CN104306658B - A kind of preparation method of Tongxiening granule - Google Patents

A kind of preparation method of Tongxiening granule Download PDF

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CN104306658B
CN104306658B CN201410610179.2A CN201410610179A CN104306658B CN 104306658 B CN104306658 B CN 104306658B CN 201410610179 A CN201410610179 A CN 201410610179A CN 104306658 B CN104306658 B CN 104306658B
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dextrin
medicinal liquid
temperature
volatile oil
granule
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CN104306658A (en
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陈烈春
王道权
刘小英
黄介
刘伟
周邦建
侯媛芳
沈浩
张壹
王茂
杨晓宏
石锦萍
刘明洁
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CHONGQING HUASEN PHARMACEUTICAL Co Ltd
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CHONGQING HUASEN PHARMACEUTICAL Co Ltd
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Abstract

The preparation method that the invention discloses a kind of Tongxiening granule, this includes the Radix Paeoniae Alba, Pericarpium Citri Reticulatae Viride, Bulbus Allii Macrostemonis, the Rhizoma Atractylodis Macrocephalae being respectively adopted water extraction and obtaining medicinal liquid and volatile oil, medicinal liquid and dextrin are mixed with extractum, volatile oil beta-schardinger dextrin-makes embedded object, then with dextrin and protein sugar mixing granulation, i.e. Tongxiening granule, this method is safe and environment-friendly, the content of paeoniflorin of the granule prepared is high, good effect.

Description

A kind of preparation method of Tongxiening granule
Technical field
The present invention relates to technical field of Chinese patent medicine, the preparation method being specifically related to a kind of Tongxiening granule.
Background technology
Irritable bowel syndrome is within nearly 10 years, just to obtain the common high incidence disease that medical circle is generally acknowledged, although to life without threat, but it is to cause that patient is painful, causes absence from duty, affects the main cause of work. It is also the disease that misdiagnosis rate is high, so that patient disorderly seeks medical advice and haphazardly medicates, particularly prolonged and repeated takes antibiotics, not only causes great financial burden and the health of serious harm patient. Owing to etiology and pathogenesis is failed to understand, current doctor trained in Western medicine is based on symptomatic treatment, and such as relieving spasm to stop pain atropine or nifedipine etc., antidiarrheal Compound Diphenoxylate, dioctahedral smectite etc., curative effect is all unsatisfactory. And the traditional Chinese medical science has the record exactly liking its symptom more in ancient books, the Ming Dynasty is initial is called that pain is rushed down, and common pattern of syndrome is hyperactive liver-QI attacking the spleen, has confirmed this disease of the doctor trained in Western medicine argument without racial difference. Though differential diagnosis in tcm opinion controls good therapeutic effect, but does not form the new drug preparation carrying taking convenience, effective and safe, it is impossible to deal with the unexpected recurrent exerbation of this disease.
New drug Tongxiening granule is clinically used for treatment abdominal pain diarrhea type irritable bowel syndrome (IBS), and raw material and percentage by weight be: the Radix Paeoniae Alba 17%~36%, the Rhizoma Atractylodis Macrocephalae 12%~27%, Pericarpium Citri Reticulatae Viride 18%~33%, Bulbus Allii Macrostemonis 15%~24%. The Radix Paeoniae Alba in component is the Main Ingredients and Appearance of the present invention, because the Radix Paeoniae Alba contains paeoniflorin, there is good spasmolysis, guinea pig in vitro small intestinal there is suppression Spontaneous Contraction, reducing the effect of tonicity, the intestinal contraction that acetylcholine is caused is without obvious effect, but can suppress the intestinal contraction that barium chloride causes, therefore, it was initially believed that the spasmolysis of the Radix Paeoniae Alba is that it directly acts on the result of intestinal tube smooth muscle. The Rhizoma Atractylodis Macrocephalae in component contains atractylol, atractylone etc., may be up to 1.32% containing volatile oil. The Rhizoma Atractylodis Macrocephalae has the wet effect adjusted just of spleen invigorating fortune, and gastrointestinal function impact is shown dual regulation. Pericarpium Citri Reticulatae Viride in component contains volatile oil, Pericarpium Citri Reticulatae glycosides etc., and composition is roughly the same with Pericarpium Citri Reticulatae, and report Main Ingredients and Appearance is Pericarpium Citri Reticulatae Viride crystalline substance I in recent years, i.e. left-handed oxedrine acetate, content is 0.22g/kg. Having the function of soothing the liver relieving distension by promoting circulation of QI, effect and atropine effect to smooth muscle are similar. Bulbus Allii Macrostemonis in component mainly contains volatile oil, additionally, still containing steroidal saponin etc. 21 kinds of Main Ingredients and Appearances such as dimethyltrisulfide are detected. Circulation of qi promoting is not well specially to control under anus weight, defecation.
In Tongxiening granule side, the Radix Paeoniae Alba is easing the affected liver to relieve pain, for one of principal agent in side, and contained peoniflorin is attached most importance to and is wanted active ingredient in the Radix Paeoniae Alba, therefore in this product national drug registered standard assay item detection composition be defined as peoniflorin, national standard (standard No. :) specify: " every bag (5g) containing the Radix Paeoniae Alba with paeoniflorin (C23H28O11) meter, must not less than 32mg ".Therefore this quality quality of peoniflorin extraction ratio height direct relation.
CN02110973 discloses a kind of method of glycoside compound monomer and extraction and separation in Radix Paeoniae. Glycoside compound monomer in described Radix Paeoniae, calls medicine glycoside monomer and hydroxypaeoniflorin monomer together including paeoniflorin monomer, Albiflorin monomer, benzoyl, and wherein paeoniflorin content of monomer more than 90% meets the purity requirement of a class plant new drug. The party's genealogy of law by the Radix Paeoniae Alba or Radix Paeoniae Rubra in alcohol-water solution swelling, be heated to reflux, be concentrated into extractum, use acetone soln supersound extraction, concentration, admix rubber powder, be condensed into dry sample, upper vacuum chromatographic column, eluting, obtain first product. The method is mainly used in the extraction of benzene Radix Paeoniae single component formyl paeoniflorin, lactone glycoside (albiflorin) and hydroxypaeoniflorin (oxypaeoniflorin).
CN200910131650 discloses the extracting method of the Radix Paeoniae Alba extract for treating diabetes, is pulverized by the Radix Paeoniae Alba, carries out supersound extraction after soaking with ethanol-water solution; After being extracted with ethyl acetate, remove solvent and obtain Radix Paeoniae Alba extract.
CN201010500118 discloses a kind of method extracting peoniflorin from the Radix Paeoniae Alba, process is: white Peony Root is pulverized, acid alcohol or ketone solution extract supersound extraction, concentrated solution adds polar macroporous resin absorption, 40-70% acidic ethanol eluting, and eluent reclaims ethanol and adds non-polar macroporous resin absorption, 30-50% methanol-eluted fractions, eluent, then through acidic alumina short column, adds ethyl acetate n-butyl alcohol mixed solution and extracts 3-5 time after concentration, vacuum drying obtains product. The method extract paeoniflorin there is significant analgesia, calmness, anticonvulsant action, also can coronary artery dilator, increase coronary flow, resist acute myocardial ischemia, the effect of reducing blood pressure.
The extracting method of above-mentioned three kinds of paeoniflorins is all adopt ethanol or other organic solvent to extract, and separated by resin absorption, obtain the paeoniflorin of high-purity degree or single composition, owing to extracting method is different, these component contents are also different, and its activity also has bigger difference, if any treatment diabetes, some treatments analgesia, calm, anticonvulsant action, also can coronary artery dilator, increase coronary flow effect.
A kind of extracting method of research is simple and environmental protection, the method that can guarantee that again peoniflorin high-load, for improving and ensureing that Tongxiening granule clinical efficacy is to be of great importance very much, completes the present invention for this.
Summary of the invention
The preparation method that it is an object of the invention to a kind of Tongxiening granule, the method can improve content and the quality of peoniflorin in Tongxiening granule, it is ensured that Tongxiening granule quality and clinical efficacy, and meanwhile, extraction process is simple and environmentally-friendly.
For realizing the purpose of the present invention, it is provided that following embodiment:
In one embodiment, the preparation method of a kind of Tongxiening granule of the present invention, wherein, the weight ratio of the raw material of Chinese medicine of described granule is the Radix Paeoniae Alba: Pericarpium Citri Reticulatae Viride: Bulbus Allii Macrostemonis: the Rhizoma Atractylodis Macrocephalae=1.6:1.6:1:1, and the method comprises the following steps:
1) in supersound extraction tank, add 8-15 times amount, it is preferable that the water of 10 times amount, ebuillition of heated, add radix paeoniae alba decoction pieces, soak 1-2 hour, then be warmed up to 48~52 DEG C, supersound extraction 2 times, preferably 45 minutes 0.5-1 hour each extraction time, centrifugation medicinal liquid and medicinal residues, medicinal residues are standby
2) medical filtration, filtrate triple effect concentrates, and stops concentration when the proportion of 50 DEG C of concentrated solutions is 1.1~1.15, filters, filtrate sterilizing;
3) taking the Pericarpium Citri Reticulatae Viride of recipe quantity, Bulbus Allii Macrostemonis and the Rhizoma Atractylodis Macrocephalae and add the water of 8 times amount, mixing is soaked, is added thermal distillation, collects volatile oil, after, isolated by filtration medicinal liquid and medicinal residues;
4) step 1) and 2) medicinal residues merge, and add the water of 6-12 times amount, heating, to boiling, is extracted 1-2 hour, is extracted 2 times, filtration, medicinal liquid and step 3) medicinal liquid merge;
5) by 4) merging medicinal liquid, adopt triple effect concentration, steam pressure not can exceed that 0.09MPa, stop concentration when the proportion of 50 DEG C of concentrated solutions is 1.1~1.15, stands, centrifugation extracting solution, filters, obtains filtrate;
6) by step 5) concentrated filtrate and step 2) sterilizing filtrate merge, add dextrin, dissolve mix homogeneously, spray drying, prepare extract powder;
7) adding in purified water by beta-schardinger dextrin-, be heated to 85~90 DEG C, stirring is completely dissolved, and is slowly added to step 3) volatile oil, add volatile oil and be incubated 0.5-1.5 hour, then crystallisation by cooling, filter, dry, prepare beta-cyclo dextrin included compound;
8) granulate: extract powder, dextrin, beta-cyclo dextrin included compound, protein sugar are mixed at multidirectional mixer, arrange, cross 10 orders and 60 orders respectively, collect granule less than 10 orders more than the conforming particle between 60 orders, will be greater than 10 order granule reformation grains, filter out conforming particle again, mix conforming particle, be distributed into bag.
In the above-described embodiment, process of the present invention it is preferred that ground, step 1) in, the consumption of water is preferably the water (times of weight) of radix paeoniae alba decoction pieces 10 times amount, and radix paeoniae alba decoction pieces is soaked 1 hour, preferably 45 minutes each supersound extraction time; Step 2) in triple effect concentration, one effect temperature less than 90 DEG C, vacuum be-0.02~-0.05Mpa, two imitate temperature be 80 ± 2 DEG C, vacuum is-0.03~-0.06Mpa, and triple effect temperature is 70 ± 2 DEG C, and vacuum is-0.04~-0.08Mpa; Step 3) in, distillation Stress control is at 0.05~0.08Mpa, and vapo(u)rizing temperature is more than 110 DEG C, and distillation time is 5 hours, and medicinal liquid is filtered by 100 order filters; Step 4) in the consumption of water be 10 times amount of medicinal residues, start timing when boiling temperature reaches 98 DEG C, extract 1.5h, when temperature reaches 98~100 DEG C, keep fluidized state, extract 1.5h, extracting solution crosses 100 order filters, medicinal liquid and step 3) medicinal liquid merge; Step 4) in, described triple effect concentrates, and steam pressure not can exceed that 0.09MPa, an effect temperature control at 80~95 DEG C, and two effect temperature control at 70~80 DEG C, and triple effect temperature controls at 60~70 DEG C, stop concentration when the concentration proportion of 50 DEG C is 1.1~1.15; Step 6) in, the weight ratio of filtrate (medicinal liquid) and dextrin is 1:0.1-0.15; Step 7) in, the solution temperature of beta-schardinger dextrin-is 85~90 DEG C; Volatile oil: beta-schardinger dextrin-: the weight ratio of purified water is 1:8:60; Adding the temperature retention time after volatile oil is 1 hour, and described crystallisation by cooling cools to 0~10 DEG C, and is incubated more than 24 hours, crystallize, and described dry, baking temperature is 40 DEG C.
In the above-described embodiment, the method for the present invention, step 8) in, the weight ratio of extract powder, dextrin, beta-cyclo dextrin included compound and protein sugar is 1:1.2-1.5:0.1-0.15:0.07-0.08.
In a preferred embodiment, the preparation method of a kind of Tongxiening granule of the present invention, the weight ratio of the raw material of Chinese medicine of described granule is the Radix Paeoniae Alba: Pericarpium Citri Reticulatae Viride: Bulbus Allii Macrostemonis: the Rhizoma Atractylodis Macrocephalae=1.6:1.6:1:1, and the method comprises the following steps:
1) in supersound extraction tank, add the water of 10 times amount, ebuillition of heated, add radix paeoniae alba decoction pieces, soak 1 hour, then be warmed up to 48~52 DEG C, supersound extraction 2 times, 45 minutes each extraction times, centrifugation medicinal liquid and medicinal residues, medicinal residues are standby;
2) filtrate triple effect concentration, stops concentration, filters, filtrate sterilizing when the proportion of 50 DEG C of concentrated solutions is 1.1~1.15;
3) taking the Pericarpium Citri Reticulatae Viride of recipe quantity, Bulbus Allii Macrostemonis and the Rhizoma Atractylodis Macrocephalae and add the water of 8 times amount, mixing immersion, Stress control are at 0.05~0.08Mpa, and temperature rises to more than 110 DEG C, distill 5 hours, collect volatile oil, after volatile oil is drawn, by medicinal liquid by 100 order filters, separating medicinal liquid, medicinal residues are standby;
4) by step 1) and 2) medicinal residues merging, add the water extraction of 10 times amount, when in tank, temperature starts timing when reaching 98 DEG C (boiling), extract 1.5h, when temperature reaches 98~100 DEG C, keep fluidized state, extract 1.5h, cross 100 order filters, medicinal liquid and step 3) medicinal liquid merge;
5) by step 4) merging medicinal liquid adopt triple effect concentration, steam pressure not can exceed that 0.09MPa, stop concentration when the proportion of 50 DEG C of concentrated solutions is 1.1~1.15, stands, centrifugation extracting solution, filters, obtains filtrate;
6) by step 5) concentrated filtrate and step 2) filtrate merge, add dextrin, dissolve mix homogeneously, spray drying, prepare extract powder, wherein, the weight ratio of filtrate and dextrin is 1:0.1-0.15;
7) adding in purified water by beta-schardinger dextrin-, be heated to 85~90 DEG C, stirring is completely dissolved, continue 85~90 DEG C of conditions, be slowly added to step 2) volatile oil, add volatile oil be incubated 1 hour, be then cooled to 0~10 DEG C, and it is incubated more than 24 hours, crystallize, drying crystalline under 40 DEG C of conditions, prepare beta-cyclo dextrin included compound, wherein, volatile oil: beta-schardinger dextrin-: the weight ratio of purified water is 1:8:60;
8) granulate: extract powder, dextrin, beta-cyclo dextrin included compound, protein sugar are pressed the weight ratio mixing granulation of 1:1.2-1.5:0.1-0.15:0.07-0.08, granulate, cross 10 orders and 60 orders respectively, collect granule less than 10 orders more than the conforming particle between 60 orders, will be greater than 10 order granule granulate again, filter out conforming particle again, mix conforming particle, be distributed into bag.
In above-mentioned preferred embodiment, the method of the present invention, described step 2) in triple effect concentration, one effect temperature is less than 90 DEG C, vacuum is-0.02~-0.05Mpa, and two effect temperature are 80 ± 2 DEG C, and vacuum is-0.03~-0.06Mpa, triple effect temperature is 70 ± 2 DEG C, and vacuum is-0.04~-0.08Mpa.
In above-mentioned preferred embodiment, the method for the present invention, described step 5) in triple effect concentration, an effect temperature controls at 80~95 DEG C, and two effect temperature control at 70~80 DEG C, and triple effect temperature controls at 60~70 DEG C.
The effect of the method for the present invention: the supersound extraction Radix Paeoniae Alba carries out extracting checking in the present inventive method, extracts the amount amount (i.e. the peoniflorin of the non-supersound extraction of decocting) higher than test specimen of peoniflorin, and result is very good. The ultrasonic extraction of the present invention compares (see table 1) with former decocting cooking method extraction process, and the amount of peoniflorin is its 1.44 times, namely higher than nearly more than 44%. Therefore, selecting supersound extraction not only to reduce extraction time, reduce energy consumption, its extraction effect is considerably better than traditional extraction process.
The ultrasonic extraction of the present invention and former water boiling and extraction (condition: 100 DEG C, 1.5 hours/time, totally 2 times) contrast, result is in Table 1.
Table 1 Radix Paeoniae Alba ultrasonic extraction process Verification extracts result with former technique and compares
Detailed description of the invention
Following example are used for further illustrating the present invention, but its scope must not be limited to following embodiment.
Embodiment 1
Tongxiening granule agent, the weight ratio of its medicinal raw material is: the Radix Paeoniae Alba: Pericarpium Citri Reticulatae Viride: Bulbus Allii Macrostemonis: the Rhizoma Atractylodis Macrocephalae=1.6:1.6:1:1, and preparation process is:
1) dispensing
By above-mentioned weight ratio, weigh the medical material Radix Paeoniae Alba of recipe quantity, the Rhizoma Atractylodis Macrocephalae, Pericarpium Citri Reticulatae Viride, Bulbus Allii Macrostemonis standby.
2) extraction of Radix Paeoniae Alba medicinal liquid
Add the water of 10 times of medical material amounts to extraction pot, allow water become acutely to seethe, in tank, put into the radix paeoniae alba decoction pieces of ormal weight, after soaking 1 hour, heating makes water temperature be raised to 48~52 DEG C, opens supersonic generator, supersound extraction 2 times, 0.5 hour each extraction time, filter, collect filtrate; Medicinal residues merge with extracting the medicinal residues after volatile oil, then add the water boiling and extraction 1.5 hours of 8 times of weight, and the thick centrifugal bag of extracting solution is centrifuged, and centrifugal rear medicinal liquid carries out plate-and-frame filtration, and medicinal residues are standby, collection filtrate, merging filtrate; Being extracted in Three-effect concentration device by filtrate, hot water temperature, less than 90 DEG C, produces steam by an effect and imitates thermal source as two, produces steam as triple effect thermal source by two effects, and two effect temperature control at 80 ± 2 DEG C, and triple effect temperature controls at 70 ± 2 DEG C, concentration time 75 minutes. 1st effective evaporator vacuum is-0.02~-0.05Mpa, and 2nd effect evaporator vacuum is-0.03~-0.06Mpa, and triple effect evaporator vacuum is-0.04~-0.08Mpa, steam pressure 0.05~0.09Mpa, survey concentration from sample point sampling examination, when 50 DEG C concentrate specific gravity control when 1.1~1.15, stop concentration, discharging, prepare Radix Paeoniae Alba medicinal liquid, Radix Paeoniae Alba medicinal liquid is put in stainless steel cask, adopt flowing steam to carry out sterilizing, sterilising temp 90 DEG C~100 DEG C, sterilization time 30min.
3) volatile oil is drawn
Extraction pot adds the Pericarpium Citri Reticulatae Viride of recipe quantity, Bulbus Allii Macrostemonis and the Rhizoma Atractylodis Macrocephalae, after adding the drinking water of medical material gross weight 8 times, passes into straight-through steam and be heated, Stress control is at 0.05~0.08Mpa, in extraction pot tank, temperature reaches more than 110 DEG C, starts timing, collects volatile oil 5 hours; By standby for the volatile oil collected;
After volatile oil is drawn, after being filtered by 100 order filters by medicinal liquid, separate medicinal liquid and medicinal residues.
4) medicinal residues extract again
By step 2) Radix Paeoniae Alba medicinal residues and step 3) Pericarpium Citri Reticulatae Viride, Bulbus Allii Macrostemonis and Rhizoma Atractylodis Macrocephalae medicinal residues are mixed pack, put into and extraction pot carries out four taste extractions, 10 times of drinking waters of medical material total amount are added to extraction pot, heating, when temperature starts timing in tank when reaching 98 DEG C of i.e. boilings, extract 1.5h, when temperature reaches 98~100 DEG C, keep fluidized state, now open spray pump and be circulated extraction. After extraction time reaches 1.5h, after medicinal liquid is filtered by 100 order filters, deslagging, it is thus achieved that medicinal liquid.
5) triple effect concentration
Combining step 3) and step 4) medicinal liquid, put in Three-effect concentration device, open vacuum valve decompression, open cap relief valve heating and steam pressure is adjusted to below 0.09Mpa. Temperature controls: an effect controls at 80~95 DEG C, and two effects control at 70~80 DEG C, and triple effect controls at 60~70 DEG C. Concentration is surveyed from sample point sampling examination, 50 DEG C of concentration specific gravity control, when 1.1~1.15, stop concentration, discharging, medicinal liquid is put in Alcohol-settling tank or static tank, static more than 12 hours, the medicinal liquid after static is put in centrifuge centrifugal, first centrifuged supernatant, last centrifugal sediment, medicinal liquid after centrifugal is carried out plate-and-frame filtration, and filtering liquid medicine is an effect heat sterilization in triple effect filter, 90~100 DEG C of sterilizing half an hour.
6) by step 5) centrifugal after sterilizing medicinal liquid and step 3) the mixing of Radix Paeoniae Alba steam sterilization liquid.
7) preparation of extract powder
By step 6) merging medicinal liquid add in medicine liquid tank, when stirring, dextrin is added by the weight ratio 1:0.1 or 1:0.15 of medicinal liquid with dextrin, dissolve, then spray drying is carried out, dried collection finished product extract powder, the condition of spray drying is on vacuum and heating unit, with suitable speed, the medicinal liquid dissolving dextrin is sprayed in drying tower again, controlling inlet temperature is 140~180 DEG C, going out tower air temperature is 80~90 DEG C, delivery temperature is 70~80 DEG C, finished product temperature is 30~40 DEG C, in tower, temperature is 55~65 DEG C, tower wall cooling air temperature is 40~50 DEG C, tower wall temperature is 40~50 DEG C. prepare 0.1 times of dextrin extract powder or 0.15 times of dextrin extract powder
8) embedding volatile oil
By weight volatile oil: beta-schardinger dextrin-: purified water=1:8:60 feeds intake, heat the water to 85~90 DEG C, add beta-schardinger dextrin-stirring to be completely dissolved, be slowly added to volatile oil, and insulation is stirred continuously 1 hour, it is subsequently cooled to 0~10 DEG C, and it is incubated more than 24 hours, crystallize, filters, crystallization is dry under 40 DEG C of conditions, prepares volatile oil beta-cyclodextrin embedded object.
9) granulate
By extract powder: dextrin: beta-schardinger dextrin-embedded object: the weight ratio of protein sugar=1:1.2-1.5:0.1-0.15:0.07-0.08 feeds intake; concrete charge ratio is in Table 2; take extract powder, volatile oil beta-cyclodextrin embedded object is placed in one-step-granulating method; add dextrin and; after mix homogeneously; spraying adds raw material gross weight 50%, concentration again be 15% ethanol is binding agent, so as to molding in one-step-granulating method, dry.
Being sieved by prepared granule, cross 10 orders and 60 orders respectively, conforming particle more than granule between 60 orders less than 10 orders, will be greater than 10 order granule granulate and selects conforming particle again. Fine grained and coarse granule enter in dry granulating machine, and screening of again granulating takes conforming particle, and merge and be mixed conforming particle.
10) subpackage and packaging
Above-mentioned conforming particle is divided in the packaging bag meeting regulation material by 5g/ bag, then by packing specification requirement carried out mounted box, vanning.
The charged material weight ratio of table 2 extract powder, dextrin, beta-schardinger dextrin-embedded object and protein sugar

Claims (8)

1. a preparation method for Tongxiening granule, the weight ratio of its medicinal raw material is: the Radix Paeoniae Alba: Pericarpium Citri Reticulatae Viride: Bulbus Allii Macrostemonis: the Rhizoma Atractylodis Macrocephalae=1.6:1.6:1:1, and the method comprises the following steps:
1) adding the water of 8-15 times amount in supersound extraction tank, heating, to boiling, adds the Radix Paeoniae Alba, stops heating, soak 1-2 hour, then be warmed up to 48~52 DEG C, supersound extraction 2 times, 0.5-1 hour each extraction time, centrifugal filtration medicinal liquid and medicinal residues, collect medicinal liquid, and medicinal residues are standby;
2) medicinal liquid of upper step adopts triple effect concentration, stops concentration when the proportion of 50 DEG C of concentrated solutions is 1.1~1.15, filters, and filtrate is standby;
3) taking Pericarpium Citri Reticulatae Viride, Bulbus Allii Macrostemonis and the Rhizoma Atractylodis Macrocephalae and add the water of 8 times amount, mixing is soaked, is added thermal distillation, collects volatile oil, after, isolated by filtration medicinal liquid and medicinal residues;
4) step 1) and 3) medicinal residues merge, add the water of 6-12 times amount, heating, to boiling, is extracted 1-2 hour, is extracted 2 times, filtration, medicinal liquid and step 3) medicinal liquid merge;
5) by 4) merging medicinal liquid, adopt triple effect concentration, steam pressure not can exceed that 0.09MPa, stop concentration when the proportion of 50 DEG C of concentrated solutions is 1.1~1.15, stands, centrifugation extracting solution, filters, obtains filtrate;
6) by step 5) filtrate and step 2) filtrate merge, add dextrin, dissolve mix homogeneously, spray drying, prepare extract powder;
7) adding in purified water by beta-schardinger dextrin-, be heated to 85~90 DEG C, stirring is completely dissolved, and is slowly added to step 3) volatile oil, add volatile oil and be incubated 0.5-1.5 hour, then crystallisation by cooling, filter, dry, prepare beta-schardinger dextrin-embedded object;
8) granulate: by extract powder, dextrin, beta-cyclo dextrin included compound, protein sugar mixing granulation, granulate, cross 10 orders and 60 mesh sieves respectively, collect granule less than 10 orders more than the conforming particle between 60 orders, will be greater than 10 order granule reformation grains, then filter out conforming particle, mix conforming particle, it is distributed into bag
Wherein, step 2) in triple effect concentration, one effect temperature is less than 90 DEG C, vacuum is-0.02~-0.05Mpa, two effect temperature are 80 ± 2 DEG C, vacuum is-0.03~-0.06Mpa, triple effect is 70 ± 2 DEG C, vacuum is-0.04~-0.08Mpa, step 4) in, described triple effect concentrates, steam pressure not can exceed that 0.09MPa, an effect temperature control at 80~95 DEG C, two effect temperature control at 70~80 DEG C, and triple effect temperature controls at 60~70 DEG C, stop concentration when the proportion of the concentrated solutions of 50 DEG C is 1.1~1.15.
2. the method for claim 1, step 1) in, the consumption of water is the Radix Paeoniae Alba 10 times amount, and Radix Paeoniae Alba soak time is 1 hour, and each supersound extraction time is 45 minutes.
3. the method for claim 1, step 3) in, distillation Stress control is at 0.05~0.08Mpa, and vapo(u)rizing temperature is more than 110 DEG C, and distillation time is 5 hours, and medicinal liquid is filtered by 100 order filters.
4. the method for claim 1, step 4) in the consumption of water be 10 times amount of medicinal residues, start timing when boiling temperature reaches 98 DEG C, extract 1.5h, when temperature reaches 98~100 DEG C, keep fluidized state, extracting 1.5h, extracting solution crosses 100 order filters.
5. the method for claim 1, step 6) in, filtrate and dextrin weight ratio 1:0.1-0.15.
6. the method for claim 1, step 7) in, volatile oil: beta-schardinger dextrin-: the weight ratio of purified water is 1:8:60; Or to add volatile oil temperature retention time be 1 hour, or described crystallisation by cooling, cool to 0~10 DEG C, and be incubated more than 24 hours, crystallize, or described dry, baking temperature is 40 DEG C.
7. the method for claim 1, step 7) in, the weight ratio of extract powder, dextrin, beta-schardinger dextrin-embedded object and protein sugar is 1:1.2-1.5:0.1-0.15:0.07-0.08.
8. the method for claim 1, step 7) in, described crystallisation by cooling, cool to 0~10 DEG C, and be incubated more than 24 hours, crystallize, or described dry, baking temperature is 40 DEG C.
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