CN105168262A - Preparation method of traditional Chinese medicine decocting-free preparation containing carbohydrate - Google Patents
Preparation method of traditional Chinese medicine decocting-free preparation containing carbohydrate Download PDFInfo
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- CN105168262A CN105168262A CN201510687106.8A CN201510687106A CN105168262A CN 105168262 A CN105168262 A CN 105168262A CN 201510687106 A CN201510687106 A CN 201510687106A CN 105168262 A CN105168262 A CN 105168262A
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Abstract
The invention belongs to the technical field of traditional Chinese medicine decocting-free preparations and in particular relates to a preparation method of a traditional Chinese medicine decocting-free preparation containing carbohydrate. The preparation method of the traditional Chinese medicine decocting-free preparation containing carbohydrate comprises the following steps: crushing raw materials, extracting with distilled water, extracting with ionic liquid aqueous solution, and carrying out column chromatography separation, so that the traditional Chinese medicine decocting-free preparation is obtained. The preparation method of the traditional Chinese medicine decocting-free preparation containing carbohydrate is environmentally friendly, the extraction ratio of an effective ingredient, namely carbohydrate, can be more than 85%, and waste of traditional Chinese medicine resources is reduced.
Description
Technical field
The invention belongs to free decoction agent technical field, be specifically related to a kind of preparation method of the free decoction agent containing saccharide compound.
Background technology
Many Chinese crude drugs contain multiple bioactive compound, have multiple curative effect, have a wide range of applications.Common active component is as polyphenol compound, nitrogen-containing compound, vitamin, terpenoid and some other endogenous metabolism thing.The extracting method that these reactive compounds adopt usually comprises decocting method, ultrasonic circumfluence method, soxhlet extraction etc., but, virulent organic solvent is used and large usage quantity in these methods experiment processes, it is very long to extract the time used, extraction efficiency is low, and experiment operator health is harmful to, environmental pollution is serious.Therefore, for a long time, Chinese medicine extraction active component replaces traditional organic solvent in the urgent need to finding a kind of nonvolatile solvent that is nontoxic, high efficiency extraction.
Chinese crude drug containing saccharide compound has important medical value clinically, such as: Fructus Momordicae, cool in nature, sweet in the mouth, has clearing heat and moistening lung, cough-relieving, sore-throat relieving, the effect of laxation relieving constipation, one of its effective ingredient is Momordica-Glycosides, sweeter than cane suger 300 times, and thermal content is low, for flu, cough, der Halsschmerz, en, gastrointestinal upset is that diabetics is stable and without fermentable perfect additive; Rhizoma Dioscoreae, property flat, sweet in the mouth, have spleen reinforcing nourishing the stomach, promote the production of body fluid lung benefiting, the effect of the kidney invigorating arresting seminal emission, have good effect for prevention and therapy diabetes and digestive system disease, enhancing and Promote immunity function, anti-ageing aspect of waiting for a long time, one of its effective ingredient is polysaccharide, and polysaccharide can improve the edible quality of food, processing characteristics and appearance characteristics, can be used for suppressing lipid oxidation, there is adjustment or strengthen immunologic function, blood sugar lowering, the effects such as antitumor; Ganoderma, nature and flavor are sweet, flat, invigorating QI and tranquilization, relieving cough and asthma, ganoderan is one of the most effective composition in Ganoderma, can improve immunity of organisms, improve body's hypoxia tolerance, eliminate free radical, Tumor suppression, radioprotective, improve liver, bone marrow, blood synthetic DNA, RNA, protein-energy, life-saving, ganoderan also has stimulation of host non-specific resistance, immune specific reaction and suppresses the characteristic of transplantation tumor physiologically active.But adopt conventional extracting method often to make to extract not exclusively containing sugar compounds in Chinese crude drug, cause the loss of effective ingredient, extraction ratio is low, causes the waste of medical material, and often adopts organic solvent extraction, seriously polluted.
Summary of the invention
For overcoming above-mentioned defect, the object of the present invention is to provide a kind of preparation method of the free decoction agent containing saccharide compound, environmental protection, effective component extraction rate is high.
For achieving the above object, the present invention adopts following technical scheme:
Containing a preparation method for the free decoction agent of saccharide compound, comprise the following steps:
(1) traditional Chinese medicinal material raw materials is dry, broken, obtain powder 10 ~ 20g;
(2) step (1) powder is adopted the distilled water lixiviate 2 ~ 4 times of 5 ~ 15 times of weight, obtain extractum;
(3) in step (2) extractum, add ionic liquid aqueous solution 80 ~ 120mL, mix homogeneously, react 5 ~ 10h under 50 ~ 80 DEG C of conditions, obtain serosity;
(4) step (3) serosity is carried out microfiltration, collect filtrate, dewater;
(5) filtrate is adopted column chromatography for separation, concentrating under reduced pressure, vacuum drying, obtain free decoction agent.
According to the preparation method of the above-mentioned free decoction agent containing saccharide compound, the aqueous solution ionic liquid concentration of the ionic liquid described in described step (3) is 0.05 ~ 0.15mol/L.
According to the preparation method of the above-mentioned free decoction agent containing saccharide compound, described step (3) ionic liquid is 1-butyl-3-methyl imidazolium tetrafluoroborate (BmimBF
4), 1-hexyl-3-Methylimidazole. bromine salt (HmimBr) and N-butyl-pyridinium tetrafluoroborate (BpyBF
4) middle at least one.
According to the preparation method of the above-mentioned free decoction agent containing saccharide compound, described step (3) ionic liquid is N-butyl-pyridinium tetrafluoroborate (BpyBF
4).
According to the preparation method of the above-mentioned free decoction agent containing saccharide compound, described step (5) column chromatography for separation condition is: 200 ~ 300 order silicagel columns, and eluant is cyclohexane extraction and ethyl acetate, and both volume ratios are 1:5 ~ 1:20.
the positive beneficial effect of the present invention:
1. first the present invention slightly carries effective ingredient in Chinese crude drug through ethanol containing the preparation method of the free decoction agent of saccharide compound, secondly extract further through ionic liquid aqueous solution, sugary effective constituents can be made to dissolve thoroughly, saccharide effective ingredient is fully retained, decreases the waste of Chinese material medicine resource.
2. ionic liquid liquid condition temperature range of the present invention is wide, from lower than or close to room temperature within the scope of 300 DEG C, can stable existence, there is good heat stability, good solvability is all shown to a large amount of inorganic and organic substances, fusing point is low, non-combustible, and steam forces down, not volatile, easy recovery, environmental protection, overcomes the problem of environmental pollution that Chinese medicine extracts organic solvent.
3. the present invention is simple containing the whole process operation of preparation method of the free decoction agent of saccharide compound, effective ingredient can up to more than 85% containing sugar compounds extraction ratio, prepared free decoction agent does not need decoction process directly to take, and has good economic benefit and social benefit.
Detailed description of the invention
Below in conjunction with some detailed description of the invention, the present invention is further described.
Embodiment 1
Containing a preparation method for the free decoction agent of saccharide compound, comprise the following steps:
(1) traditional Chinese medicinal material raw materials Fructus Momordicae is removed the peel, dry, broken, obtain powder 10g;
(2) step (1) powder is adopted the distilled water lixiviate 2 times of 5 times of weight, obtain extractum;
(3) in step (2) extractum, add ionic liquid aqueous solution 80mL, mix homogeneously, ionic liquid is BmimBF
4, concentration is 0.05mol/L, reacts 10h, obtain serosity under 50 DEG C of conditions;
(4) step (3) serosity is carried out microfiltration, collect filtrate, dewater;
(5) filtrate is adopted column chromatography for separation, concentrating under reduced pressure, vacuum drying, obtain free decoction agent; Column chromatography for separation condition is: 200 ~ 300 order silicagel columns, and eluant is cyclohexane extraction and ethyl acetate, and both volume ratios are 1:5 ~ 1:20.
In Momordica-Glycosides active constituent content, the results are shown in following table 1.
Embodiment 2
Containing a preparation method for the free decoction agent of saccharide compound, comprise the following steps:
(1) traditional Chinese medicinal material raw materials Fructus Momordicae is removed the peel, dry, broken, obtain powder 12g;
(2) step (1) powder is adopted the distilled water lixiviate 3 times of 6 times of weight, obtain extractum;
(3) in step (2) extractum, add ionic liquid aqueous solution 90mL, mix homogeneously, ionic liquid is BpyBF
4, concentration is 0.07mol/L, reacts 9h, obtain serosity under 60 DEG C of conditions;
(4) step (3) serosity is carried out microfiltration, collect filtrate, dewater;
(5) filtrate is adopted column chromatography for separation, concentrating under reduced pressure, vacuum drying, obtain free decoction agent; Column chromatography for separation condition is: 200 ~ 300 order silicagel columns, and eluant is cyclohexane extraction and ethyl acetate, and both volume ratios are 1:5 ~ 1:20.
In Momordica-Glycosides active constituent content, the results are shown in following table 1.
Embodiment 3
Containing a preparation method for the free decoction agent of saccharide compound, comprise the following steps:
(1) traditional Chinese medicinal material raw materials Fructus Momordicae is removed the peel, dry, broken, obtain powder 13g;
(2) step (1) powder is adopted the distilled water lixiviate 4 times of 10 times of weight, obtain extractum;
(3) in step (2) extractum, add ionic liquid 100mL, mix homogeneously, ionic liquid is HmimBr, and concentration is 0.13mol/L, reacts 5h, obtain serosity under 80 DEG C of conditions;
(4) step (3) serosity is carried out microfiltration, collect filtrate, dewater;
(5) filtrate is adopted column chromatography for separation, concentrating under reduced pressure, vacuum drying, obtain free decoction agent; Column chromatography for separation condition is: 200 ~ 300 order silicagel columns, and eluant is cyclohexane extraction and ethyl acetate, and both volume ratios are 1:5 ~ 1:20.
In Momordica-Glycosides active constituent content, the results are shown in following table 1.
Embodiment 4
Containing a preparation method for the free decoction agent of saccharide compound, comprise the following steps:
(1) traditional Chinese medicinal material raw materials Ganoderma is dry, broken, obtain powder 15g;
(2) step (1) powder is adopted the distilled water lixiviate 3 times of 9 times of weight, obtain extractum;
(3) in step (2) extractum, add ionic liquid 100mL, mix homogeneously, ionic liquid is BpyBF
4, concentration is 0.09mol/L, reacts 7h, obtain serosity under 70 DEG C of conditions;
(4) step (3) serosity is carried out microfiltration, collect filtrate, dewater;
(5) filtrate is adopted column chromatography for separation, concentrating under reduced pressure, vacuum drying, obtain free decoction agent; Column chromatography for separation condition is: 200 ~ 300 order silicagel columns, and eluant is cyclohexane extraction and ethyl acetate, and both volume ratios are 1:5 ~ 1:20.
In ganoderan active constituent content, the results are shown in following table 1.
Embodiment 5
Containing a preparation method for the free decoction agent of saccharide compound, comprise the following steps:
(1) traditional Chinese medicinal material raw materials Ganoderma is dry, broken, obtain powder 16g;
(2) step (1) powder is adopted the distilled water lixiviate 3 times of 10 times of weight, obtain extractum;
(3) in step (2) extractum, add ionic liquid 100mL, mix homogeneously, ionic liquid is HmimBr, and concentration is 0.1mol/L, reacts 8h, obtain serosity under 60 DEG C of conditions;
(4) step (3) serosity is carried out microfiltration, collect filtrate, dewater;
(5) filtrate is adopted column chromatography for separation, concentrating under reduced pressure, vacuum drying, obtain free decoction agent; Column chromatography for separation condition is: 200 ~ 300 order silicagel columns, and eluant is cyclohexane extraction and ethyl acetate, and both volume ratios are 1:5 ~ 1:20.
In ganoderan active constituent content, the results are shown in following table 1.
Embodiment 6
Containing a preparation method for the free decoction agent of saccharide compound, comprise the following steps:
(1) traditional Chinese medicinal material raw materials Rhizoma Dioscoreae is removed the peel, dry, broken, obtain powder 18g;
(2) step (1) powder is adopted the distilled water lixiviate 4 times of 12 times of weight, obtain extractum;
(3) in step (2) extractum, add ionic liquid 110mL, mix homogeneously, ionic liquid is BpyBF
4, concentration is 0.12mol/L, reacts 6h, obtain serosity under 70 DEG C of conditions;
(4) step (3) serosity is carried out microfiltration, collect filtrate, dewater;
(5) filtrate is adopted column chromatography for separation, concentrating under reduced pressure, vacuum drying, obtain free decoction agent; Column chromatography for separation condition is: 200 ~ 300 order silicagel columns, and eluant is cyclohexane extraction and ethyl acetate, and both volume ratios are 1:5 ~ 1:20.
In Chinese yam polysaccharide active constituent content, the results are shown in following table 1.
Embodiment 7
Containing a preparation method for the free decoction agent of saccharide compound, comprise the following steps:
(1) traditional Chinese medicinal material raw materials Rhizoma Dioscoreae is removed the peel, dry, broken, obtain powder 20g;
(2) step (1) powder is adopted the distilled water lixiviate 4 times of 15 times of weight, obtain extractum;
(3) in step (2) extractum, add ionic liquid 120mL, mix homogeneously, ionic liquid is BmimBF
4, concentration is 0.15mol/L, reacts 5h, obtain serosity under 80 DEG C of conditions;
(4) step (3) serosity is carried out microfiltration, collect filtrate, dewater;
(5) filtrate is adopted column chromatography for separation, concentrating under reduced pressure, vacuum drying, obtain free decoction agent; Column chromatography for separation condition is: 200 ~ 300 order silicagel columns, and eluant is cyclohexane extraction and ethyl acetate, and both volume ratios are 1:5 ~ 1:20.
In Chinese yam polysaccharide active constituent content, the results are shown in following table 1.
Table 1 embodiment of the present invention 1 ~ 7 containing sugar compounds effective substance result
As can be seen from Table 1, adopt the present invention containing the preparation method of the free decoction agent of saccharide compound, in Fructus Momordicae, in Momordica-Glycosides, Ganoderma, in ganoderan and Rhizoma Dioscoreae, the extraction ratio of Chinese yam polysaccharide is respectively up to more than 85%, high containing sugar compounds effective component extraction rate.
Claims (5)
1., containing a preparation method for the free decoction agent of saccharide compound, it is characterized in that, comprise the following steps:
(1) traditional Chinese medicinal material raw materials is dry, broken, obtain powder 10 ~ 20g;
(2) step (1) powder is adopted the distilled water lixiviate 2 ~ 4 times of 5 ~ 15 times of weight, obtain extractum;
(3) in step (2) extractum, add ionic liquid aqueous solution 80 ~ 120mL, mix homogeneously, react 5 ~ 10h under 50 ~ 80 DEG C of conditions, obtain serosity;
(4) step (3) serosity is carried out microfiltration, collect filtrate, dewater;
(5) filtrate is adopted column chromatography for separation, concentrating under reduced pressure, vacuum drying, obtain free decoction agent.
2. the preparation method of the free decoction agent containing saccharide compound according to claim 1, it is characterized in that, the ionic liquid aqueous solution intermediate ion strength of fluid described in described step (3) is 0.05 ~ 0.15mol/L.
3. the preparation method of the free decoction agent containing saccharide compound according to claim 1, it is characterized in that, described step (3) ionic liquid is at least one in 1-butyl-3-methyl imidazolium tetrafluoroborate, 1-hexyl-3-Methylimidazole. bromine salt and N-butyl-pyridinium tetrafluoroborate.
4. the preparation method of the free decoction agent containing saccharide compound according to claim 3, it is characterized in that, described step (3) ionic liquid is N-butyl-pyridinium tetrafluoroborate.
5. the preparation method of the free decoction agent containing saccharide compound according to claim 1, it is characterized in that, described step (5) column chromatography for separation condition is: 200 ~ 300 order silicagel columns, and eluant is cyclohexane extraction and ethyl acetate, and both volume ratios are 1:5 ~ 1:20.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108610432A (en) * | 2018-04-03 | 2018-10-02 | 徐州工程学院 | A kind of method of high efficiency extraction edible burdock inulin |
Citations (3)
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|---|---|---|---|---|
| CN101167782A (en) * | 2007-11-03 | 2008-04-30 | 广西中医学院 | Momordica grosvenori liver-protecting preparation and production method thereof |
| CN101999493A (en) * | 2010-12-08 | 2011-04-06 | 费维来 | Preparation method of plant health-care cool tea |
| CN102018766A (en) * | 2009-09-16 | 2011-04-20 | 博仲盛景医药技术（北京）有限公司 | Plant extractive, extraction method and application thereof as well as composite comprising same |
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- 2015-10-22 CN CN201510687106.8A patent/CN105168262A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101167782A (en) * | 2007-11-03 | 2008-04-30 | 广西中医学院 | Momordica grosvenori liver-protecting preparation and production method thereof |
| CN102018766A (en) * | 2009-09-16 | 2011-04-20 | 博仲盛景医药技术（北京）有限公司 | Plant extractive, extraction method and application thereof as well as composite comprising same |
| CN101999493A (en) * | 2010-12-08 | 2011-04-06 | 费维来 | Preparation method of plant health-care cool tea |
Non-Patent Citations (1)
| Title |
|---|
| 鞠伟等: "罗汉果研究概况综述", 《广西轻工业》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108610432A (en) * | 2018-04-03 | 2018-10-02 | 徐州工程学院 | A kind of method of high efficiency extraction edible burdock inulin |
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