Xiao Chai Hu granules and preparation method thereof
Technical field
The present invention relates to traditional Chinese medicine preparation field, be specifically related to a kind of Xiao Chai Hu granules and preparation method thereof.
Background technology
Influenza (influenza is called for short influenza) is the ARI that influenza virus causes, and is also a kind of
The disease that infectiousness is strong, spread speed is fast.Its mainly by the spittle in air, interpersonal contact or with contaminated thing
The contact transmission of product.Typical clinical symptoms are: anxious high heat, overall pain, the most weak and slight respiratory symptom.Typically
Autumn and winter season is its high-incidence season, and caused complication and the phenomena of mortality are the most serious.Thus while influenza is very universal, but to it
Prevention and treatment have important clinical value.But, although medical procedure is the most flourishing at present, but still without being directly effective against disease
The medicine of poison and methods for the treatment of, method previously is only to increase body autoimmunity, extra-nutrition so that self is to antiviral
Ability strengthen, to reach the purpose for the treatment of, be i.e. to add with antiviral agent, but it also have a lot of side effect.Inoculation influenza vaccines
Also it is the more effective method of one, but characteristic based on virus self easily variation, and the vaccine often inoculated also is that It dones't help the situation,
Therefore, constantly find that the method updating treatment influenza has important value for clinic.
Influenza be caused by influenza virus, through the acute upper respiratory tract infectious disease of droplet transmission, have onset anxious,
The feature that infectiousness is strong, clinic often have heating, headache, weak, muscular soreness of whole body, have a stuffy nose, cough, the symptom such as have sore throat,
Inconvenience is brought to people's productive life, the elderly poor for resistance and infant, often induce other basic diseases
Disease, causes serious harm.At present, there is no the specific drug of resisiting influenza virus, the many uses of western medical treatment improve symptom, antiviral, carry
The treatment means such as high immunity;And traditional Chinese medicine preparation often has original merit in terms for the treatment of influenza, research before finds the traditional Chinese medical science
Medicine treatment has symptom to eliminate the advantages such as the time is short, expense is low relative to Western medicine, uses as cipher prescription in flu outbreak area
In treatment or prevention, especially there is promotional value.
Chinese patent 201110315091.4 discloses a kind of small radix bupleuri granular agent and preparation method thereof, and the method uses alcohol
Heavy, and fluidized bed granulation, cause final products yield low and operating difficulties, mix heterogeneity, occur defective existing under discriminating item
As (as the root of large-flowered skullcap and Radix Glycyrrhizae differentiate item).
Chinese patent 02125805.8 discloses the preparation technology of sugarless small radix bupleuri granular agent, and this technique is not to volatilization
Oil is collected, and end product quality has affected.Phenomenon, the stability such as mouthfeel difference is there will be bad after storage a period of time.
Summary of the invention
The invention provides a kind of Xiao Chai Hu granules and preparation method thereof, the Xiao Chai Hu granules mouthfeel that this preparation method obtains
Good, stability is high;Dissolubility is good simultaneously, it is simple to take.
The preparation method of a kind of Xiao Chai Hu granules, comprises the steps:
(1) in radix bupleuri, the root of large-flowered skullcap, Radix Codonopsis, Radix Glycyrrhizae and date add medicinal material weight 5~15 times amount water, be heated to 88~
102 DEG C, stirring is extracted 2~4 hours, and after extraction, liquid obtains the first extract through ultracentrifugation;
During extraction, collect after making volatile component condensation and obtain volatile oil;
(2) use the ethanol water of 70% that pinellia and ginger are carried out diacolation and obtain the second extract;
(3) combining step (1) obtains the first extract and the second extract that step (2) obtains, be concentrated under reduced pressure to give
Concentrate;
(4) in the volatile oil that step (1) obtains, add betadex, add thermal agitation to the most molten, obtain his ring paste again
Spermatophore closes liquid;
(5) the betadex inclusion liquid that the concentrate obtained step (3) and step (4) obtain uses and is spray-dried
Method, is dried successively and obtains Xiao Chai Hu granules dried cream powder;
(6) adding dextrin, maltodextrin and Steviosin in the Xiao Chai Hu granules dried cream powder that step (5) obtains, mixing is all
Use dry granulation after even, after sieving, obtain described Xiao Chai Hu granules.
In the present invention, when radix bupleuri, the root of large-flowered skullcap, Radix Codonopsis, Radix Glycyrrhizae and date five kinds of Chinese medicine are extracted, volatile components is received
After collection, use betadex to carry out inclusion, make volatile components be preserved;Meanwhile, extract is under conditions of heating
Centrifugal purification, saves the component of easily precipitation;The extract obtained can be adopted through the Xiao Chai Hu granules dried cream powder being dried to obtain
Obtain product with dry granulation, simplify operation;The Xiao Chai Hu granules solubility obtained is good and good stability, and result for the treatment of
Significantly.
As preferably, medicinal material and auxiliary material are as follows:
As preferably, in step (1), the temperature keeping liquid during ultracentrifugation is 80~86 DEG C, rotating speed control 1.0~
2.0 ten thousand revs/min.When being centrifuged separating, the temperature of liquid is the lowest, and active ingredient can be made to separate out, and reduces product yield,
Affect product quality.
As preferably, in step (2), the speed of diacolation is 5kg/h.
As preferably, in step (3), the temperature of reduced pressure concentration is 60~70 DEG C, and vacuum is-0.08~-0.086MPa.
As preferably, in step (4), the temperature adding thermal agitation is 60~75 DEG C.This temperature can make described volatile oil
Preferably inclusion, can prevent again the loss of volatile component.As further preferably, by weight, described volatile oil: times he
Cyclodextrin=3~6:1
As preferably, in step (5), EAT controls at 165~185 DEG C, and leaving air temp controls at 85~100 DEG C,
Pressure is maintained at 40~50Pa.As further preferably, described spray drying is EAT 170~180 DEG C, goes out wind-warm syndrome
It is spray-dried under conditions of spending 90~100 DEG C
As preferably, in the dry granulation of step (6), dry granulating machine nip pressure is 50Pa~70Pa, pressure roller rotating speed
Being 12 revs/min~18 revs/min, mixture transfer rate is 40 revs/min~60 revs/min;As the most preferred,
Described dry granulating machine nip pressure is 60Pa, and pressure roller rotating speed is 14 revs/min, and mixture transfer rate is 50 revs/min.
As preferably, in step (6), the mesh number of the medicine sieve sieving used is 12 mesh~40 mesh.
Present invention also offers a kind of Xiao Chai Hu granules, above-mentioned preparation method prepare.
Crude drug of the present invention is described in detail below:
Radix bupleuri: for umbelliferae bupleurum or the dry root of radix bupleuri scorzoneraefolii, pungent, bitter, it is slightly cold.Return liver, courage, lung channel;Tool
Evacuation is had to bring down a fever, soothing liver-qi stagnation, rise and lift yang-energy.For cold, fever, fevers and chills alternate, distending pain in the chest and hypochondrium, irregular menstruation, uterus takes off
Hang down, prolapse of the anus.
Pinellia: for the Preparation process product of the tuber of pinellia, pungent, temperature.Return spleen, stomach, lung channel.Have in temperature and reduce phlegm, stopping nausea and vomiting by lowering the adverse flow of QI.With
In phlematic vomiting, gastral cavilty ruffian is full.
The root of large-flowered skullcap: for the dry root of the labiate root of large-flowered skullcap.Bitter, cold.Return lung, courage, spleen, large intestine, small intestinl channel.There is heat-clearing dry
Wet, purging intense heat and detonicating, hemostasis, antiabortive.For damp-warm syndrome, summer-heat and damp, evil of vomitting uncomfortable in chest, damp and hot ruffian is full, rushes down dysentery, jaundice, cough with lung heat, high heat
Polydipsia, blood-head tells nosebleed, carbuncle pyogenic infections
Radix Codonopsis: for Campanulaceae Radix Codonopsis, element flower Radix Codonopsis or the dry root of radix codonpsis tangshen.Sweet, flat.Return spleen, lung channel.Invigorating the spleen benefit
Lung, nourishes blood and promotes the production of body fluid.For spleen-lung Qi deficiency, eating few burnout, cough void is breathed heavily, insufficiency of vital energy and blood, sallow complexion, palpitation, Tianjin wound
Yearningly, interior heat is quenched one's thirst.
Radix Glycyrrhizae: for glycyrrhizic legume, swollen fruit Radix Glycyrrhizae or the dry root of glycyrrhiza glabra and rhizome.Sweet, flat.The thoughts of returning home, lung,
Spleen, stomach warp.
Ginger: for the fresh rhizome of zingiber.Pungent, tepor.Return lung, spleen, stomach warp.Relieving exterior syndrome and dispelling cold, warming middle energizer to arrest vomiting, change
Phlegm and relieving cough, solving toxin of fish and crab.For anemofrigid cold, gastrofrigid vomiting, cold productive cough coughs, and fish crab is poisoned.
Date: for the dry mature fruit of Rhamnaceae plant jujube.Sweet, temperature.Return spleen, stomach, the heart channel of Hang-Shaoyin.Tonifying middle-Jiao and Qi, nourish blood peace
God.Few for insufficiency of the spleen food, weak loose stool, hysteria of womam.
Compared with the existing technology, the invention have the benefit that
(1) during the extraction to radix bupleuri, the root of large-flowered skullcap, Radix Codonopsis, Radix Glycyrrhizae and date, collect volatile oil and spray bag, to extraction
Liquid uses centrifugal method to purify, and improves the quality of product, and improves stability;
(2) the Xiao Chai Hu granules dried cream powder obtained can use dry granulation, the problem solving difficulty of pelletizing, and obtains
Particle dissolves in water rapidly, forms the solution that clear is in good taste, it is simple to take.
Detailed description of the invention
Embodiment 1
Radix bupleuri 200kg pinellia 75kg root of large-flowered skullcap 75kg Radix Codonopsis 75kg
Radix Glycyrrhizae 75kg ginger 75kg date 75kg dextrin 24kg
Maltodextrin 8kg betadex 10kg Steviosin 0.4kg
(1) medicinal material pre-treatment: above crude drug is ground into coarse granule standby:
(2) separation is extracted: take radix bupleuri 200kg, root of large-flowered skullcap 75kg, Radix Codonopsis 75kg, Radix Glycyrrhizae 75kg, date 75kg gomi herbs,
Add 3250kg water, be heated to 90 DEG C, under stirring, extract 2 hours, collect volatile oil simultaneously;Extract complete, centrifuge hypervelocity from
The heart, rotating speed controls at 1.0 ten thousand revs/min, and fluid temperature is maintained at 80 DEG C, standby;
(3) diacolation: using pinellia 75kg, ginger 75kg with 70% ethanol as solvent, impregnate 24 hours, with 5kg/h,
Slowly diacolation, filters, is recycled to without alcohol taste, standby;
(4) reduced pressure concentration: merging both the above liquid, concentrate, temperature is maintained at 60 DEG C, vacuum is maintained at-
0.08mpa, is 1.10(50 DEG C by concentration of liquid medicine to relative density), obtain concentrate, standby;
(5) parcel of volatile oil: the volatile oil 30kg that will collect, adds in pot, is heated to 60 DEG C, and limit heating edge adds again
He is cyclodextrin 10kg, and limit is stirred to the most molten, standby;
(6) it is dried: wink-dry.First spraying liquid, then connect the betadex inclusion liquid that spray mixes, spray process
In, EAT controls at 165 DEG C, and leaving air temp controls at 90 DEG C, and it is-5mmH that tower internal pressure power is maintained at 49.05Pa(2O);
(7) always mix: the Xiao Chai Hu granules dried cream powder being spray-dried gained adds dextrin 24kg, maltodextrin 8kg, Steviosin
0.4kg pours in mixer, mixes 30 minutes,;
(8) medicinal powder obtained as above is added dry granulating machine setting nip pressure as 50Pa, pressure roller rotating speed is 12 turns/
Minute, mixture transfer rate is 40 revs/min, and gained mixture, by crossing 12 mesh~40 mesh sieves after dry granulation, obtains little
Bupleurum particles.
Embodiment 2
Radix bupleuri 240kg pinellia 90kg root of large-flowered skullcap 90kg Radix Codonopsis 90kg
Radix Glycyrrhizae 90kg ginger 90kg date 90kg dextrin 30kg
Maltodextrin 10kg betadex 14kg Steviosin 0.6kg
(1) medicinal material pre-treatment: above crude drug is ground into coarse granule standby:
(2) separation is extracted: take radix bupleuri 240kg, root of large-flowered skullcap 90kg, Radix Codonopsis 90kg, Radix Glycyrrhizae 90kg, date 90kg gomi herbs,
Add 3600kg water, be heated to 95 DEG C, under stirring, extract 2.5 hours, collect volatile oil simultaneously;Extracting complete, centrifuge exceeds the speed limit
Centrifugal, rotating speed controls at 1.5 ten thousand revs/min, and fluid temperature is maintained at 82 DEG C, standby;
(3) diacolation: using pinellia 90kg, ginger 90kg with 70% ethanol as solvent, impregnate 24 hours, with 5kg/h,
Slowly diacolation, filters, is recycled to without alcohol taste, standby;
(4) reduced pressure concentration: merging both the above liquid, concentrate, temperature is maintained at 65 DEG C, vacuum is maintained at-
0.08mpa, is 1.12(50 DEG C by concentration of liquid medicine to relative density), obtain concentrate, standby;
(5) parcel of volatile oil: the volatile oil 42kg that will collect, adds in pot, is heated to 65 DEG C, and limit heating edge adds again
He is cyclodextrin 14kg, and limit is stirred to the most molten;
(6) it is dried: wink-dry.First spraying liquid, then connect the betadex inclusion liquid that spray mixes, spray process
In, EAT controls at 168 DEG C, and leaving air temp controls at 98 DEG C, and tower internal pressure power is maintained at 49.05Pa;
(7) always mix: the Xiao Chai Hu granules dried cream powder being spray-dried gained adds dextrin 30kg, maltodextrin 10kg, Steviosin
0.6kg pours in mixer, mixes 30 minutes,;
(8) medicinal powder obtained as above is added dry granulating machine setting nip pressure as 55Pa, pressure roller rotating speed is 14 turns/
Minute, mixture transfer rate is 45 revs/min, and gained mixture, by crossing 12 mesh~40 mesh sieves after dry granulation, obtains little
Bupleurum particles.
Embodiment 3
Radix bupleuri 300kg pinellia 112.5kg root of large-flowered skullcap 112.5kg Radix Codonopsis 112.5kg
Radix Glycyrrhizae 112.5kg ginger 112.5kg date 112.5kg dextrin 33kg
Maltodextrin 11kg betadex 20kg Steviosin 0.8kg
(1) medicinal material pre-treatment: above crude drug is ground into coarse granule standby:
(2) separation is extracted: take radix bupleuri 300kg, root of large-flowered skullcap 112.5kg, Radix Codonopsis 112.5kg, Radix Glycyrrhizae 112.5kg, date
112.5kg gomi herbs, adds 5250kg water, is heated to 98 DEG C, under stirring, extracts 3 hours, collect volatile oil simultaneously;Extract
Complete, centrifuge ultracentrifugation, rotating speed controls at 1.7 ten thousand revs/min, and fluid temperature is maintained at 85 DEG C, standby;
(3) diacolation: using pinellia 112.5kg, ginger 112.5kg with 70% ethanol as solvent, impregnate 24 hours, with
5kg/h, slow diacolation, filter, be recycled to without alcohol taste, standby;
(4) reduced pressure concentration: merging both the above liquid, concentrate, temperature is maintained at 68 DEG C, vacuum is maintained at-
0.08mpa, is 1.12(50 DEG C by concentration of liquid medicine to relative density), obtain concentrate, standby;
(5) parcel of volatile oil: the volatile oil 80kg that will collect, adds in pot, is heated to 68 DEG C, and limit heating edge adds again
He is cyclodextrin 20kg, and limit is stirred to the most molten;
(6) it is dried: wink-dry.First spraying liquid, then connect the betadex inclusion liquid that spray mixes, spray process
In, EAT controls at 170 DEG C, and leaving air temp controls at 100 DEG C, and tower internal pressure power is maintained at 49.05Pa;
(7) always mix: the Xiao Chai Hu granules dried cream powder being spray-dried gained adds dextrin 33kg, maltodextrin 11kg, Steviosin
0.8kg pours in mixer, mixes 30 minutes,;
(8) medicinal powder obtained as above is added dry granulating machine setting nip pressure as 60Pa, pressure roller rotating speed is 16 turns/
Minute, mixture transfer rate is 50 revs/min, and gained mixture, by crossing 12 mesh~40 mesh sieves after dry granulation, obtains little
Bupleurum particles.
Embodiment 4
Radix bupleuri 320kg pinellia 120kg root of large-flowered skullcap 120kg Radix Codonopsis 120kg
Radix Glycyrrhizae 120kg ginger 120kg date 120kg dextrin 39kg
Maltodextrin 13kg betadex 16kg Steviosin 0.8kg
(1) medicinal material pre-treatment: above crude drug is ground into coarse granule standby:
(2) separation is extracted: take radix bupleuri 320kg, root of large-flowered skullcap 120kg, Radix Codonopsis 120kg, Radix Glycyrrhizae 120kg, date 120kg five kinds of Chinese medicine
Material, adds 8000kg water, is heated to 98 DEG C, under stirring, extracts 3 hours, collect volatile oil simultaneously;Extracting complete, centrifuge surpasses
Speed is centrifugal, and rotating speed controls at 2.0 ten thousand revs/min, and fluid temperature is maintained at 86 DEG C, standby;
(3) diacolation: using pinellia 120kg, ginger 120kg with 70% ethanol as solvent, impregnate 24 hours, with 5kg/
H, slow diacolation, filter, be recycled to without alcohol taste, standby;
(4) reduced pressure concentration: merging both the above liquid, concentrate, temperature is maintained at 70 DEG C, vacuum is maintained at-
0.08mpa, is 1.12(50 DEG C by concentration of liquid medicine to relative density), obtain concentrate, standby;
(5) parcel of volatile oil: the volatile oil 48kg that will collect, adds in pot, is heated to 70 DEG C, and limit heating edge adds again
He is cyclodextrin 16kg, and limit is stirred to the most molten;
(6) it is dried: wink-dry.First spraying liquid, then connect the betadex inclusion liquid that spray mixes, spray process
In, EAT controls at 180 DEG C, and leaving air temp controls at 95 DEG C, and tower internal pressure power is maintained at 49.05Pa;
(7) always mix: the Xiao Chai Hu granules dried cream powder being spray-dried gained adds dextrin 39kg, maltodextrin 13kg, Steviosin
0.8kg pours in mixer, mixes 30 minutes,;
(8) medicinal powder obtained as above is added dry granulating machine setting nip pressure as 70Pa, pressure roller rotating speed is 18 turns/
Minute, mixture transfer rate is 55 revs/min, and gained mixture, by crossing 12 mesh~40 mesh sieves after dry granulation, obtains little
Bupleurum particles.
Comparative example 1
Except not adding volatile oil in prescription, remaining operation is with embodiment 1.
Comparative example 2
Except using wet granulation in prescription, remaining operation is with embodiment 2.
Comparative example 3
Radix bupleuri 150g, the tuber of pinellia, the root of large-flowered skullcap, ginseng, date, Radix Glycyrrhizae, each 56g of ginger, its preparation method:
(1) by radix bupleuri boiling 3 times, 12 times of medicinal material amounts for the first time, for the second time 10 times of medicinal material amounts, for the third time 8 times of medicinal materials
Amount, each 2 hours, collecting decoction, filter the clear cream being condensed into 60~65 DEG C of condition little survey relative densities are 1.15~1.18.
Cooling, adds ethanol and makes alcohol content reach 60%, stir, stand, filter, obtain filter residue and filtrate A;
(2) filter residue washs 3 times with the ethanol of 60%, merges washing lotion and filtrate A, reclaims ethanol and is condensed into 40 DEG C of conditions
Lower survey relative density is the thick paste A of 1.30~1.32
(3) root of large-flowered skullcap, ginseng, date, Radix Glycyrrhizae respectively with percent by volume be 50~95% ethanol solution dipping 10~25 little
Time, filter, filtrate recycling ethanol, be condensed into thick paste B;
(4) by the tuber of pinellia, ginger boiling 2~3 times, each 1~3 hour, collecting decoction, stand, filter, filtrate is with thick
Cream A, B mix, and are condensed into obtain the thick paste that relative density is 1.10~1.35 further;
(5) gained thick paste is added fluid bed on conventional use of auxiliary material and carry out fluidized granulating, obtain of the present invention
Granule.
In described step (5) fluid bed granulation, the optimization technique parameter of fluid bed fluidized granulating is: atomisation pressure
0.15~0.45 MPa;Temperature of charge 50~65 DEG C;EAT 68~100 DEG C;Leaving air temp 35~65 DEG C;Optimize, spraying
Pressure 0.15~0.45 MPa;Temperature of charge 55~60 DEG C;EAT 80~100 DEG C;Leaving air temp 60~65 DEG C.
By embodiment 1~4 and the Xiao Chai Hu granules for preparing respectively of comparative example 1~3 by Chinese Pharmacopoeia two attached I of version in 2010
Rules of preparations IN carries out quality inspection, concrete assay such as table 1:
Table 1
As shown in Table 1, prescription and preparation method, the Xiao Chai Hu granules mobility obtained and the mouth of the present invention are used
Feeling, and content is high, dissolubility is good, it is simple to absorb.
Xiao Chai Hu granules pin prepared by the Xiao Chai Hu granules embodiment of the present invention 1~4 prepared and comparative example 3 carries out stable
Property test, use accelerated test method it is carried out study on the stability, in temperature 28 DEG C~32 DEG C, relative humidity 55%~65%
Condition is accelerated to place 6 months, the results are shown in Table 2.
Table 2
Visible, the stability of the Xiao Chai Hu granules that preparation method of the present invention obtains is better than particle prepared by prior art.
Clinical testing
Subjects is for making a definite diagnosis patients with influenza;Experimental group is taken the present embodiment 1~4 and is prepared the little radix bupleuri of gained
Grain.
Result of the test such as table 3: observe case 200 example.
Table 3
Group |
Total number of cases |
Recovery from illness |
Effective |
Effectively |
Invalid |
Total effectively example |
Embodiment 1 |
200 |
145(72.5%) |
25(12.5%) |
22(11%) |
8(4%) |
96% |
Embodiment 2 |
200 |
145(72.5%) |
29(14.5%) |
20(10%) |
6(3%) |
97% |
Embodiment 3 |
200 |
140(70%) |
30(15%) |
21(10.5%) |
9(4.5%) |
95.5% |
Embodiment 4 |
200 |
136(68%) |
32(16%) |
22(11%) |
10(5%) |
95% |
As shown in Table 3, what the Xiao Chai Hu granules popularity using the preparation method of the present invention to prepare was caught a cold has
Efficiency is more than 95%.