CN102973653A - Preparation method of tanshinone extract and water soluble substance thereof - Google Patents
Preparation method of tanshinone extract and water soluble substance thereof Download PDFInfo
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- CN102973653A CN102973653A CN2012105499106A CN201210549910A CN102973653A CN 102973653 A CN102973653 A CN 102973653A CN 2012105499106 A CN2012105499106 A CN 2012105499106A CN 201210549910 A CN201210549910 A CN 201210549910A CN 102973653 A CN102973653 A CN 102973653A
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- salviae miltiorrhizae
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Abstract
The invention provides a preparation method of a tanshinone extract and a water soluble substance thereof. The preparation method comprises the following steps of: extracting tanshinone by alcohol with the concentration being greater than or equal to 80%, wherein the tanshinone is segmented tanshinone or a complete material, and the mass ratio of the alcohol to the tanshinone is (5-20):1, heating and carrying out refluxing extraction for 2-5 times, combining and filtrating to obtain an extracting solution, wherein the extraction lasts for 0.25-3h every time; carrying out vacuum concentration on the extracting solution till an extract without the alcohol taste is obtained; and washing the extract by water for 5-12 times and drying under reduced pressure to obtain the tanshinone extract which contains 10.0-15.0% of tanshinone IIA and 8.0-11.0% of cryptotanshinone. The tanshinone extract prepared by the method provided by the invention has the advantages that the content of active substances is high, and the solubility of the water soluble substance of the tanshinone extract is good.
Description
[technical field]
The present invention relates to a kind of Chinese medicine extract, specifically relate to the preparation method of a kind of tanshinone extract and the hydrotrope thereof.
[background technology]
TANSHINONES is the effective ingredient that extracts from salviamiltiorrhizabung, and it is that a class has o-quinone or para-quinoid structure Diterpenes quinone ketone compounds.Because the quinones composition is reduced and is transformed into diphenols, the latter is oxidized to quinone again and plays the electronic induction effect, and tanshinone compound metabolite in vivo participates in the multiple biochemical reaction of body, as coenzyme some biochemical reaction is risen to promote or interference effect.The pharmacological action of the extract of TANSHINONES concentrates on the aspects such as antioxidation, antiviral, anti-inflammation and cardiovascular and cerebrovascular vessel, as clinically being used for the treatment of tonsillitis, otitis externa, mastitis, osteomyelitis, furuncle, carbuncle, injuring burn infection and coronary heart diseases and angina pectoris etc. outward.Do not produce drug resistance and to fastbacteria its special feature effectively especially.Because tanshinone compound is insoluble in water, absorption difference in the body, pharmacological action is difficult for giving full play to, thereby taking dose is large, thereby has influence on the compliance that patient takes medicine, and then has influence on clinical efficacy.The character of its poor solubility for a change, many researcheres are with the monomer component in the tanshinone compound such as Tanshinone I I
A, Tanshinone I etc., chemically in its molecular structure, introduce water solublity functional group, as introduce sulfonic group and make it to form sodium salt or make the Mannich dietary alkali and improve its water solublity, but its structure of these tanshinone derivatives changes, and pharmacology and function that its effect can not have been explained former tanshinone extract cure mainly to the ill.Also there are many problems not fully up to expectations in the production method of extracting at present TANSHINONES from Radix Salviae Miltiorrhizae.As application number be 200510200056.2, denomination of invention pulverizes Radix Salviae Miltiorrhizae for disclosing in " a kind of preparation method of red sage formulation and method of quality control ", alcoholic solution with 70～95% extracts, filter, merging filtrate, the pressurization Recycled ethanol also is condensed into thick paste, remove the hydrotrope with 70～90 ℃ of hot water wash, remaining extract dry is pulverized to get extract.But this method has adopted the processing step of pulverizing Radix Salviae Miltiorrhizae so that in the extract that reality obtains complicated component, the unstable or content of effective ingredient is low etc., and then has influence on the performance etc. of suiting the medicine to the illness that function cures mainly.
[summary of the invention]
For deficiency and the poorly soluble problem of TANSHINONES of preparation TANSHINONES in the prior art, the invention provides a kind of improvedly, be fit to the preparation method of the good water soluble tanshinone of the TANSHINONES extraction process of suitability for industrialized production and dissolubility.The inventor is through for many years research, unexpectedly find, directly add ethanol extraction with the material all in one piece salviamiltiorrhizabung, it is too complicated to overcome in the prior art extract component, the corresponding low problem of effective component extraction rate, and cut off the extract of the effective ingredient can obtain different proportion content, can reach the effect of the different pharmacological actions (cardiovascular and cerebrovascular vessel or anti-inflammation etc.) of TANSHINONES and different clinical indication (coronary heart disease or infection etc.).Material all in one piece of the present invention is the root after Radix Salviae Miltiorrhizae is removed earth, impurity and the position of going mouldy, or the Radix Salviae Miltiorrhizae for material all in one piece is carried out cutting, and the staple fiber ppd of the Radix Salviae Miltiorrhizae that adopts among the present invention is more than the 5cm.For achieving the above object, the present invention is by the following technical solutions:
A kind of method of extracting TANSHINONES comprises the steps:
A) with concentration 〉=80% ethanol extraction Radix Salviae Miltiorrhizae, Radix Salviae Miltiorrhizae is cutting Radix Salviae Miltiorrhizae or material all in one piece, and the mass ratio of ethanol and Radix Salviae Miltiorrhizae is 5～20:1, heating and reflux, extract, 2～5 times, and each 0.25～3h, merging filtrate gets extracting solution;
B) described extracting solution is evaporated to the extractum of distinguishing the flavor of without alcohol;
C) wash drying under reduced pressure behind the described extractum 5～12 times with water, get tanshinone extract;
Tanshinone I I in the described tanshinone extract
AContent be 10.0～15.0%, cryptotanshinone content is 8.0～11.0%.
The preparation method of a kind of tanshinone extract of the present invention, wherein, step a) in, the mass ratio that described ethanol is preferably ethanol and Radix Salviae Miltiorrhizae is 5～20:1, heating and reflux, extract, 2～5 times, each 0.25～3h, merging filtrate; The slurry amount is preferably 8～10 times in the step c); The drying under reduced pressure condition optimization is: vacuum-0.08MPa～0MPa, air pressure 0～0.5MPa, bake out temperature≤80 ℃.
A kind of method of extracting TANSHINONES of the present invention, the reflux temperature in the step a)≤80 ℃.
A kind of method of extracting TANSHINONES of the present invention, wherein, the temperature of reflux is 70～75 ℃ in the step a), constant temperature extracts.
A kind of method of extracting TANSHINONES of the present invention, wherein, Tanshinone I I in concentration of alcohol 〉=95% tanshinone extract
AContent be 13.1～15.0%, cryptotanshinone content is 10.1～11%;
A kind of method of extracting TANSHINONES of the present invention, wherein, concentration of alcohol in the step a) 〉=90%.
Tanshinone I I
AContent be 11～13%, cryptotanshinone content is 8～10%.
The invention further relates to will with said method obtain and tanshinone extract be prepared into the method for the hydrotrope.The method comprises the steps:
A) with concentration 〉=80 ethanol extraction Radix Salviae Miltiorrhizaes, wherein, Radix Salviae Miltiorrhizae is cutting Radix Salviae Miltiorrhizae or material all in one piece, and the mass ratio of ethanol and Radix Salviae Miltiorrhizae is 5～20:1, heating and reflux, extract, 2～5 times, and each 0.25～3h, merging filtrate gets extracting solution;
B) said extracted liquid is evaporated to the extractum of distinguishing the flavor of without alcohol;
C) wash drying under reduced pressure behind the described extractum 5～12 times with 8～10 times of water gagings, get tanshinone extract;
Wherein, the content of tanshinone ⅡA is 10.0～15.0%.0% in the tanshinone extract, and cryptotanshinone content is 8.0～11.0%;
D) above-mentioned tanshinone extract is dissolved in ethanol and makes the TANSHINONES lysate;
E) with the water-soluble cyclodextrin aqueous solution that gets of cyclodextrin;
F) described TANSHINONES alcoholic solution is splashed in the cyclodextrin solution, add the excessive TANSHINONES of heat evolution, get supernatant, leave standstill under 4～8 ℃ behind the 24h dryly, namely get described water soluble tanshinone or the TANSHINONES hydrotrope;
The mass ratio that feeds intake of described tanshinone extract and cyclodextrin is 1:1～20.
The preparation method of a kind of water soluble tanshinone of the present invention, wherein, the mass ratio that feeds intake of tanshinone extract and cyclodextrin is 1:6.
The preparation method of a kind of water soluble tanshinone of the present invention, wherein, cyclodextrin is selected from alpha-cyclodextrin, beta-schardinger dextrin-and gamma-cyclodextrin.
Radix Salviae Miltiorrhizae extract is by Tanshinone I I contained in the Radix Salviae Miltiorrhizae
A, the mixture that forms of the multiple phenolic acid compounds such as the multiple phenanthrenequione class such as cryptotanshinone, Tanshinone I, miltirone and salvianolic acid A, salvianolic acid B, rosmarinic acid, shikonin.The present invention is mainly with Tanshinone I I
AWith cryptotanshinone be index, the processing step of taking is fit to industrialized great production, and Tanshinone I I in the prepared tanshinone extract
AContent be 8～15.0%, cryptotanshinone content is 5～11.0%; All improve by dissolution and the dissolubility that adopts cyclodextrin of the present invention to wrap up the TANSHINONES that makes.The product that the method is produced, it is poor thoroughly to change in the prior art TANSHINONES drug solubility, the shortcoming of industrialized producing technology complexity.
With the prior art ratio, the present invention adopts improves one's methods, and for industrialized great production, does not need to carry out crushing process and has both simplified technique, has shortened extraction time again, so that preparation technology is more suitable for the needs of suitability for industrialized production.With method of the present invention obtain and tanshinone extract also avoided simultaneously the too complicated problem of extract composition, and improved content and extraction ratio that active ingredient is cryptotanshinone etc.The tanshinone extract that makes is carried out the enclose of cyclodextrin, obtained the clathrate of the TANSHINONES cyclodextrin of excellent performance, its water solublity is improved greatly, absorb and improve, taking dose can be the order of magnitude to be reduced, and then has improved medicine stability and clinical efficacy, reduced poisonous side effect of medicine, has reduced the medicinal raw material consumption, natural resources is rationally used, saved total production cost.The preparation technology of water soluble tanshinone is easy, and the needed raw material cost is low, uses equipment to be basic condition indispensable in the pharmaceuticals industry.Product efficiency is high, and preferably repeatability is arranged.
The tanshinone extract that adopts method preparation provided by the invention is carried out assay:
TANSHINONES and Tanshinone I I
AMensuration: high performance liquid chromatography.
Chromatographic condition and system suitability: take octadecylsilane chemically bonded silica as filler; Take acetonitrile-water (60:40) as mobile phase; The detection wavelength is 269nm.Number of theoretical plate is pressed cryptotanshinone, Tanshinone I I
AThe peak calculates all should be not less than 2000.
The preparation of reference substance solution: get cryptotanshinone reference substance, Tanshinone I I
AReference substance is an amount of, and is accurately weighed, puts respectively in the brown measuring bottle, adds ethanol and makes every 1ml and contain cryptotanshinone 50 μ g, contain Tanshinone I I
AThe solution of 60 μ g, and get final product.
The preparation of need testing solution: get this product, porphyrize is got about 30mg, accurately weighed, put in the tool plug conical flask the accurate ethanol 50ml that adds, close plug, weighed weight, supersound process (power 250W, frequency 50kHz) 10 minutes, lets cool, more weighed weight, supply the weight that subtracts mistake with ethanol, shake up, filter, get subsequent filtrate, and get final product.
Algoscopy: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
Concrete experimental data: the Tanshinone I I that measures each sample among the embodiment 1
AContent with cryptotanshinone the results are shown in Table 1.
Table 1 effective component extraction rate content (%)
| ? | Tanshinone I I A | Cryptotanshinone | ? | Tanshinone I I A | Cryptotanshinone |
| Sample 1 | 10.2% | 8.4% | Sample 10 | 13.8% | 9.9% |
| Sample 2 | 10.0% | 8.2% | Sample 11 | 12.7% | 9.4% |
| Sample 3 | 10.6% | 9.2% | Sample 12 | 13.5% | 10.6% |
| Sample 4 | 13.8% | 10.5% | Sample 13 | 12.4% | 10.0% |
| Sample 5 | 12.9% | 10.3% | Sample 14 | 13.9% | 10.8% |
| Sample 6 | 13.2% | 10.1% | Sample 15 | 11.6% | 9.4% |
| Sample 7 | 12.8% | 9.6% | Sample 16 | 10.4% | 9.4% |
| Sample 8 | 13.6% | 10.4% | Sample 17 | 10.9% | 9.0% |
| Sample 9 | 10.9% | 8.6% | ? | ? | ? |
[specific embodiment]
Embodiment 1 preparation tanshinone extract
Sample 1
Get 80% ethanol that clean material Radix Salviae Miltiorrhizae material all in one piece adds 8 times of amounts of Radix Salviae Miltiorrhizae gross weight, heated constant temperature, 80 ℃ of reflux, extract, 3 times, 1.5h.Merge 3 times and extract filtrate, be evaporated to without the alcohol flavor, wash extractum 9 times with 90 ℃ of purified water of 8 times of amounts, under-0.08MPa, bake out temperature is 75 ℃, gets tanshinone extract.
Sample 2
Get 85% ethanol that clean material Radix Salviae Miltiorrhizae material all in one piece adds 6 times of amounts of Radix Salviae Miltiorrhizae gross weight, 75 ℃ of reflux, extract, of heated constant temperature 3 times, each 0.5h.Merge 3 times and extract filtrate, be evaporated to without the alcohol flavor, wash extractum 10 times with 90 ℃ of purified water of 9 times of amounts, under-0.08MPa, bake out temperature is 75 ℃, gets tanshinone extract.
Sample 3
Get clean material Radix Salviae Miltiorrhizae material all in one piece, add 90% ethanol of 5 times of amounts of Radix Salviae Miltiorrhizae gross weight, 70 ℃ of reflux, extract, of heated constant temperature 3 times, 1h refluxes at every turn.Merge 3 times and extract filtrate, be evaporated to without the alcohol flavor, wash extractum 10 times with 90 ℃ of purified water of 10 times of amounts, under-0.08MPa, bake out temperature is 78 ℃, gets tanshinone extract.
Sample 4
Getting clean material Radix Salviae Miltiorrhizae shearing length is 8cm, adds 95% ethanol of 10 times of amounts of Radix Salviae Miltiorrhizae gross weight, 75 ℃ of reflux, extract, of heated constant temperature 3 times, and 1.5h refluxes at every turn.Merge 3 times and extract filtrate, be evaporated to without the alcohol flavor, wash extractum 9 times with 90 ℃ of purified water of 8 times of amounts, under-0.08MPa, bake out temperature is 75 ℃, gets tanshinone extract.
Sample 5
Get 95% ethanol that clean material Radix Salviae Miltiorrhizae material all in one piece adds 6 times of amounts of Radix Salviae Miltiorrhizae gross weight, 75 ℃ of reflux, extract, of heated constant temperature 2 times, 2h refluxes at every turn.Merge 2 times and extract filtrate, be evaporated to without the alcohol flavor, wash extractum 9 times with 90 ℃ of purified water of 8 times of amounts, under-0.08MPa, bake out temperature is 78 ℃, gets tanshinone extract.
Sample 6
Get 95% ethanol that clean material Radix Salviae Miltiorrhizae material all in one piece adds 8 times of amounts of Radix Salviae Miltiorrhizae gross weight, 75 ℃ of reflux, extract, of heated constant temperature 2 times, 1h refluxes at every turn.Merge 2 times and extract filtrate, be evaporated to without the alcohol flavor, wash extractum 10 times with 90 ℃ of purified water of 9 times of amounts, under-0.09MPa, bake out temperature is 75 ℃, gets tanshinone extract.
Sample 7
Get clean material Radix Salviae Miltiorrhizae material all in one piece, 75 ℃ of reflux, extract, of heated constant temperature, for the first time with 95% alcohol reflux 3h of 6 times of amounts, 92% alcohol reflux of 8 times of amounts of second and third time usefulness, 1.5h refluxes at every turn.Merge 3 times and extract filtrate, be evaporated to without the alcohol flavor, wash extractum 9 times with 90 ℃ of purified water of 8 times of amounts, under-0.08MPa, bake out temperature is 75 ℃, gets tanshinone extract.
Sample 8
Get clean material Radix Salviae Miltiorrhizae material all in one piece, 75 ℃ of reflux, extract, of heated constant temperature, for the first time with 8 times of amounts, 95% alcohol reflux 15min, with 93% alcohol reflux of 6 times of amounts, 1.5h refluxes at every turn for the second time.Merge 2 times and extract filtrate, be evaporated to without the alcohol flavor, wash extractum 9 times with 90 ℃ of purified water of 8 times of amounts, under 0MPa, bake out temperature is 75 ℃, gets tanshinone extract.
Sample 9
Get clean material Radix Salviae Miltiorrhizae material all in one piece, 78 ℃ of reflux, extract, of heated constant temperature, for the first time with 90% alcohol reflux 3h of 8 times of amounts, second and third time 92% alcohol reflux, 1.5h refluxes at every turn.Merge 3 times and extract filtrate, be evaporated to without the alcohol flavor, wash extractum 9 times with 90 ℃ of purified water of 8 times of amounts, under-0.09MPa, bake out temperature is 75 ℃, gets tanshinone extract.
Sample 10
Get clean material Radix Salviae Miltiorrhizae material all in one piece, 75 ℃ of reflux, extract, of heated constant temperature, for the first time with 95% alcohol reflux 3h of 10 times of amounts, 92% alcohol reflux of 8 times of amounts of second and third time usefulness, 1.5h refluxes at every turn.Merge 3 times and extract filtrate, be evaporated to without the alcohol flavor, wash extractum 9 times with 90 ℃ of purified water of 8 times of amounts, under-0.08MPa, bake out temperature is 75 ℃, gets tanshinone extract.
Sample 11
Get 95% ethanol that clean material Radix Salviae Miltiorrhizae material all in one piece adds 10 times of amounts of Radix Salviae Miltiorrhizae gross weight, 70 ℃ of reflux, extract, of heated constant temperature 3 times, 1.5h refluxes at every turn.Merge 3 times and extract filtrate, be evaporated to without the alcohol flavor, wash extractum 9 times with 90 ℃ of purified water of 10 times of amounts, under-0.08MPa, bake out temperature is 75 ℃, gets tanshinone extract.
Sample 12
Get 95% ethanol that clean material Radix Salviae Miltiorrhizae material all in one piece adds 9 times of amounts of Radix Salviae Miltiorrhizae gross weight, 75 ℃ of reflux, extract, of heated constant temperature 3 times, 3h refluxes at every turn.Merge 3 times and extract filtrate, be evaporated to without the alcohol flavor, wash extractum 9 times with 90 ℃ of purified water of 8 times of amounts, under 0MPa, bake out temperature is 75 ℃, gets tanshinone extract.
Sample 13
Get clean material Radix Salviae Miltiorrhizae material all in one piece, 75 ℃ of reflux, extract, of heated constant temperature, for the first time with 98% alcohol reflux 3h of 8 times of amounts, second and third time 95% alcohol reflux, 1.5h refluxes at every turn.Merge 3 times and extract filtrate, be evaporated to without the alcohol flavor, wash extractum 9 times with 90 ℃ of purified water of 8 times of amounts, under-0.08MPa, bake out temperature is 75 ℃, gets tanshinone extract.
Sample 14
Get 98% ethanol that clean material Radix Salviae Miltiorrhizae material all in one piece adds 8 times of amounts of Radix Salviae Miltiorrhizae gross weight, 75 ℃ of reflux, extract, of heated constant temperature 3 times, 3h refluxes at every turn.Merge 3 times and extract filtrate, be evaporated to without the alcohol flavor, wash extractum 8 times with 90 ℃ of purified water of 9 times of amounts, under 0MPa, bake out temperature is 75 ℃, gets tanshinone extract.
Sample 15
Get clean material Radix Salviae Miltiorrhizae material all in one piece, 75 ℃ of reflux, extract, of heated constant temperature, for the first time with 95% alcohol reflux 3h of 9 times of amounts, second and third time 85% alcohol reflux, 1.5h refluxes at every turn.Merge 3 times and extract filtrate, be evaporated to without the alcohol flavor, wash extractum 9 times with 90 ℃ of purified water of 8 times of amounts, under-0.08MPa, bake out temperature is 75 ℃, gets tanshinone extract.
Sample 16
Get clean material Radix Salviae Miltiorrhizae material all in one piece, 75 ℃ of reflux, extract, of heated constant temperature, for the first time with 95% alcohol reflux 3h, second and third time 85% alcohol reflux, 1.5h refluxes at every turn.Merge 3 times and extract filtrate, be evaporated to without the alcohol flavor, wash extractum 9 times with 90 ℃ of purified water of 8 times of amounts, under-0.08MPa, bake out temperature is 75 ℃, gets tanshinone extract.
Sample 17
Get clean material Radix Salviae Miltiorrhizae material all in one piece, 75 ℃ of reflux, extract, of heated constant temperature, for the first time with 95% alcohol reflux 3h of 8 times of amounts, second and third time 80% alcohol reflux, 1.5h refluxes at every turn.Merge 3 times and extract filtrate, be evaporated to without the alcohol flavor, wash extractum 9 times with 90 ℃ of purified water of 8 times of amounts, under-0.08MPa, bake out temperature is 75 ℃, gets tanshinone extract.Embodiment 2
Get 95% ethanol that clean material Radix Salviae Miltiorrhizae material all in one piece adds 8 times of amounts of Radix Salviae Miltiorrhizae gross weight, 75 ℃ of reflux, extract, of heated constant temperature, for the first time with 95% alcohol reflux 3h, 92% alcohol reflux of 6 times of amounts of second and third time usefulness, 1.5h refluxes at every turn.Merge 3 times and extract filtrate, artistic skills are concentrated to be without the alcohol flavor, washs extractum 9 times with 90 ℃ of purified water of 8 times of amounts, and under-0.08MPa, bake out temperature is 75 ℃, gets tanshinone extract.
Wherein tanshinone ⅡA content is 13.5%, and cryptotanshinone content is 10.2%.
Embodiment 2
Get clean material Radix Salviae Miltiorrhizae material all in one piece, add 95% ethanol of 8 times of amounts of Radix Salviae Miltiorrhizae gross weight for the first time, the heated constant temperature reflux cycle, reflux, extract, 15min adds 91% alcohol reflux 1h for the second time.Merge 2 times and extract filtrate, be evaporated to without the alcohol flavor, wash extractum 9 times with 90 ℃ of purified water of 8 times of amounts, under-0.08MPa, bake out temperature is 75 ℃, gets tanshinone extract.
Wherein tanshinone ⅡA content is 13.1%, and cryptotanshinone content is 10.1%.
Embodiment 3
Get clean material Radix Salviae Miltiorrhizae material all in one piece, add 95% ethanol of 6 times of amounts of medical material, keep little backflow 3h that boils, get filtrate; Use again the 90% ethanol extraction medicinal residues 2 times of 6 times of amounts of medical material, keep little backflow 90min that boils, merge 3 times extracting solution, the concentrating under reduced pressure Recycled ethanol, extractum is waved residual to the greatest extent alcohol, washs drying under reduced pressure 9 times with 90 ℃ of purified water of 8 times of amounts, under-the 0.08MPa, bake out temperature is 75 ℃, gets tanshinone extract.
Wherein tanshinone ⅡA content is 13.2%, and cryptotanshinone content is 10.4%.
Embodiment 4 preparation water soluble tanshinones
The tanshinone extract of getting the preparation of any embodiment among the embodiment 1～3 is dissolved in ethanol and makes the TANSHINONES lysate;
Described TANSHINONES alcoholic solution is splashed in the cyclodextrin solution of proportioning as described in Table 3, add the excessive TANSHINONES of heat evolution, get supernatant, leave standstill under 4 ℃ behind the 24h dryly, get described water soluble tanshinone.
Embodiment 5 TANSHINONES are proved conclusively by beta-cyclodextrin inclusion compound
The TANSHINONES Benexate Hydrochloride silica gel G tlc analysis that utilizes soluble in water that the tanshinone extract that the present invention is made makes with ether dissolution, with the present invention, developing solvent is high point petroleum ether (60～90 ℃), TANSHINONES can be launched as a result, the TANSHINONES Benexate Hydrochloride still is parked in initial point and does not launch, prove TANSHINONES by enclose in the beta-schardinger dextrin-molecule.
Embodiment 5
Get the Radix Salviae Miltiorrhizae of same batch, choose cutting and material all in one piece Radix Salviae Miltiorrhizae, according to preparation technology provided by the invention, under identical extraction conditions, carry out repeated trials 2 times, average, the results are shown in Table 2.
Table 2 Radix Salviae Miltiorrhizae staple fiber ppd is on the impact of TANSHINONES extraction ratio
Clean material Radix Salviae Miltiorrhizae of the present invention is the medicinal part of the Radix Salviae Miltiorrhizae removing silt, impurity and go mouldy, namely gets the root of Radix Salviae Miltiorrhizae.
The proportioning of cyclodextrin in table 3 water soluble tanshinone
| ? | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | 11 | 12 | 13 | 14 | 15 | 16 | 17 |
| Alpha-cyclodextrin | 6 | 8 | 0 | 2 | 0 | 0 | 4 | 3 | 4.5 | 2 | 3 | 3 | 5 | 0 | 0 | 4 | 7 |
| Beta-schardinger dextrin- | 0 | 0 | 9 | 5 | 9 | 0 | 2 | 5 | 4.5 | 2 | 0 | 0 | 2 | 5 | 4 | 4 | 5 |
| Gamma-cyclodextrin | 0 | 0 | 0 | 2 | 0 | 6 | 1 | 0 | 0 | 2 | 4 | 6 | 1 | 5 | 5 | 4 | 2 |
| The consumption of cyclodextrin | 6 | 8 | 9 | 10 | 9 | 6 | 7 | 8 | 9 | 6 | 7 | 9 | 8 | 10 | 9 | 12 | 14 |
The consumption of cyclodextrin is alpha-cyclodextrin, beta-schardinger dextrin-and gamma-cyclodextrin consumption sum.
The tanshinone extract that finally makes with sample 4 among the embodiment 1 is example, get 1.25 kilograms of TANSHINONES, be dissolved in 95% ethanol 13 liters, press the proportioning of cyclodextrin in the table 3, cyclodextrin is dissolved in 30 kilograms of the pure water, the mass ratio of tanshinone extract and cyclodextrin is 1:6, be 011414367 with reference to application number, name is called the preparation technology of " preparation method of water soluble tanshinone ", the water soluble tanshinone that makes compares with the tanshinone extract of not selecting cyclodextrin to carry out enclose, dissolution and dissolution rate significantly improve, and water soluble tanshinone dissolubility in the environment of simulation gastric acid that the present invention makes also is improved.
Claims (10)
1. a method of extracting TANSHINONES comprises the steps:
A) with concentration 〉=80% ethanol extraction Radix Salviae Miltiorrhizae, described Radix Salviae Miltiorrhizae is cutting Radix Salviae Miltiorrhizae or material all in one piece, and the mass ratio of described ethanol and Radix Salviae Miltiorrhizae is 5～20:1, heating and reflux, extract, 2～5 times, and each 0.25～3h, merging filtrate gets extracting solution;
B) described extracting solution is evaporated to the extractum of distinguishing the flavor of without alcohol;
C) wash drying under reduced pressure behind the described extractum 5～12 times with 8～10 times of water gagings, get tanshinone extract;
The content of tanshinone ⅡA is 10.0～15.0% in the described tanshinone extract, and cryptotanshinone content is 8.0～11.0%.
2. a kind of method of extracting TANSHINONES as claimed in claim 1 is characterized in that the temperature of reflux described in the step a)≤80 ℃;
The temperature of reflux described in the described step a) is 70～75 ℃, and constant temperature extracts.
3. a kind of method of extracting TANSHINONES as claimed in claim 1 is characterized in that the drying under reduced pressure condition is in the described step c): vacuum-0.08MPa～0MPa, air pressure 0～0.5MPa, bake out temperature≤80 ℃.
4. a kind of method of extracting TANSHINONES as claimed in claim 1 is characterized in that Tanshinone I I in the described tanshinone extract
AContent be 13.1～15.0%, cryptotanshinone content is 10.1～11%.
5. a kind of method of extracting TANSHINONES as claimed in claim 1 is characterized in that concentration of alcohol in the described step a) 〉=90%.
6. the preparation method of a water soluble tanshinone, described method comprises the steps:
A) with concentration 〉=80% ethanol extraction Radix Salviae Miltiorrhizae, described Radix Salviae Miltiorrhizae is cutting Radix Salviae Miltiorrhizae or material all in one piece, and the mass ratio of described ethanol and Radix Salviae Miltiorrhizae is 5～20:1, heating and reflux, extract, 2～5 times, and each 0.25～3h, merging filtrate gets extracting solution;
B) described extracting solution is evaporated to the extractum of distinguishing the flavor of without alcohol;
C) wash drying under reduced pressure behind the described extractum 5～12 times with 8～10 times of water gagings, get tanshinone extract;
Tanshinone I I in the described tanshinone extract
AContent be 10.0～15.0%, cryptotanshinone content is 8.0～11.0%;
D) above-mentioned tanshinone extract is dissolved in ethanol and makes the TANSHINONES alcoholic solution;
E) with the water-soluble cyclodextrin aqueous solution that gets of cyclodextrin;
F) described TANSHINONES alcoholic solution is splashed in the cyclodextrin solution, add the excessive TANSHINONES of heat evolution, get supernatant, leave standstill under 4～8 ℃ behind the 24h dryly, namely get described water soluble tanshinone;
The mass ratio that feeds intake of described tanshinone extract and cyclodextrin is 1:1～20.
7. the preparation method of a kind of water soluble tanshinone as claimed in claim 6 is characterized in that the mass ratio that feeds intake of described tanshinone extract and cyclodextrin is 1:6.
8. the preparation method of a kind of water soluble tanshinone as claimed in claim 6 is characterized in that described cyclodextrin is selected from alpha-cyclodextrin, beta-schardinger dextrin-and gamma-cyclodextrin.
9. the preparation method of a kind of water soluble tanshinone as claimed in claim 6 is characterized in that described cyclodextrin is beta-schardinger dextrin-.
10. the as claimed in claim 6 application of the tanshinone extract that makes of method in preparation treatment cardiovascular and cerebrovascular disease and antibacterial-anti-inflammatory drug.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106265487A (en) * | 2016-08-31 | 2017-01-04 | 上海新亚药业高邮有限公司 | A kind of TANSHINONES emulsifiable paste process of preparing |
| CN108663337A (en) * | 2018-02-12 | 2018-10-16 | 广州白云山和记黄埔中药有限公司 | A kind of method and its application measuring tanshinone component |
Citations (2)
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|---|---|---|---|---|
| CN1410068A (en) * | 2001-09-25 | 2003-04-16 | 房其年 | Preparation method of water soluble tanshinone |
| CN1810272A (en) * | 2005-01-25 | 2006-08-02 | 黄伟民 | Prepn process of red sage prepn and its quality control method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1410068A (en) * | 2001-09-25 | 2003-04-16 | 房其年 | Preparation method of water soluble tanshinone |
| CN1810272A (en) * | 2005-01-25 | 2006-08-02 | 黄伟民 | Prepn process of red sage prepn and its quality control method |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106265487A (en) * | 2016-08-31 | 2017-01-04 | 上海新亚药业高邮有限公司 | A kind of TANSHINONES emulsifiable paste process of preparing |
| CN108663337A (en) * | 2018-02-12 | 2018-10-16 | 广州白云山和记黄埔中药有限公司 | A kind of method and its application measuring tanshinone component |
| CN108663337B (en) * | 2018-02-12 | 2021-07-13 | 广州白云山和记黄埔中药有限公司 | Method for measuring tanshinone component and application thereof |
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