuum, temperature is 72 ℃, steam pressure is to carry out vacuum decompression with spherical concentration tank under the condition of 0.1Mpa to be concentrated into 70 ℃ time relative density be that 1.2~1.25 Rhizoma Atractylodis clear paste is standby, amounts to 3.1kg;
(3) pulverize: will be through unhairing Cornu Cervi Pantotrichum, Carapax et Plastrum Testudinis(processed with vinegar), the calcine Melanteritum of step (1) pre-treatment, fry Massa Medicata Fermentata and mix, be ground into the fine powder that can cross 100 mesh sieves, it is even that the fine powder range estimation does not have caking, no foreign body, color and luster;
(4) granulation is encapsulated: step (3) gained fine powder 14.62kg is added among the Rhizoma Atractylodis clear paste 3.1kg of step (2) gained; after closing evenly; drying and crushing is made granule; granulation order number is 20 orders; granule carries out granulate with pelletizing machine; granulate order number is 20 orders, evenly sprays Rhzoma Atractylodis Lanceae volatile oil 0.2kg and mix with granule in three-dimensional motion mixer, and the granule 16.87kg that mixes is encapsulated 70,000 by the specification of 0.3g/ grain.
Embodiment 2
A kind of preparation method for the treatment of the medicine of anemia may further comprise the steps:
(1) medical material pre-treatment: with Rhizoma Atractylodis sections, Cornu Cervi Pantotrichum unhairing, Carapax Et Plastrum Testudinis vinegar system, the Melanteritum calcine, Massa Medicata Fermentata is fried, and the Rhizoma Atractylodis of wherein cutting into slices, unhairing Cornu Cervi Pantotrichum, Carapax et Plastrum Testudinis(processed with vinegar), calcine Melanteritum, the weight ratio of frying Massa Medicata Fermentata are 6:1:3:5:5; Wherein, Melanteritum calcine step is: clean Melanteritum is ground into the fine powder that can cross 200 mesh sieves, fine powder is warming up to 400 ℃ in heating under 160 ℃ of temperature after 20 minutes again, calcined 1 hour, with the refining of quenching while hot of the rice vinegar of 0.2 times of Melanteritum weight, then 200 ℃ of calcinings 1 hour down, cool and get final product;
(2) water extraction: get Rhizoma Atractylodis with 8 times of weight floodings after 1 hour under the condition of steam pressure 0.18Mpa reflux, extract, 2 hours, collect volatile oil, filter decocting liquid, medicinal residues are added 5 times of weight water, 2 hours after-filtration of reflux, extract, get decocting liquid again, twice decocting liquid merged after-filtration, filtrate is 0.05Mpa in vacuum, temperature is 80 ℃, and steam pressure is to carry out vacuum decompression with spherical concentration tank under the condition of 0.15Mpa to be concentrated into 70 ℃ time relative density be that 1.2~1.25 Rhizoma Atractylodis clear paste is standby;
(3) pulverize: will be through unhairing Cornu Cervi Pantotrichum, Carapax et Plastrum Testudinis(processed with vinegar), the calcine Melanteritum of step (1) pre-treatment, fry Massa Medicata Fermentata and mix, be ground into the fine powder that can cross 100 mesh sieves, it is even that the fine powder range estimation does not have caking, no foreign body, color and luster;
(4) granulation is encapsulated: step (3) gained fine powder is added in the Rhizoma Atractylodis clear paste of step (2) gained; behind the mix homogeneously; drying and crushing is made granule; granulation order number is 20 orders; granule carries out granulate with pelletizing machine; granulate order number is 20 orders, evenly sprays Rhzoma Atractylodis Lanceae volatile oil and mix with granule in three-dimensional motion mixer, and the granule that mixes is encapsulated by the specification of 0.3g/ grain.
Embodiment 3
A kind of preparation method for the treatment of the medicine of anemia may further comprise the steps:
(1) medical material pre-treatment: with Rhizoma Atractylodis sections, Cornu Cervi Pantotrichum unhairing, Carapax Et Plastrum Testudinis vinegar system, the Melanteritum calcine, Massa Medicata Fermentata is fried, and the Rhizoma Atractylodis of wherein cutting into slices, unhairing Cornu Cervi Pantotrichum, Carapax et Plastrum Testudinis(processed with vinegar), calcine Melanteritum, the weight ratio of frying Massa Medicata Fermentata are 6:1:3:5:5; Wherein, Melanteritum calcine step is: clean Melanteritum is ground into the fine powder that can cross 200 mesh sieves, fine powder is warming up to 400 ℃ in heating under 160 ℃ of temperature after 20 minutes again, calcined 1 hour, with the refining of quenching while hot of the rice vinegar of 0.2 times of Melanteritum weight, then 200 ℃ of calcinings 1 hour down, cool and get final product;
(2) water extraction: get Rhizoma Atractylodis with 8 times of weight floodings after 1 hour under the condition of steam pressure 0.17Mpa reflux, extract, 2 hours, collect volatile oil, filter decocting liquid, medicinal residues are added 5 times of weight water, 2 hours after-filtration of reflux, extract, get decocting liquid again, and twice decocting liquid merged after-filtration, and filtrate is 0.08Mpa in vacuum, temperature is 70 ℃, and steam pressure is to carry out vacuum decompression with spherical concentration tank under the condition of 0.2Mpa to be concentrated into 70 ℃ time relative density be that 1.2~1.25 Rhizoma Atractylodis clear paste is standby;
(3) pulverize: will be through unhairing Cornu Cervi Pantotrichum, Carapax et Plastrum Testudinis(processed with vinegar), the calcine Melanteritum of step (1) pre-treatment, fry Massa Medicata Fermentata and mix, be ground into the fine powder that can cross 100 mesh sieves, it is even that the fine powder range estimation does not have caking, no foreign body, color and luster;
(4) granulation is encapsulated: step (3) gained fine powder is added in the Rhizoma Atractylodis clear paste of step (2) gained; behind the mix homogeneously; drying and crushing is made granule; granulation order number is 20 orders; granule carries out granulate with pelletizing machine; granulate order number is 20 orders, evenly sprays Rhzoma Atractylodis Lanceae volatile oil and mix with granule in three-dimensional motion mixer, and the granule that mixes is encapsulated by the specification of 0.3g/ grain.

Claims (1)

1. preparation method for the treatment of the medicine of anemia is characterized in that may further comprise the steps:
(1) medical material pre-treatment: with Rhizoma Atractylodis sections, Cornu Cervi Pantotrichum unhairing, Carapax Et Plastrum Testudinis vinegar system, the Melanteritum calcine, Massa Medicata Fermentata is fried, and the Rhizoma Atractylodis of wherein cutting into slices, unhairing Cornu Cervi Pantotrichum, Carapax et Plastrum Testudinis(processed with vinegar), calcine Melanteritum, the weight ratio of frying Massa Medicata Fermentata are 6:1:3:5:5;
Wherein, Melanteritum calcine step is: clean Melanteritum is ground into the fine powder that can cross 200 mesh sieves, fine powder is warming up to 400 ℃ in heating under 160 ℃ of temperature after 20 minutes again, calcined 1 hour, with the refining of quenching while hot of the rice vinegar of 0.2 times of Melanteritum weight, then 200 ℃ of calcinings 1 hour down, cool and get final product;
(2) water extraction: get Rhizoma Atractylodis with 8 times of weight floodings after 1 hour under the condition of steam pressure≤0.2Mpa reflux, extract, 2 hours, collect volatile oil, filter decocting liquid, medicinal residues are added 5 times of weight water, 2 hours after-filtration of reflux, extract, get decocting liquid again, twice decocting liquid merged after-filtration, filtrate is 0.05~0.08Mpa in vacuum, temperature is 70~80 ℃, and steam pressure is to carry out vacuum decompression with spherical concentration tank under the condition of 0.1~0.2Mpa to be concentrated into 70 ℃ time relative density be that 1.2~1.25 Rhizoma Atractylodis clear paste is standby;
(3) pulverize: will be through unhairing Cornu Cervi Pantotrichum, Carapax et Plastrum Testudinis(processed with vinegar), the calcine Melanteritum of step (1) pre-treatment, fry Massa Medicata Fermentata and mix, be ground into the fine powder that can cross 100 mesh sieves, it is even that the fine powder range estimation does not have caking, no foreign body, color and luster;
(4) granulation is encapsulated: step (3) gained fine powder is added in the Rhizoma Atractylodis clear paste of step (2) gained; behind the mix homogeneously; drying and crushing is made granule; granulation order number is 20 orders; granule carries out granulate with pelletizing machine; granulate order number is 20 orders, evenly sprays Rhzoma Atractylodis Lanceae volatile oil and mix with granule in three-dimensional motion mixer, and the granule that mixes is encapsulated by the specification of 0.3g/ grain.
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