CN108210810A - A kind of preparation process of Chinese medicine composition - Google Patents
A kind of preparation process of Chinese medicine composition Download PDFInfo
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- CN108210810A CN108210810A CN201611157194.1A CN201611157194A CN108210810A CN 108210810 A CN108210810 A CN 108210810A CN 201611157194 A CN201611157194 A CN 201611157194A CN 108210810 A CN108210810 A CN 108210810A
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Classifications
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Abstract
The present invention relates to a kind of preparation processes of Chinese medicine composition, containing Radix Salviae Miltiorrhizae 400 480, santal 44 52, dalbergia wood 89 107, santal 44 52, nutmeg 132 158, fructus choerospondiatis 132 158, sea-buckthorn 132 158, agalloch eaglewood 200 240, the Bi roots of grass 122 146, kaempferia galanga 66 80, following (1) santal of step, dalbergia wood, santal, nutmeg extraction volatile oil；(2) volatile oil is included with beta cyclodextrin；(3) Radix Salviae Miltiorrhizae adds ethyl alcohol heating and refluxing extraction, and filtering is condensed into clear cream；(4) the Radix Salviae Miltiorrhizae dregs of a decoction and fructus choerospondiatis, sea-buckthorn, agalloch eaglewood, kaempferia galanga, the Bi roots of grass add ethyl alcohol heating and refluxing extraction, and filtering is condensed into clear cream；(5) the ten taste dregs of a decoction in step (1) (4) add water to cook, and filtrate merges with step (1) Aqueous extracts, and alcohol precipitation takes supernatant concentration into clear cream；(6) clear cream obtained by step (3) (5) merges, and spray drying adds in step (2) volatile oil clathrate compound, and mixing to obtain the final product.
Description
Technical field
The invention belongs to technical field of traditional Chinese medicines, more particularly to a kind of preparation process for the Chinese medicine composition for treating coronary heart disease.
Background technology
Incidence of the coronary heart disease in middle old man is higher and higher, and shows gradually to the developing state of rejuvenation.Hat
Cardiaopath would generally be with situations such as palpitaition, angina pectoris, heart blood supply insufficiencies, it is impossible to be engaged in manual labor, serious life is not
It can take care of oneself or even dead.Treatment coronary heart disease is expensive often with Western medicine at present, and toxic side effect is also very big, and in applying at present
Medicine is treated or auxiliary treatment can only mitigate patient suffering, it is impossible to be effected a radical cure, and curative effect can not be satisfactory.Therefore clinically convection potential
Effect is notable, safety is good, Chinese medicine preparation easy to use is still to be badly in need of.
Coronary disease Huoxue Capsule disclosed in CN101554466 is a kind of Chinese medicine composition for treating coronary heart disease, it is by following
Medicinal material forms：Radix Salviae Miltiorrhizae 230g, Bi roots of grass 70g, agalloch eaglewood 115g, dalbergia wood 51g, nutmeg 76g, kaempferia galanga 38g, fructus choerospondiatis 76g, santal 25g,
Sea-buckthorn 76g, red sandalwood 25g.Its preparation process is as follows：Radix Salviae Miltiorrhizae, the Bi roots of grass, kaempferia galanga, fructus choerospondiatis, sea-buckthorn, nutmeg extract three times, for the first time
14 times of 75% ethyl alcohol of amount is added to be heated to reflux 2 hours, for the second time plus 12 times of 75% ethyl alcohol of amount are heated to reflux 2 hours, third time plus 10
75% ethyl alcohol of amount is heated to reflux 2 hours again, recycles ethyl alcohol；Agalloch eaglewood, dalbergia wood, red sandalwood, santal 8 times of water of coarse powder impregnate 5 hours after
Volatile oil is extracted, is extracted 2 times, 14 hours every time, Aqueous extracts filtering, the dregs of a decoction added 8 times of water to be heated to reflux 2 hours, filter, and merge
Extracting solution, concentration obtain dried cream powder after dry.
Documents and materials report Radix Salviae Miltiorrhizae contains tanshinone and tanshin polyphenolic acid B, santal contain volatile oil santalol, dalbergia wood contains volatilization
Containing pterocarpin, homopterocarpine, angolensin, nutmeg contains volatile oil, fat by oil, flavone compound, santal master
The ingredients such as acid, sucrose；Fructus choerospondiatis contains the ingredients such as flavones and gallic acid；Sea-buckthorn master contains flavones and isoflavone compound, agalloch eaglewood
Containing volatile oil and flavones ingredient, kaempferia galanga contains Kaempferol, and the Bi roots of grass contains volatile oil, pipering.It is effective in above-mentioned medicinal material
The existing alcohol-soluble active ingredient tanshinone of ingredient, flavones, isoflavone compound, alkaloid, chlorogenic acid and phytosterin compound,
Again containing aqueous soluble active constituent tanshin polyphenolic acid B and polysaccharide, while also contain volatile oil.But failing in above-mentioned technique will be in nutmeg
Volatile oil extract.Although containing volatile oil in agalloch eaglewood, the flavones ingredient physiological activity wherein contained is stronger, has
Apparent the effect of understanding oxygen radical.Therefore, it is necessary to be improved to above-mentioned preparation process, it is made preferably to play treatment
Effect.
Invention content
The purpose of the present invention is to provide a kind of preparation process for the Chinese medicine composition for treating coronary heart disease,
The Chinese medicine composition contains following component：Radix Salviae Miltiorrhizae 400-480 parts by weight, santal 44-52 parts by weight, dalbergia wood
89-107 parts by weight, santal 44-52 parts by weight, nutmeg 132-158 parts by weight, fructus choerospondiatis 132-158 parts by weight, sea-buckthorn 132-
158 parts by weight, agalloch eaglewood 200-240 parts by weight, Bi roots of grass 122-146 parts by weight, preferably kaempferia galanga 66-80 parts by weight, Radix Salviae Miltiorrhizae 440g
Parts by weight, santal 48g parts by weight, dalbergia wood 98g parts by weight, santal 48g parts by weight, nutmeg 145g parts by weight, fructus choerospondiatis 145g
Parts by weight, sea-buckthorn 145g parts by weight, agalloch eaglewood 220g parts by weight, Bi roots of grass 134g parts by weight, kaempferia galanga 73g parts by weight.
According to the physicochemical property of effective ingredient, produce reality situation, by test repeatedly, study, analyze compare and
It is as follows to formulate preparation process：
(1) santal, dalbergia wood, santal are broken into coarse powder, nutmeg is knocked broken addition water and impregnated, and refluxing extraction obtains volatile oil
And Aqueous extracts, it is spare；
(2) gained volatile oil is added in containing beta-cyclodextrin inclusion compound in step (1), obtains volatile oil clathrate compound, spare；
(3) Radix Salviae Miltiorrhizae adds ethyl alcohol heating and refluxing extraction, and extracting solution filtration, filtrate recycling ethanol is simultaneously condensed into clear cream, spare；
(4) step (3) the Radix Salviae Miltiorrhizae dregs of a decoction and fructus choerospondiatis, sea-buckthorn, agalloch eaglewood, kaempferia galanga, the Bi roots of grass five tastes add ethyl alcohol heating and refluxing extraction, close
And extracting solution, filtration, filtrate recycling ethanol is simultaneously condensed into clear cream, spare；
(5) the ten taste dregs of a decoction merging in step (1)-(4) adds water to cook, and decocting liquid filtration, filtrate is closed with step (1) Aqueous extracts
And concentrate and ethyl alcohol is added to make precipitation, supernatant is taken, ethyl alcohol is recycled and is simultaneously condensed into clear cream, it is spare；
(6) clear cream obtained by step (3)-(5) merges, spray drying, adds in step (2) volatile oil clathrate compound, mixing to get
Chinese medicine composition.
Step (1) is preferably：Santal, dalbergia wood, santal are broken into coarse powder, nutmeg knocks broken 6-10 times of addition and measures water, soak
Bubble 1-3 hours, refluxing extraction 4-8 hours, more preferably santal, dalbergia wood, santal are broken into coarse powder, nutmeg knocks broken addition 8
Amount water again impregnates 2 hours, refluxing extraction 8 hours；
Step (2) is preferably：Every milliliter of volatile oil of gained adds in the saturated aqueous solution of the beta-cyclodextrin containing 3-5g in step (1)
It is included under the conditions of 40~60 DEG C 1-3 hours, more preferably every milliliter of volatile oil adds in the saturated aqueous solution of the beta-cyclodextrin containing 4g
It is included 2 hours under the conditions of 60 DEG C；
Step (3) is preferably：Radix Salviae Miltiorrhizae adds 6-10 times of 60~90% ethyl alcohol heating and refluxing extraction measured 1-3 times, every time 1.5~
2.5 hours, extracting solution filtered, filtrate recycling ethanol and the clear cream for being concentrated into relative density 1.03~1.08 (40 DEG C of surveys), spare,
More preferably Radix Salviae Miltiorrhizae adds the 90% ethyl alcohol heating and refluxing extraction 3 times of 10 times of amounts, 1.5 hours every time, extracting solution filtration, filtrate recycling
Ethyl alcohol and the clear cream for being concentrated into relative density 1.05 (40 DEG C of surveys)；
Step (4) is preferably：The Radix Salviae Miltiorrhizae dregs of a decoction and fructus choerospondiatis in step (3), sea-buckthorn, agalloch eaglewood, kaempferia galanga, the Bi roots of grass five tastes add 6-10 times
It measures 40~80% ethyl alcohol heating and refluxing extraction 1~3 time, 1.5~2.5 hours every time, merges extracting solution, filtration, filtrate recycling second
Alcohol and the clear cream for being concentrated into relative density 1.03~1.08 (40 DEG C of surveys), more preferably step (3) the Radix Salviae Miltiorrhizae dregs of a decoction and fructus choerospondiatis, it is husky
Spine, agalloch eaglewood, kaempferia galanga, the Bi roots of grass five tastes add 10 times to measure 60% ethyl alcohol heating and refluxing extraction 2 times, 2 hours every time, merge extracting solution, filter
It crosses, filtrate recycling ethanol and the clear cream for being concentrated into relative density 1.05 (40 DEG C of surveys)；
Step (5) is preferably：The ten taste dregs of a decoction in step (1)-(4) merge plus 6-10 times is measured water and decoct 1~3 time, and every time 1
~3 hours, decocting liquid filtration, filtrate merged with step (1) Aqueous extracts, was concentrated into the clear of relative density 1.05~1.08 (40 DEG C of surveys)
Cream, ethyl alcohol is added to make alcohol content, and up to 60~80%, standing makes precipitation, takes supernatant, recycles ethyl alcohol and is concentrated into relative density
The clear cream of 1.05~1.08 (40 DEG C of surveys)；The ten taste dregs of a decoction more preferably in step (1)-(4) merge plus 8 times of amount water decoct 2 times,
2 hours every time, decocting liquid filtration, filtrate merged with step (1) Aqueous extracts, was concentrated into the clear cream of relative density 1.06 (40 DEG C of surveys),
Ethyl alcohol is added to make alcohol content, and up to 60%, standing 24 hours makes precipitation, takes supernatant, recycles ethyl alcohol and is concentrated into relative density 1.05
The clear cream of (40 DEG C of surveys)；
Step (6) resulting composition adds suitable auxiliary material that the oral preparations such as capsule, granule, tablet can be made.
Specific embodiment
1 Extraction Process of Volatile Oil of embodiment
Document report, santal, dalbergia wood, santal, nutmeg four traditional Chinese medicine material contain volatile oil in prescription, and volatile oil has virtue
The effect of perfume (or spice) is had one's ideas straightened out.To explore the extraction process of volatile oil in prescription, using the collecting amount of volatile oil as Testing index, use is orthogonal
The method of experiment has carried out system research to the extraction process of volatile oil.Designing investigation factor is：Soaking time, liquid volume added and steaming
The time is evaporated, each factor determines three levels, refers to table 1.
1 coronary disease Huoxue Capsule Extraction Process of Volatile Oil of table investigates factor and level
Experimental method：9 parts of sample is taken, every part of precision weighs santal 25g, dalbergia wood 51g, santal 25g, nutmeg 76g, presses
According to orthogonal test L9(34) table condition arrangement experiment, with volatile oil extracting instrument measure each sample volatile oil collecting amount.It will measure
As a result it is included in table 2, the results are shown in Table 2.
2 L of table9(34) orthogonal table and experimental result
The result shows that：The affecting laws of each factor are：A ＞ B ＞ C, optimum process condition A2B2C1, i.e. 8 times of liquid volume addeds,
It impregnates 2 hours, extracts 8 hours.
3 Extraction Process of Volatile Oil variance analysis of table
The result shows that：The results of analysis of variance shows that there was no significant difference between each factor level, so according to intuitive analysis
As a result Extraction Process of Volatile Oil is finally set to 8 times of liquid volume addeds, impregnates 2 hours, extracts 8 hours.
2 inclusion essential oil technique of embodiment
To reduce volatilization of the volatile oil in storage period, we use beta-cyclodextrin inclusion compound.It is real according to documents and materials and production
Border situation determines that investigation factor is：The ratio, inclusion temperature, inclusion time of oil and beta-cyclodextrin, each factor determines three water
It is flat, refer to table 4.
4 coronary disease Huoxue Capsule inclusion essential oil technique of table investigates factor and level
Experimental method：Precision draws 9 parts, every part of 10ml of volatile oil, and L is pressed with saturated water solution method9(34) orthogonal array institute
Row experiment condition is included, and is put in refrigerator and is stood 24 hours.It filters, after inclusion compound is dry under the conditions of 40 DEG C and bring public affairs into
Formula, inclusion compound actual weight/(β-CD+ throw oil mass) × 100%, calculates inclusion compound recovery rate, and be included in table 5, the results are shown in Table
5。
5 L of table9(34) orthogonal table and experimental result
The result shows that：The affecting laws of each factor are：C ＞ A ＞ B ＞, optimum process condition A2B1C2, i.e., it is oily: cyclodextrin
1: 4,60 DEG C include 2 hours.
6 inclusion essential oil technique variance analysis of table
As a result：The results of analysis of variance shows that there was no significant difference between each factor level, so according to intuitive analysis result
Inclusion essential oil technique is finally set to every ml volatile oil and adds in the beta-cyclodextrin saturated solution containing 4g that 2 are included under the conditions of 60 DEG C is small
When.
3 tanshinone alcohol extraction process of embodiment
Designing investigation factor is：Determining alcohol, liquid volume added, return evaporate the time and return evaporate number, each factor determines three levels, in detail
It is shown in Table 7.
7 coronary disease Huoxue Capsule tanshinol extraction process of table investigates factor and level
Test method：9 parts of sample is taken, every part of precision weighs Radix Salviae Miltiorrhizae 300g, pacifies according to the condition of orthogonal test L9 (34) table
Row's experiment after the completion of extraction, recycles ethyl alcohol, and concentration is settled in 1000ml volumetric flasks, obtains 9 parts of extracting solution samples.Each sample liquid
It shakes up, respectively takes 1ml, put in triangular flask be evaporated respectively, add in methanol 50ml, flow back 1h, filtering, and constant volume is spare.Precision weighs pellet
Join ketone IIA (lot numbers：110766200417) 2.04mg is in 10ml volumetric flasks, and precision draws 2ml, with methanol constant volume to 25ml,
It is spare.By 9 parts of sample liquids of said extracted, with filtering with microporous membrane, primary filtrate is discarded, collects subsequent filtrate in EP pipes, sample introduction
10 μ l, with methanol/water=75: 25 be mobile phase, gas pressure 3.0kpa, 70 DEG C of detector temperature measures containing for tanshinone IIA
Amount.It the results are shown in Table 8.
The content of 8 Tanshinone I I A of table
By assay in table as a result, being handled through mathematical statistics, 9. are the results are shown in Table
9 L of table9(34) orthogonal table and experimental result
The result shows that：The affecting laws of each factor are：B ＞ D ＞ C ＞ A, optimum process condition A3B3C3D3I.e. 90%
Ethanol solution, 10 times of liquid volume addeds, refluxing extraction 2.5h are extracted 3 times.Variance analysis is carried out after 9 data of table are statistically analyzed,
It the results are shown in Table 10.
10 analysis of variance table of table
The results of analysis of variance shows：There is the difference of conspicuousness, without aobvious between A, C, D factor level between B factor levels
The difference of work property.
As a result：With reference to intuitive analysis result and the results of analysis of variance, Radix Salviae Miltiorrhizae alcohol extracting optimised process item in coronary disease Huoxue Capsule
Part is：A3B3C3D3, i.e., medicinal material every time extract 3 times by 10 times of 90% ethyl alcohol measured of addition, refluxing extraction 2.5 hours.
4 total flavone extracting process of embodiment
Document report, kaempferia galanga in prescription, fructus choerospondiatis, sea-buckthorn, agalloch eaglewood, the Bi roots of grass active constituent be flavone compound, flavones
The effects that class compound, which has, calms the nerves, allevating angina pectoris, the improvement rhythm of the heart, anti-cardiovascular disease.To explore general flavone in prescription
Extraction conditions, using Stellera chamaejasme chromone be standard items general flavone content as inspection target, using the method for orthogonal test to general flavone
Extraction process has carried out system research.
Designing investigation factor is：Determining alcohol, liquid volume added, return time and extraction time, each factor determine three levels, in detail
It is shown in Table 11.
11 coronary disease Huoxue Capsule general flavone alcohol extracting taking technique of table investigates factor and level
Experimental method：9 parts of sample is taken, every part of precision weighs agalloch eaglewood 115g, fructus choerospondiatis 76g, sea-buckthorn 76g, kaempferia galanga 38g, the Bi roots of grass
70g, altogether 375g.It puts in 5000ml ground flasks, by L9(34) orthogonal array experiment arrangement.After the completion of extraction, second is recycled
Alcohol, concentration, is settled in 1000ml volumetric flasks, shakes up respectively.Precision is measured in each sample liquid 10ml to evaporating dish, is evaporated, residual
Slag adds 10ml methanol heating extraction 1h, and filtering, filter residue is rinsed with methanol, and filtrate is settled to 25ml volumetric flasks, shakes up, spare.Through
Detection Stellera chamaejasme chromone and coronary disease Huoxue Capsule in general flavone have similar absorption peak at 297nm, therefore select 297nm for
Measure wavelength.
The investigation of linear relationship and the preparation of standard curve：Take the dry Stellera chamaejasme chromone reference substance to constant weight, precision amount
1ml is taken, adds suitable 70% ethyl alcohol is quantitative the solution of the 100 μ g containing chromone in every 1ml is made, shakes up in 10ml volumetric flasks,
To obtain the final product.Precision draws 0.5,1.0,1.5,2.0,2.5ml reference substance solutions and series of standards solution is made.It shakes up, stands 15 points
Zhong Hou, using extracting solution as reference solution (70% ethyl alcohol), according to UV-VIS spectrophotometry (China's coastal port one
Portion annex V A), ultraviolet-visible spectrophotometer is got at UV, using 70% ethyl alcohol as blank, is measured at 297nm wavelength
Trap.Regression analysis is carried out to solution concentration with trap, as a result concentration is in good line in the range of 5.00-25.00 μ g/ml
Sexual intercourse.Regression equation Y=0.0361X+0.0031, r=0.9994.It the results are shown in Table 12.
The standard curve data of 12 Determination of Total Flavonoids of table
The assay of sample liquid：Above-mentioned 9 parts of sample liquids are taken, every part of accurate measurement 0.2ml is held with methanol constant volume to 25ml
It in measuring bottle, shakes up, absorbance value is measured at 297nm wavelength, substitute into the content of general flavone in regression equation calculation each sample, knot
Fruit is shown in Table 13：
The assay result of 13 coronary disease Huoxue Capsule general flavone of table
By assay in table 13 as a result, being handled through mathematical statistics, 14 are the results are shown in Table
14 L of table9(34) orthogonal table and experimental result
The result shows that：The affecting laws of each factor are：D ＞ C ＞ A ＞ B, optimum process condition A2B2C2D3, i.e., 60%
Ethanol solution, 8 times of liquid volume addeds, refluxing extraction 2h are extracted 3 times.Variance analysis is carried out after 14 data of table are statistically analyzed, is tied
Fruit is shown in Table 15.
15 analysis of variance table of table
The results of analysis of variance shows：There was no significant difference between each factor level.From the final technique item of produce reality
Part is A2B2C2D3, i.e., 60% ethanol solution, 10 times of liquid volume addeds, refluxing extraction 2h, extraction 2 times.
5 Salvia miltiorrhiza slag extraction process by water of embodiment
Document report, Radix Salviae Miltiorrhizae contains aqueous soluble active constituent tanshin polyphenolic acid B and polysaccharide in prescription.For ensure it is water-soluble effectively into
Us can fully be extracted by, which dividing, is optimized extraction process by water by orthogonal design.According to produce reality situation determine investigate because
Element is soaking time, liquid volume added, extraction time and extraction time.Each factor determines three levels.Refer to 16.
16 coronary disease Huoxue Capsule Radix Salviae Miltiorrhizae extraction process by water of table investigates factor and level
Experimental method：9 parts of sample is taken, every part of precision weighs Radix Salviae Miltiorrhizae 230g, agalloch eaglewood 115g, fructus choerospondiatis 76g, sea-buckthorn 76g, kaempferia galanga
38g, Bi roots of grass 70g, santal 25g, dalbergia wood 51g, santal 25g, nutmeg 76g, put in 10000ml ground flasks, by table 17L9
(34) orthogonal array experiment arrangement.After the completion of extraction, it is concentrated under reduced pressure, is settled in 1000ml volumetric flasks, shakes up respectively.Respectively take
1ml puts in triangular flask and is evaporated, and adds in methanol 50ml, and flow back 1h, filtering, and constant volume is spare.According to Chinese Pharmacopoeia 2005 editions.
The content assaying method of tanshin polyphenolic acid B measures the content of tanshin polyphenolic acid B in each sample liquid, and is included in table 17, as a result sees
Table 17.
17 L of table9(34) orthogonal table and experimental result
The result shows that：The affecting laws of each factor are：C ＞ B ＞ A ＞, optimum process condition A2B2C2I.e. every time 8 extraordinarily
Liquid measure, refluxing extraction 2.0h are extracted 2 times.Variance analysis is carried out after 17 data of table are statistically analyzed, the results are shown in Table 18.
18 extraction process by water analysis of variance table of table
Variance the result shows that；The results of analysis of variance shows that there was no significant difference between each factor level, so according to intuitive
Analysis result extraction process by water is finally set to：Medicinal material adds in 8 times of amount water and decocts every time, and decoction is secondary, 2 hours every time.
To sum up Study on extraction the result shows that：Radix Salviae Miltiorrhizae alcohol extracting optimum process condition is in coronary disease Huoxue Capsule：
A3B3C3D3, i.e., medicinal material every time extract 3 times by 10 times of 90% ethyl alcohol measured of addition, refluxing extraction 2.5 hours.The results of analysis of variance table
It is bright, there is the difference of conspicuousness, A (determining alcohol), C (extraction time), D (extractions time between B factors (solvent adding amount) are horizontal
Number) have the difference without conspicuousness between factor level.General flavone optimal extract process is A2B2C2D3, i.e., 60% ethyl alcohol
Solution, 8 times of liquid volume addeds, refluxing extraction 2h are extracted 3 times, and the results of analysis of variance shows that there was no significant difference between each factor level.
So going out from produce reality with reference to the results of analysis of variance, the final process conditions of coronary disease Huoxue Capsule alcohol extracting add in 10 times of amounts for Radix Salviae Miltiorrhizae
90% ethyl alcohol, refluxing extraction 2.5 hours, the Radix Salviae Miltiorrhizae dregs of a decoction and fructus choerospondiatis, sea-buckthorn, agalloch eaglewood, kaempferia galanga, Bi roots of grass gomi herbs adds in 60%
Ethanol solution, 8 times of liquid volume addeds, refluxing extraction 2h, extract 2 times.Extraction Process of Volatile Oil condition adds in 8 times of amount water for medicinal material,
It impregnates 2 hours, extraction by steam distillation 8 hours.Volatile oil beta-cyclodextrin inclusion compound process conditions are oil: 1: 4,60 DEG C of cyclodextrin
Inclusion 2 hours.Water carries optimum process condition, every time 8 times of liquid volume addeds, refluxing extraction 2.0 hours, extracts 2 times.
6 alcohol precipitation process of embodiment is studied
Precision weighs 3 parts of sample, contains Radix Salviae Miltiorrhizae 1624g, santal 200g, dalbergia wood 408g, santal respectively in every part of sample
200g, nutmeg 608g, fructus choerospondiatis 608g, sea-buckthorn 608g, agalloch eaglewood 920g, Bi roots of grass 560g, kaempferia galanga 3052g.By optimum process condition
A3B2C2, i.e., 8 times of liquid volume addeds, refluxing extraction 2.0h are extracted 2 times every time.After the completion of being extracted by above-mentioned condition, concentration is settled to
In 50L volumetric flasks, five parts are divided into, alcohol precipitation concentration screening is carried out by table 19, using content of danshinolic acid B as Testing index.
It the results are shown in Table 19.
19 coronary disease Huoxue Capsule alcohol precipitation concentration of table screens table
The result shows that：When alcohol precipitation concentration is 60%, alcohol precipitation works well, and content of danshinolic acid B declines less.
Embodiment 7 extracts paste volume research
Precision weighs 3 parts of sample, contains Radix Salviae Miltiorrhizae 406g, santal 50g, dalbergia wood 102g, santal respectively in every part of sample
50g, nutmeg 152g, fructus choerospondiatis 152g, sea-buckthorn 152g, agalloch eaglewood 230g, Bi roots of grass 140g, kaempferia galanga 763g.Aforementioned best work is pressed respectively
Skill extract, more than ten tastes, santal, dalbergia wood, santal, four taste of nutmeg knock it is broken after using extraction by steam distillation volatile oil it is standby
With (adding in 8 times of amount water in medicinal material, impregnate 20min, refluxing extraction 8h, volatile oil extracting amount 1.3%), beta-cyclodextrin inclusion compound is (every
Milliliter volatile oil adds in the beta-cyclodextrin saturated solution containing 4g and is included 2 hours under the conditions of 60 DEG C), inclusion compound, the dregs of a decoction and water carry
Liquid is spare.Radix Salviae Miltiorrhizae ethyl alcohol extracts, and (90% ethyl alcohol of medicinal material 10 times of amounts of addition, refluxing extraction 2.5 hours) filtration, ethyl alcohol is recycled,
Relative density 1.05 (40 DEG C of surveys) is concentrated into, concentrate is spare.The Radix Salviae Miltiorrhizae dregs of a decoction and fructus choerospondiatis, sea-buckthorn, agalloch eaglewood, kaempferia galanga, the Bi roots of grass five tastes
Medicinal material extracts with 60% ethyl alcohol and (adds in 10 times of amounts, 60% ethyl alcohol, refluxing extraction 2h is extracted 2 times) filtrate and merges, filter, recycling
Ethyl alcohol is concentrated into relative density 1.05 (40 DEG C of surveys), and concentrate is spare.The alcohol extracting dregs of a decoction and santal, dalbergia wood, santal, nutmeg
Dregs of a decoction merging adds water to cook and (adds in 8 times of amount water, refluxing extraction 2h is extracted 2 times), filtration, filtrate and santal, dalbergia wood, santal,
Nutmeg steam distillation liquid merges, and being concentrated into relative density 1.06 (40 DEG C of surveys) addition ethyl alcohol makes determining alcohol stand 24 for 60%
Hour, filtration, filtrate recycling ethanol is concentrated into relative density 1.05 (40 DEG C of surveys), and concentrate merges with above-mentioned concentrate, spraying
Dry (extracting solution density is 1.05, is entered in machine cavity with the speed of 19ppm, dry at a temperature of 110-120), will be above-mentioned
Spray dried powder is mixed with Benexate Hydrochloride to uniform, calculating paste volume.It the results are shown in Table 20.
20 coronary disease Huoxue Capsule of table extracts paste volume list
The result shows that：Coronary disease Huoxue Capsule extraction paste volume average out to 20.82%.
The preparation of 8 coronary disease Huoxue Capsule of embodiment
Radix Salviae Miltiorrhizae 440g, santal 48g, dalbergia wood 98g, santal 48g, nutmeg 145g, fructus choerospondiatis 145g, sea-buckthorn 145g, agalloch eaglewood
220g, Bi roots of grass 134g, kaempferia galanga 73g.
Preparation process：Santal, dalbergia wood, santal are broken into coarse powder, nutmeg knocks broken 8 times of amount water of addition, impregnate 2 hours,
Refluxing extraction 8 hours, obtains volatile oil, and the dregs of a decoction and Aqueous extracts are spare；Every milliliter of volatile oil adds in the saturated water of the beta-cyclodextrin containing 4g
Solution includes 2 hours under the conditions of 60 DEG C, and it is spare to obtain volatile oil clathrate compound.Radix Salviae Miltiorrhizae adds 90% ethyl alcohol of 10 times of amounts to be heated to reflux carrying
It takes three times, 1.5 hours every time, extracting solution filtration, filtrate recycling ethanol and the clear cream for being concentrated into relative density 1.05 (40 DEG C of surveys),
It is spare；The Radix Salviae Miltiorrhizae dregs of a decoction and fructus choerospondiatis, sea-buckthorn, agalloch eaglewood, kaempferia galanga, the Bi roots of grass five tastes add 10 times to measure 60% ethyl alcohol heating and refluxing extraction 2 times, often
Secondary 2 hours, merge extracting solution, filtration, filtrate recycling ethanol and the clear cream for being concentrated into relative density 1.05 (40 DEG C of surveys), it is spare.
More than the ten taste dregs of a decoction merge plus 8 times amount water decoct 2 times, 2 hours every time, decocting liquid filtration, filtrate merges with volatile oil Aqueous extracts, dense
The clear cream of relative density 1.06 (40 DEG C of surveys) is reduced to, ethyl alcohol is added to make alcohol content, and standing 24 hours makes precipitation, takes supernatant up to 60%
Liquid recycles ethyl alcohol and is concentrated into the clear cream of relative density 1.05 (40 DEG C of surveys)；Above-mentioned clear cream merges, and spray drying adds in volatilization
The magnesium stearate of 1% weight of oily inclusion compound and total amount, mixing are packed into capsule, capsule are made.
Present invention combination most preferred embodiment is described, however after the above for having read the present invention, ability
Field technique personnel can appreciate the fact that make in the embodiment disclosed it is many change can also obtain it is same or similar as a result, and without departing from this
The design of invention, spirit and scope.More specifically, it is clear that some chemistry and the related reagent of physiological can replace this paper institutes public
The reagent opened and obtain same or similar result.All similar substitutions and modification it is evident to the person skilled in the art that
It is regarded as in the spirit, scope and spirit and right of the present invention, i.e., all above-mentioned such equivalent forms are all same
Sample falls within claims of the present invention limited range.The application of this process route, for the rule of " coronary disease Huoxue preparation "
Modelling produces, and the claim model that various forms of products (such as pharmaceutical preparation, food and health products) belong to the present invention is made
In enclosing.
Claims (10)
1. a kind of preparation process of Chinese medicine composition, which contains Radix Salviae Miltiorrhizae 400-480 parts by weight, santal 44-52 weights
Measure part, dalbergia wood 89-107 parts by weight, santal 44-52 parts by weight, nutmeg 132-158 parts by weight, fructus choerospondiatis 132-158 weight
Part, sea-buckthorn 132-158 parts by weight, agalloch eaglewood 200-240 parts by weight, Bi roots of grass 122-146 parts by weight, kaempferia galanga 66-80 parts by weight, technique
Step is as follows：
(1) santal, dalbergia wood, santal are broken into coarse powder, nutmeg is knocked broken addition water and impregnated, and refluxing extraction obtains volatile oil and water
Extract, it is spare；
(2) gained volatile oil is added in containing beta-cyclodextrin inclusion compound in step (1), obtains volatile oil clathrate compound, spare；
(3) Radix Salviae Miltiorrhizae adds ethyl alcohol heating and refluxing extraction, and extracting solution filtration, filtrate recycling ethanol is simultaneously condensed into clear cream, spare；
(4) step (3) the Radix Salviae Miltiorrhizae dregs of a decoction and fructus choerospondiatis, sea-buckthorn, agalloch eaglewood, kaempferia galanga, the Bi roots of grass five tastes add ethyl alcohol heating and refluxing extraction, and merging carries
Liquid is taken, is filtered, filtrate recycling ethanol is simultaneously condensed into clear cream, spare；
(5) the ten taste dregs of a decoction merging in step (1)-(4) adds water to cook, and decocting liquid filtration, filtrate merges with step (1) Aqueous extracts,
Concentration plus ethyl alcohol make precipitation, take supernatant, recycle ethyl alcohol and are condensed into clear cream, spare；
(6) clear cream obtained by step (3)-(5) merges, and spray drying adds in step (2) volatile oil clathrate compound, and mixing is to get Chinese medicine
Composition.
2. the preparation process of the Chinese medicine composition according to right wants 1, which is characterized in that contain Radix Salviae Miltiorrhizae 440g parts by weight, wingceltis
Fragrant 48g parts by weight, dalbergia wood 98g parts by weight, santal 48g parts by weight, nutmeg 145g parts by weight, fructus choerospondiatis 145g parts by weight are husky
Spine 145g parts by weight, agalloch eaglewood 220g parts by weight, Bi roots of grass 134g parts by weight, kaempferia galanga 73g parts by weight.
3. the preparation process of Chinese medicine composition according to claim 1 or 2, which is characterized in that santal, drop in step (1)
Fragrant, santal is broken into coarse powder, nutmeg knocks broken 6-10 times of addition and measures water, impregnates 1-3 hours, refluxing extraction 4-8 hours is more excellent
Be selected as santal, dalbergia wood, santal be broken into coarse powder, nutmeg knock it is broken add in 8 times amount water, impregnate 2 hours, refluxing extraction 8 hours.
4. the preparation process of Chinese medicine composition according to claim 1 or 2, which is characterized in that by step in step (2)
(1) it is small to include 1-3 under the conditions of 40~60 DEG C for the saturated aqueous solution of every milliliter of volatile oil addition beta-cyclodextrin containing 3-5g of gained in
When, the saturated aqueous solution that more preferably every milliliter of volatile oil adds in the beta-cyclodextrin containing 4g includes 2 hours under the conditions of 60 DEG C.
5. the preparation process of Chinese medicine composition according to claim 1 or 2, which is characterized in that Radix Salviae Miltiorrhizae adds 6- in step (3)
60~90% ethyl alcohol heating and refluxing extraction of 10 times of amounts 1-3 times, 1.5~2.5 hours every time, extracting solution filtration, filtrate recycling second
Alcohol and the clear cream for being concentrated into relative density 1.03~1.08 (40 DEG C of surveys), spare, more preferably Radix Salviae Miltiorrhizae adds 90% second of 10 times of amounts
Alcohol heating and refluxing extraction 3 times, 1.5 hours every time, extracting solution filtration, filtrate recycling ethanol was simultaneously concentrated into relative density 1.05 (40
DEG C survey) clear cream.
6. the preparation process of Chinese medicine composition according to claim 1 or 2, which is characterized in that by step in step (4)
(3) the Radix Salviae Miltiorrhizae dregs of a decoction and fructus choerospondiatis, sea-buckthorn, agalloch eaglewood, kaempferia galanga, the Bi roots of grass five tastes add 6-10 times to measure 40~80% ethyl alcohol heating and refluxing extractions 1
~3 times, 1.5~2.5 hours every time, merge extracting solution, filtration, filtrate recycling ethanol is simultaneously concentrated into relative density 1.03~1.08
The clear cream of (40 DEG C of surveys), more preferably step (3) the Radix Salviae Miltiorrhizae dregs of a decoction and fructus choerospondiatis, sea-buckthorn, agalloch eaglewood, kaempferia galanga, the Bi roots of grass five tastes add 10 times of amounts
60% ethyl alcohol heating and refluxing extraction 2 times 2 hours every time, merges extracting solution, filtration, and filtrate recycling ethanol is simultaneously concentrated into relatively close
The clear cream of degree 1.05 (40 DEG C of surveys).
7. the preparation process of Chinese medicine composition according to claim 1 or 2, which is characterized in that by step in step (5)
(1) the ten taste dregs of a decoction in-(4) merge plus 6-10 times is measured water and decocted 1~3 time, and 1~3 hour every time, decocting liquid filtered, filtrate and step
Suddenly (1) Aqueous extracts merge, and are concentrated into the clear cream of relative density 1.05~1.08 (40 DEG C survey), add ethyl alcohol make alcohol content up to 60~
80%, standing makes precipitation, takes supernatant, recycles ethyl alcohol and is concentrated into the clear cream of relative density 1.05~1.08 (40 DEG C of surveys)；
The ten taste dregs of a decoction more preferably in step (1)-(4) merge plus 8 times of amount water decoct 2 times, 2 hours every time, decocting liquid filtration, filtrate with
Step (1) Aqueous extracts merge, and are concentrated into the clear cream of relative density 1.06 (40 DEG C of surveys), add ethyl alcohol that alcohol content is made to be stood up to 60%
Make precipitation within 24 hours, take supernatant, recycle ethyl alcohol and be concentrated into the clear cream of relative density 1.05 (40 DEG C of surveys).
8. a kind of Chinese medicine composition made of preparation process using described in claim 1-7 any claims.
9. capsule made of Chinese medicine composition according to claim 8.
10. tablet made of Chinese medicine composition according to claim 8.
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| CN115590828A (en) * | 2022-10-12 | 2023-01-13 | 江苏海洋大学（Cn） | Preparation method of Mongolian medicine tablets |
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| CN115590828A (en) * | 2022-10-12 | 2023-01-13 | 江苏海洋大学（Cn） | Preparation method of Mongolian medicine tablets |
| CN115590828B (en) * | 2022-10-12 | 2023-09-29 | 江苏海洋大学 | Preparation method of Mongolian medicine tablet |
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Application publication date: 20180629 |