A kind of preparation method of the effective ingredient in Chinese for treating hyperlipidemia
Technical field
The invention belongs to technical field of extraction of Chinese traditional medicine, more particularly, to a kind of effective portion of the Chinese medicine for treating hyperlipidemia
The preparation method of position.
Background technology
Polygonum cuspidatum Sieb. et Zucc is the dry rhizome and root of polygonaceae herbaceos perennial giant knotweed, has long medication history in China,
It is used as medicine earliest and sees《Lei Gong Pao Zhi Lun》.Taste bitter and cold, Return liver, courage, lung channel have normalizing gallbladder to cure jaundice, clearing heat and detoxicating, promoting blood circulation and removing blood stasis, dispel
The effects such as phlegm and relieving cough, it is clinically used for the diseases such as treatment jaundice with damp-heat pathogen, stranguria with turbid discharge, under band, blood stasis is through closing, cough with lung heat, constipation with heat retention.
Pharmaceutical research shows, giant knotweed to cardiovascular system of human body, digestive system, respiratory system, internal system, reproductive system and
Immune system is respectively provided with pharmacological effect effect.Wherein mainly have to cardiovascular system expansion of blood vessels, improve microcirculation, Hemorrhagic shock,
Suppress the effect of platelet aggregation, antithrombus formation and antiatherosclerosis, its mainly action material base be stilbene class(Tiger
Cane glycosides, resveratrol)And anthraquinone(Such as rheum emodin)Class material.For example, Peng Yuangui is reported prepares one kind containing multiple from giant knotweed
The composition of active ingredient(Containing polygonin more than 68.0%, resveratrol more than 2.0%, anthraquinone 4.0% ~ 6.5%)Method(Patent
Number CN101049348B), and pharmacodynamics, toxicologic study have been carried out to said composition preparation, as a result show by the active component
Chinese medicine preparation clinical application that composition is made safety, with notable regulating blood lipid action.
But unstability due to Rhizoma Polygoni Cuspidati quality, cause to report that the stability of production technology is very poor, used in technique
The class organic solvent ethyl acetate of big flow control three, acetone, certain burden is caused to control of product quality and environmental protection, and
Former technique process is more complicated, and the production cycle is long, main only to develop stilbene effective constituents in giant knotweed, herb resource is wasted compared with
Greatly.
The content of the invention
The present invention is directed to deficiency of the prior art, there is provided a kind of preparation of the effective ingredient in Chinese for treating hyperlipidemia
Method.
The present invention further investigate giant knotweed principle active component chemical property on the basis of, by technical study, it is proposed that
One kind more can ensure that active component production technology, quality stability than literature procedure, and cost is lower, more environmental protection, more
Be conducive to the process of preparing that herb resource makes full use of.
Technical purpose of the invention is achieved through the following technical solutions:
The present invention provides a kind of preparation method of the Chinese medicinal effective-part composition for treating hyperlipidemia, comprises the following steps:
S1. giant knotweed is extracted using 95% ethanol, is heated to reflux 2 ~ 3 times, filtered, take filtrate at a temperature of 50 ~ 65 DEG C, very
Sky is concentrated into the clear cream of relative density 1.15 ~ 1.20, and clear cream plus 8 times of amount water are heated into micro-boiling, is kept for 10 minutes, stands 12h,
It is filtrated to get supernatant and sediment;
S2. supernatant is taken, adds 0.2% ~ 1% activated carbon to boil, filtered while hot, take filtrate, be then concentrated to give clear cream, added
The ethanol of 3%-5%, stirs, and places crystallization, obtains brown color coarse crystallization, recrystallizes 1 ~ 2 time, obtains active component 1;
S3. sediment is centrifuged, is dissolved using 3% ~ 5% sodium carbonate liquor and extracted, filtering takes filtrate and adjusts pH to 2 ~ 3 with hydrochloric acid,
Stand, filtering, taking precipitate recrystallizes treatment 1 ~ 3 time with 70%-80% acidic ethanols, obtains active component 2.
Preferably, the pH of acidic ethanol is 2 ~ 3 in S3.
In patent 200610031480.3, there is provided a kind of Traditional Chinese medicine extraction method for treating hyperlipidemia, inventor has found,
Due to giant knotweed Chinese medicine less stable, when emodin content is less in Chinese medicine, it is impossible in order to be effective, thus medicine is had a strong impact on
Effect, finds by after numerous studies and experiment, the active component 1 for preparing of preparation method that is provided using the present invention and effectively
Position 2, it is ensured that due to the unstable unfavorable effect brought of giant knotweed raw material, be applied to prepare in treatment hyperlipidemia should
With.
Preferably, by active component 1, or compatibility obtains Gentrin Knotweed P.E in proportion by live part 1 and active component 2;
The Gentrin Knotweed P.E contains polygonin more than 68.0%, resveratrol more than 2.0%, anthraquinone component 4.0%-6.5%.
Additionally, active component 1 can press proper proportion compatibility individually or with active component 2, treatment hyperlipemia is made
Bulk drug -- Gentrin Knotweed P.E;Active component 2 can be separately as other preparations based on rheum emodin anthraquinone effective constituents
Raw material.
Compared with prior art, the present invention has advantages below and beneficial effect:
The present invention provide preparation method can overcome due to Rhizoma Polygoni Cuspidati quality it is unstable, cause the stability of production technology
The defect of variation, and overcome and used in the prior art a large amount of organic solvents, such as ethyl acetate, acetone etc. give product matter
Amount control and environmental protection cause the shortcoming of certain burden and pollution, and preparation method of the present invention is simple, takes full advantage of tiger
Cane Chinese medicine, realizes the reasonable utilization to giant knotweed Chinese medicine, possesses preferable application value.
Brief description of the drawings
Fig. 1 is the liquid phase detection collection of illustrative plates of active component 1 in embodiment 1.Wherein, 1 polygonin is represented in Fig. 1,2 represent white lamb's-quarters
Reed alcohol.
Fig. 2 is the liquid phase detection collection of illustrative plates of active component 1 in embodiment 1.3 represent rheum emodin in Fig. 2.
Fig. 3 is the liquid phase detection collection of illustrative plates of active component 2 in embodiment 1.4 represent rheum emodin in Fig. 3.
Specific embodiment
The present invention is specifically described below by embodiment, it is necessary to it is pointed out here that to be that the present embodiment is served only for right
The present invention is further described, but it is not intended that limiting the scope of the invention.
Unless stated otherwise, reagent, the method and apparatus for using of the invention is for the art conventional reagent, method and sets
It is standby.
Embodiment 1:The preparation method of active component composition:
1st, the Rhizoma Polygoni Cuspidati of recipe quantity is taken(Emodin content is relatively low), it is ground into meal.Plus 95% ethanol heating and refluxing extraction three times
(5 times, 1.5h, 4 times, 1h, 3 times, 0.5h), filtration.
2nd, filter vacuum concentration(50-65 DEG C of temperature)To the clear cream of relative density 1.15-1.20.
3rd, add 8 times of amount water to be heated to micro-boiling 10 minutes in clear cream, be sufficiently stirred for, be cooled to room temperature, stand 12 hours, from
The heart is filtered, and obtains supernatant and sediment, takes supernatant(The another method treatment of sediment), add 0.5% activated carbon to boil 10min, while hot
Filtered with titanium rod, filtrate is concentrated in vacuo to the clear cream of relative density 1.17-1.20 under 50-65 DEG C of temperature conditionss.
4th, the ethanol of clear cream amount 3% is added, is stirred, place crystallization, filter collection obtains brown color coarse crystallization.
5th, coarse-grain adds 10% ethyl alcohol recrystallization 1-2 times, active component 1 is obtained, shown in liquid phase detection collection of illustrative plates as Fig. 1 and Fig. 2.
Wherein, 1 polygonin is represented in Fig. 1,2 represent resveratrol, and 3 represent rheum emodin in Fig. 2.(Containing polygonin more than 68.0%, white lamb's-quarters
The anthraquinone component such as reed alcohol more than 2.0% and the rheum emodin less than 4% content).
6th, centrifuged deposit thing is first dissolved with 3%-5% sodium carbonate liquors and extracted, filtering, and filtrate adjusts pH to acidity with hydrochloric acid,
Stand, filtering obtains sediment.
7th, sediment is acid with 80%(pH2-3)Ethyl alcohol recrystallization is processed 1-3 times, obtains active component 2, liquid phase detection figure
Compose as shown in Figure 3, wherein, 4 represent rheum emodin.(Containing rheum emodin more than 30%).
8th, active component 1 and active component 2 compatibility, composition in proportion(Containing polygonin more than 68.0%, resveratrol 2.0%
More than, anthraquinone 4.0% ~ 6.5%, other are carbohydrate, flavonoids, and each component sum is 100%)Treat the raw material of hyperlipemia -- tiger
Cane extract.
9th, Gentrin Knotweed P.E add appropriate amount of auxiliary materials be made tablet, granule, powder, capsule, oral liquid, parenteral solution and other
Formulation.
Embodiment 2:The preparation method of active component composition:
1st, the Rhizoma Polygoni Cuspidati of recipe quantity is taken(Emodin content is higher), it is ground into meal.Plus 95% ethanol heating and refluxing extraction three times
(5 times, 1.5h, 4 times, 1h, 3 times, 0.5h), filtration.
2nd, filter vacuum concentration(50-65 DEG C of temperature)To the clear cream of relative density 1.15-1.20.
3rd, add 8 times of amount water to be heated to micro-boiling 10 minutes in clear cream, be sufficiently stirred for, be cooled to room temperature, stand 12 hours, from
The heart is filtered, and obtains supernatant and sediment, takes supernatant(The another method treatment of sediment), add 0.5% activated carbon to boil 10min, while hot
Filtered with titanium rod, filtrate is concentrated in vacuo to the clear cream of relative density 1.17-1.20 under 50-65 DEG C of temperature conditionss.
4th, the ethanol of clear cream amount 3% is added, is stirred, place crystallization, filter collection obtains brown color coarse crystallization.
5th, coarse-grain adds 10% ethyl alcohol recrystallization 1-2 times, obtains active component 1(Containing polygonin more than 68.0%, resveratrol
More than 2.0%, anthraquinone component 4.0%-6.5%).
6th, centrifuged deposit thing is first dissolved with 3%-5% sodium carbonate liquors and extracted, filtering, and filtrate adjusts pH to acidity with hydrochloric acid,
Stand, filtering obtains sediment.
7th, sediment is acid with 80%(pH2-3)Ethyl alcohol recrystallization is processed 1-3 times, obtains active component 2(Containing rheum emodin 30%
More than).
8th, active component 1(Containing polygonin more than 68.0%, resveratrol more than 2.0%, anthraquinone 4.0%-6.5%, other are sugar
Class, flavonoids, each component sum are 100%)Separately as bulk drug -- the Gentrin Knotweed P.E for the treatment of hyperlipemia.
9th, Gentrin Knotweed P.E add appropriate amount of auxiliary materials be made tablet, granule, powder, capsule, oral liquid, parenteral solution and other
Formulation.
Embodiment 3:
Gentrin Knotweed P.E 25-30g in Example 1, plus PVPP 10-15g, microcrystalline cellulose 100-
120g, pregelatinized starch 10-15g, lactose 20-30g, mixing are crushed, plus Diluted Alcohol, and granulation is dried, whole grain, add crosslinking poly-
Vinylpyrrolidone 15-20g, superfine silica gel powder 1-2g, magnesium stearate 1-2g, mix, and compressing tablet is made 1000, film coating, i.e.,
.
Embodiment 4:
Gentrin Knotweed P.E 25-30g in Example 2, microcrystalline cellulose 100-120g, pregelatinized starch 20-25g, lactose 20-
30g, mixing is crushed, plus Diluted Alcohol, and granulation is dried, whole grain, adds PVPP 15-20g, superfine silica gel powder 1-
2g, magnesium stearate 1-2g, mix, and compressing tablet is made 1000, and film coating is obtained final product.
Embodiment 5:
Gentrin Knotweed P.E 25-30g in Example 2, starch 250-300g, lactose 200-250g, low-substituted hydroxypropyl cellulose
15-20g, mixing is crushed, plus starch slurry, and granulation is dried, whole grain, adds superfine silica gel powder 1-2g, magnesium stearate 1-2g, is mixed,
Packing, obtains final product.