CN102885985A - Preparation method and application of rhizoma gastrodiae and rhizoma chuanxiong compound extract - Google Patents
Preparation method and application of rhizoma gastrodiae and rhizoma chuanxiong compound extract Download PDFInfo
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Abstract
The invention relates to a preparation method of a rhizoma gastrodiae and rhizoma chuanxiong compound extract, and the preparation method comprises the following steps of: mixing raw medicines, namely rhizoma gastrodiae and rhizoma chuanxiong at the ratio of (1:4)-(2:1) and smashing; extracting the smashed raw medicines for 2-3 times by using 30-95% of ethanol (by volume) with the weight 6-18 times that of the raw medicines through the method of percolation or heating reflux; concentrating the obtained extract, removing impurities and filtering; adsorbing the filtrate through a macroporous resin column or a silicagel column, eluting the filtrate by using the 30-95% of ethanol (by volume) and collecting the eluent; and drying the eluent after recovering the solvent to obtain the rhizoma gastrodiae and rhizoma chuanxiong compound extract. The method disclosed by the invention is simplified in process and low in cost and the obtained extract has the characteristics of exact curative effect, clear material base, stable and controllable quality, convenience in use and the like.
Description
Technical field
The present invention relates to the preparation method of a kind of Rhizoma Gastrodiae, Rhizoma Chuanxiong compound extract, and the application in the medicine of the diseases such as preparation treatment vascular dementia, migraine, medical technical field belonged to.
Background technology
Gastrodia elata is the dry tuber of orchid Rhizoma Gastrodiae Gastrodia elata Bl., is rare Chinese medicine commonly used.Its nature and flavor are sweet, flat, return Liver Channel, have the effect of suppressing the hyperactive liver to relieve the wind syndrome relieving convulsion.Clinical dizzy be used to having a headache, numb limbs and tense tendons, infantile convulsion, epilepsy clonus, the diseases such as tetanus.Rhizoma Gastrodiae contains gastrodine, vanillyl alcohol, vanillin, succinic acid, cupreol, vitamin A sample material, glycoside, alkaloid, lymphatic temperament and gastrodia elata polysaccharide etc., and wherein gastrodine is main component.Gastrodine has preferably calmness and soporific function, and neurasthenia, insomnia, headache symptom are had mitigation.Gastrodia elata can be treated dizzy, the numb limbs and tense tendons of pain, frightened pain is twitched.
Chuanxiong is the dry rhizome of samphire Rhizoma Chuanxiong Ligusticum chuanxiong Hort., has the effect of blood-activating and qi-promoting, wind-expelling pain-stopping.The active component of Rhizoma Chuanxiong has the alkaloids take ligustrazine as representative, the organic acid take ferulic acid as representative, the phthalide-type take ligustilide, cnidium lactone as representative.Modern clinic is usually used in treating the disease of the aspects such as cardiovascular and cerebrovascular vessel, gynecological.
Chinese medicine is the valuable medical resource of China's uniqueness, has accumulated abundant theory and practice experience in the treatment of the diseases such as vascular dementia.The Overall View of Chinese medicine compound and multi-target effect are used for transferring homeostasis, the self-reparing capability of body by multicomponent, multipath, multi-level comprehensive coordination, thereby reach the effect for the treatment of disease.The Chinese medicine compound material base of bringing into play simultaneously drug action has again the complexity of composition and the complexity of relation.Therefore the research of Chinese medicine compound material base has complexity and difficulties.At present in the production chain of Chinese medicine, extraction, separation, exquisite effective active position or components group and the guardian technique bottleneck that their quality control level has been become modernization of industry of Chinese materia medica.Solve these technical bottlenecks and fall behind for changing present Chinese herbal medicine industry production technology, enhancing the competitiveness to wait has real meaning.
Summary of the invention
Main purpose of the present invention is to provide the preparation method of a kind of Rhizoma Gastrodiae, Rhizoma Chuanxiong compound extract, and the application of described active component in the medicine of the diseases such as preparation treatment and prevention vascular dementia, migraine.
For achieving the above object, the present invention takes following technical scheme:
A kind of preparation method of Rhizoma Gastrodiae Rhizoma Chuanxiong compound extract is characterized in that,
A. the material medicine with Rhizoma Gastrodiae and Rhizoma Chuanxiong mixes rear the pulverizing according to the weight ratio of 1:4～2:1;
B. the material medicine after extracting pulverizing with the 6-18 times of ethanol to the percent by volume 30～95% of described material medicine weight by the mode of percolation or reflux 2-3 time;
C. the extracting solution that obtains of step b is after concentrated, and remove impurity filters;
D. filtrate with the ethanol elution of percent by volume 30～95%, is collected eluent by macroporous resin column or silicagel column absorption;
E. dry behind the eluent recovery solvent, namely obtain described Rhizoma Gastrodiae Rhizoma Chuanxiong compound extract.
Aforesaid preparation method, it is characterized in that, the material medicine of described Rhizoma Gastrodiae is the dry tuber of orchid Rhizoma Gastrodiae Gastrodia elata Bl., and the material medicine of described Rhizoma Chuanxiong is the dry rhizome of samphire Rhizoma Chuanxiong Ligusticum chuanxiong Hort..
Aforesaid preparation method, among the step b, when adopting the percolation mode to extract, the preferred percolation time is 12 ~ 48h.
Aforesaid preparation method, among the step b, when adopting the percolation mode to extract, the preferred percolation time is 16 ~ 32h.
Aforesaid preparation method, among the step b, when adopting the percolation mode to extract, the most preferred percolation time is 18 ~ 24h.
Aforesaid preparation method, among the step b, when adopting the reflux mode to extract, preferred return time is 1 ~ 3h.
Aforesaid preparation method among the step b, when adopting the reflux mode to extract, most preferably is reflux, extract, twice, and the time is the 1.5h first time, is 1h for the second time.
Aforesaid preparation method, preferably, among the step b, used concentration of alcohol is percent by volume 50 ~ 80%.
Aforesaid preparation method, most preferably, among the step b, used concentration of alcohol is percent by volume 70%.
Aforesaid preparation method, preferably, in the steps d, used concentration of alcohol is percent by volume 40 ~ 70%.
Aforesaid preparation method, most preferably, in the steps d, used concentration of alcohol is percent by volume 50%.
Aforesaid preparation method, preferably, described macroporous resin is one or more in AB-8, D101, D4020, D101C, NKA-9, HPD-450 and the ADS-F8 type adsorbent resin.
Aforesaid preparation method, more preferably, the model of described macroporous resin is AB-8, D101 or D101C.
Aforesaid preparation method, most preferably, the model of described macroporous resin is AB-8.
The application in preparation treatment and prevention vascular dementia or migrainous medicine of the Rhizoma Gastrodiae that aforesaid preparation method makes and Rhizoma Chuanxiong extract.
Aforesaid application is characterized in that, described treatment and prevention vascular dementia or migrainous medicine are comprised of acceptable adjuvant on described Rhizoma Gastrodiae and Rhizoma Chuanxiong extract and the pharmaceutics.
Aforesaid application is characterized in that, the dosage form of described treatment and prevention vascular dementia or migrainous medicine comprises: drop pill, the watered pill, capsule, tablet, soft capsule, slow releasing capsule, slow releasing tablet, slow-releasing microcapsule, injection and injectable powder.
Aforesaid application is characterized in that, the gastrodin content in described treatment and prevention vascular dementia or the migrainous medicine must not be lower than 0.1%, and the content of ligustrazine must not be lower than 0.1%, and the content of ferulic acid must not be lower than 0.1%.
Beneficial effect of the present invention is:
The invention provides a kind of preparation method that contains the extract of Rhizoma Gastrodiae, Rhizoma Chuanxiong compound active composition, and the application of described extract in the medicine of the diseases such as preparation treatment and prevention vascular dementia, migraine, its work simplification, with low cost, meet the characteristic of Chinese medicine tradition medication Overall View, and have the characteristics such as determined curative effect, material base be clear and definite, stable and controllable for quality, easy to use.
Description of drawings
Fig. 1 is effective ingredient ligustrazine of the present invention, gastrodine and the leakage plot of ferulic acid on the AB-8 resin.
Fig. 2 is effective ingredient ligustrazine of the present invention, gastrodine and the elution curve of ferulic acid on the AB-8 resin.
The specific embodiment
Basic ideas of the present invention are: after a certain proportion of Rhizoma Gastrodiae and Ligusticum chuanxiong Hort are ground into coarse powder, and take ethanol as solvent, the whole active materials that extracts Rhizoma Gastrodiae and Rhizoma Chuanxiong.
The ratio that the ratio of Rhizoma Gastrodiae, Rhizoma Chuanxiong is can be according to the different choice for the treatment of disease different, it is 1:1～2:1(weight ratio that vascular dementia can be selected the ratio of Rhizoma Gastrodiae, Rhizoma Chuanxiong, lower with), it is 1:2～1:4 that migraine can be selected the ratio of Rhizoma Gastrodiae, Rhizoma Chuanxiong.
Be determined by experiment, concentration of alcohol should be 30～95%(percent by volume, and is lower same), the ethanol consumption is 6-18 times of quality of medicinal material, and the percolation time is 12 ~ 48h, and the time of alcohol reflux is 1 ~ 3h.
Determine that according to single factor and orthogonal experiment preferred concentration of alcohol is 50～80%, optimum is 70%; Preferred ethanol consumption be quality of medicinal material 8-16 doubly, optimum is 12 times; If adopt the percolation mode to extract, the preferred percolation time is 16～32h, and optimum is 18 ~ 24h; If adopt the mode of reflux to extract, optimum is reflux, extract, twice, and the time is 1.5 hours for the first time, is 1h for the second time.
After the filtrate merging, concentrating, filter, hold over night, afterwards remove impurity, filtration contain crude drug 0.5 ~ 1.0g/mL in the filtrate.
The filtrate of above-mentioned gained is passed through macroporous resin or silicagel column, use again ethanol elution, collect eluent, reclaim solvent and dry, namely obtain the Rhizoma Gastrodiae Rhizoma Chuanxiong extract.The used concentration of alcohol of eluting is 30～95%, is preferably 40～70%, most preferably is 50%.
The model of macroporous resin can be one or more in AB-8, D101, D4020, D101C, NKA-9, HPD-450, the ADS-F8 type adsorbent resin, is preferably AB-8, D101 or D101C.
Adopt AB-8, D101 resin to test, pass through Staticadsorption experiment, adsorbance is conciliate adsorbance investigate, content assaying method is with reference to 2010 editions " ultraviolet-spectrophotography in the Chinese pharmacopoeia appendix, the final selected purifying process that are fit to Rhizoma Gastrodiae Rhizoma Chuanxiong compound recipe.Conciliate adsorption experiment by dynamic adsorption, dynamic adsorption and the desorption attached kinetics of heterogeneity in the Rhizoma Gastrodiae Rhizoma Chuanxiong extracting solution on macroporous resin is studied, selected AB-8 is optimum resin.
Eluent by the macroporous resin eluting carries out ethanol recovery and concentrated, and concentrated solution carries out drying with vacuum drying, microwave drying or spraying, collects xeraphium, namely gets the active component of Rhizoma Gastrodiae, Rhizoma Chuanxiong.
Active component of the present invention can be for the preparation of vascular dementia and migrainous medicine, this active component and pharmaceutical carrier can be made into the various dosage forms on the pharmaceutics, the dispersity of the active component of Rhizoma Gastrodiae, Rhizoma Chuanxiong in preparation can be liquid, also can be solid, the route of administration of calcium preparation can be oral, injection and topical.
(1) is ground into coarse powder after the weight ratio mixing of material medicine according to 1:3 with Rhizoma Gastrodiae and Rhizoma Chuanxiong;
(2) with 12 times to material medicine weight 70% alcohol heating reflux extract twice, the time be 1.5h for the first time, be 1h the second time;
(3) merging filtrate filters remove impurity, and Recycled ethanol also is concentrated into and contains crude drug 0.5 ~ 1.0g/mL in the filtrate;
(4) filtrate is crossed the AB-8 macroporous resin column, uses 50% ethanol elution, reclaims eluent, behind the Recycled ethanol, concentrated, vacuum drying, obtains Rhizoma Gastrodiae Rhizoma Chuanxiong extract of the present invention;
(5) take extract obtained as effective ingredient, be aided with corresponding adjuvant on the pharmaceutics, can be prepared into the patent medicine such as Rhizoma Gastrodiae Rhizoma Chuanxiong compound dripping pill, the watered pill, capsule, tablet, soft capsule, slow releasing capsule, slow releasing tablet, slow-releasing microcapsule, injection and/or injectable powder.
(1) pretreatment of macroporous resin
Get respectively a certain amount of D101 type, AB-8 type macroporous adsorbent resin, with an amount of 95% soak with ethanol 24h, make its abundant swelling.Emitting immersion, with the ethanol elution of percentage by volume 95%, is that 1:2 mixes and do not produce muddiness to effluent and distilled water volume ratio.Use distilled water instead and be eluted to without the alcohol flavor, place for subsequent use.
(2) static adsorption and desorption experiment
Each 2g of wet macroporous resin that precision takes by weighing above-mentioned two kinds of models after pretreatment puts in the 50mL conical flask, adds the Rhizoma Gastrodiae Rhizoma Chuanxiong extracting solution 20mL that obtains according to preceding method contain crude drug amount 0.5g/mL, supersound extraction 1h leaves standstill 24h, makes its absorption that reaches capacity, filter, collect filtrate.Use distilled water washing resin, cleaning mixture and filtrate merge, and are settled to 25mL, measure the content of the composition such as ligustrazine in the absorption residual liquid, calculate respectively adsorbance S
InhaleWith the resin filtering redundant solution behind the saturated adsorption, the distilled water diafiltration resin with 4 times of resin volumes adds 50% ethanol 20mL, and sonic oscillation 1h places 24h.Filter, be settled to 25mL, measure the content of ferulic acid in the eluent, calculate desorption quantity S
SeparateWith desorption efficiency S:
S
Inhale=(C1V1-C2V2)/W;
S
Separate=C3V3/W;
S=C3V3/(S
InhaleW)
In the formula:
C1 is the extracting solution mass concentration, the μ g/mL of unit;
C2 is absorption residual liquid mass concentration, the μ g/mL of unit;
C3 is the stripping liquid mass concentration, the μ g/mL of unit;
V1 is extracting liquid volume, Unit/mL;
V2 is absorption residual liquid volume, Unit/mL;
V3 is the stripping liquid volume, Unit/mL;
W is the dry mass of resin, the g of unit.
Two kinds of resin Staticadsorption experiment results are referring to table 1.
Table 1
| Resinous type | Adsorbance (μ g/g) | Desorption quantity (μ g/g) | Desorption efficiency (%) |
| D-101 | 2021.34 | 352.4 | 17.43 |
| AB-8 | 2203.79 | 705.87 | 31.65 |
Use macroporous resin to carry out purification, not only requiring has larger absorbability, also preferably desorption ability need be arranged.As shown in Table 1, AB-8 type macroporous resin all is better than D-101 type macroporous resin on the sorption and desorption ability, so be the AB-8 type the preferred of macroporous resin.
(3) dynamic adsorption dynamic experiment
It is an amount of to get the Rhizoma Gastrodiae Rhizoma Chuanxiong extracting solution that obtains according to preceding method, glass column with the flow velocity of the 2BV/h internal diameter 1cm by the 2gAB-8 wet resin is housed, every 1BV(1 times of resin bed volume, being 3mL) effluent collects 1 part, measures as stated above the content of ligustrazine and ferulic acid in each part effluent and with the slip of 2 kinds of compositions in each part of cubage effluent of upper prop prodrug liquid.Take effluent times bed volume (hereinafter to be referred as " volume ") as abscissa, the slip of 3 kinds of compositions is vertical coordinate, draws ligustrazine, gastrodine and the leakage plot of ferulic acid on the AB-8 resin column.
The result of dynamic adsorption dynamic experiment: ligustrazine, gastrodine, the ferulic acid slip (%) on the AB-8 resin column is as shown in table 2, and the leakage plot of ligustrazine, gastrodine, ferulic acid as shown in Figure 1.
Table 2
| BV | Ligustrazine | | Ferulic acid | |
| 1 | 0.1013 | 0.1025 | 0.1111 | |
| 2 | 0.0868 | 0.1239 | 0.1114 | |
| 3 | 0.3054 | 0.3425 | 0.1189 | |
| 4 | 0.3357 | 0.4366 | 0.124 | |
| 5 | 0.3444 | 0.4817 | 0.1344 | |
| 6 | 0.4515 | 0.6039 | 0.2506 | |
| 7 | 0.4978 | 0.6771 | 0.2558 | |
| 8 | 0.5152 | 0.6772 | 0.248 | |
| 9 | 0.5716 | 0.6935 | 0.2765 | |
| 10 | 0.5847 | 0.7172 | 0.2817 |
By Fig. 1 and table 2 as can be known, ligustrazine and gastrodine begin to leak when 2BV, ferulic acid just has obvious leakage at 5BV, and there have figure to find out for the dynamic adsorption of ferulic acid to be less, three factors are all adsorbed obviously gradually slow when 6-7BV, illustrate that dynamic adsorption is saturated gradually, and really do not reach capacity.
(4) the dynamic attached dynamic experiment of desorption
Get and adsorbed saturated AB-8 resin column in the above-mentioned dynamic adsorption dynamic test, wash post with the distillation of 2BV first, flush away does not adsorb and is attached to impurity on the resin, carry out eluting with 50% alcoholic solution with the 10BV/h flow velocity again, every 1BV effluent is collected 1 part, the content of ligustrazine and ferulic acid in the same each part of mensuration effluent.Take eluent times bed volume as abscissa, the content of 2 kinds of compositions is vertical coordinate in the eluent, draws ferulic acid and the elution curve of ligustrazine on the AB-8 resin column.
The dynamic attached dynamic experiment result of desorption: the content (mg/mL) of ligustrazine, gastrodine, ferulic acid is as shown in table 3 in each times bed volume eluent, and ligustrazine and the ferulic acid elution curve on the AB-8 resin as shown in Figure 2.
Table 3
| BV | Ligustrazine | | Gastrodine | |
| 1 | 6.0816 | 1.0585 | 26.033 | |
| 2 | 10.1224 | 3.9312 | 30.147 |
| 3 | 13.8061 | 5.6467 | 30.673 |
| 4 | 14.4286 | 5.8918 | 31.13 |
| 5 | 10.2551 | 3.7815 | 22.031 |
| 6 | 3.3673 | 0.6161 | 9.15 |
| 7 | 1.4286 | 0.3233 | 4.496 |
| 8 | 0.3775 | 0.0004 | 4.385 |
By Fig. 2 and table 3 as can be known, in the situation take 50% ethanol as eluting solvent, ferulic acid is comparatively similar to the elution curve form of ligustrazine, shows that the desorption additive process of two kinds of compositions on resin column is tending towards synchronous.When eluent reached 4BV, all eluting was complete substantially for the two, so can this terminal point as eluting.
Claims (10)
1. the preparation method of a Rhizoma Gastrodiae Rhizoma Chuanxiong compound extract is characterized in that,
A. the material medicine with Rhizoma Gastrodiae and Rhizoma Chuanxiong mixes rear the pulverizing according to the ratio of 1:4～2:1;
B. the material medicine after extracting pulverizing with the 6-18 times of ethanol to the percent by volume 30～95% of described material medicine weight by the mode of percolation or reflux 2-3 time;
C. the extracting solution that obtains of step b is after concentrated, and remove impurity filters;
D. filtrate with the ethanol elution of percent by volume 30～95%, is collected eluent by macroporous resin column or silicagel column absorption;
E. dry behind the eluent recovery solvent, namely obtain described Rhizoma Gastrodiae Rhizoma Chuanxiong compound extract.
2. preparation method as claimed in claim 1 is characterized in that, among the step b, when adopting the percolation mode to extract, the percolation time is 12 ~ 48h; When adopting the reflux mode to extract, return time is 1 ~ 3h.
3. preparation method as claimed in claim 1 or 2 is characterized in that, among the step b, used concentration of alcohol is percent by volume 50 ~ 80%.
4. preparation method as claimed in claim 1 or 2 is characterized in that, in the steps d, used concentration of alcohol is percent by volume 40 ~ 70%.
5. preparation method as claimed in claim 1 or 2 is characterized in that, described macroporous resin is one or more in AB-8, D101, D4020, D101C, NKA-9, HPD-450 and the ADS-F8 type adsorbent resin.
6. preparation method as claimed in claim 1 or 2 is characterized in that, the model of described macroporous resin is AB-8, D101 or D101C.
7. the Rhizoma Gastrodiae that makes of preparation method as claimed in claim 1 or 2 and the Rhizoma Chuanxiong extract application in preparation treatment and prevention vascular dementia or migrainous medicine.
8. application as claimed in claim 7 is characterized in that, described treatment and prevention vascular dementia or migrainous medicine are comprised of acceptable adjuvant on described Rhizoma Gastrodiae and Rhizoma Chuanxiong extract and the pharmaceutics.
9. application as claimed in claim 7 is characterized in that, the dosage form of described treatment and prevention vascular dementia or migrainous medicine comprises: drop pill, the watered pill, capsule, tablet, soft capsule, slow releasing capsule, slow releasing tablet, slow-releasing microcapsule, injection and injectable powder.
10. application as claimed in claim 7 is characterized in that, the gastrodin content in described treatment and prevention vascular dementia or the migrainous medicine is not less than 0.1%, and the content of ligustrazine is not less than 0.1%, and the content of ferulic acid is not less than 0.1%.
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Cited By (3)
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| CN104000840A (en) * | 2014-06-16 | 2014-08-27 | 四川中医药高等专科学校 | Preparation method of extractive containing gastrodin and gastrodia elata polysaccharide |
| CN106266632A (en) * | 2016-08-25 | 2017-01-04 | 江苏康缘药业股份有限公司 | The purposes of Chinese medicine composition |
| CN108143929A (en) * | 2018-01-11 | 2018-06-12 | 深圳市中医院 | A kind of drug for treating vascular dementia |
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| CN100518798C (en) * | 2006-04-17 | 2009-07-29 | 浙江大德药业集团有限公司 | Dispersible tablet with gastrodia tuber for treating headache, and its testing method |
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| CN100518798C (en) * | 2006-04-17 | 2009-07-29 | 浙江大德药业集团有限公司 | Dispersible tablet with gastrodia tuber for treating headache, and its testing method |
| CN1883661A (en) * | 2006-05-31 | 2006-12-27 | 本溪市中心医院 | Dry powder preparation of chuanxiong rhizome, its preparation method and use |
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| CN104000840A (en) * | 2014-06-16 | 2014-08-27 | 四川中医药高等专科学校 | Preparation method of extractive containing gastrodin and gastrodia elata polysaccharide |
| CN106266632A (en) * | 2016-08-25 | 2017-01-04 | 江苏康缘药业股份有限公司 | The purposes of Chinese medicine composition |
| CN108143929A (en) * | 2018-01-11 | 2018-06-12 | 深圳市中医院 | A kind of drug for treating vascular dementia |
| CN108143929B (en) * | 2018-01-11 | 2020-11-24 | 深圳市中医院 | Medicine for treating vascular dementia |
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Application publication date: 20130123 |