CN102920767A - Preparation method of wild chrysanthemum extract - Google Patents
Preparation method of wild chrysanthemum extract Download PDFInfo
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- CN102920767A CN102920767A CN 201210482811 CN201210482811A CN102920767A CN 102920767 A CN102920767 A CN 102920767A CN 201210482811 CN201210482811 CN 201210482811 CN 201210482811 A CN201210482811 A CN 201210482811A CN 102920767 A CN102920767 A CN 102920767A
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- flos chrysanthemi
- chrysanthemi indici
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- deionized water
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Abstract
The invention relates to a preparation method of an extract, in particular to a preparation method of a wild chrysanthemum extract. The invention aims at solving the problems that the wild chrysanthemum extract prepared by the conventional preparation method for industry production mostly is a crude extract with low content of general flavone and can not meet the requirement of industrialized production. The preparation method comprises the following steps: I, wild chrysanthemum Chinese medicinal plant is boiled in deionized water to get concentrated clear paste; II, water is added to the clear paste, the PH value is adjusted and the upper layer liquid is collected; III, ethanol eluant is collected; and IV, ethanol is recovered, PH value is adjusted, the liquid is concentrated, the pressure is reduced and wild chrysanthemum extract is obtained. The extract obtained through the method provided by the invention has a high yield rate of 2.5%, and the obtained wild chrysanthemum extract contains more than 80% of general flavone contents, calculated by anhydrous rutin (CHO). The invention is used for preparing wild chrysanthemum extract, and the wild chrysanthemum extract can be used as raw materials for traditional Chinese medicine injection or oral liquid.
Description
Technical field
The present invention relates to a kind of preparation method of extract.
Background technology
Flos Chrysanthemi Indici is the dry capitulum of feverfew Herba Dendranthematis indici (Chrysanthemum indicumL.), records in " Chinese Pharmacopoeia 2010 version one one " 295 pages.The effect of tool heat-clearing and toxic substances removing, pathogenic fire purging suppressing the hyperactive liver.Be used for that the fourth carbuncle sore is swollen, conjunctival congestion and swelling pain, headache be dizzy.In recent years, along with the develop rapidly that the modern times are extracted separation and Wave Spectrum technology and modern pharmacology, more and more deep to chemical constituent and the bioactive research of Flos Chrysanthemi Indici platymiscium.Through chemical analysis, its Main Ingredients and Appearance is the materials such as flavonoid, phenolic acids and terpenoid, is the material base of its performance pharmacologically active.Modern pharmacological research confirms that the Flos Chrysanthemi Indici extract pharmacological action is comparatively extensive: (1) heart, cerebrovascular protective effect; Have the increase coronary flow, reduce oxygen metabolism, improve hypoxia-bearing capability, to the therapeutical effect of experimental myocardial infarction, increase cerebral blood flow, improve microcirculation, the vasoconstrictive effect.(2) to the effect of blood system; Has antiplatelet aggregation, fortifying fibre proteinase activity, blood fat reducing, blood circulation promoting and blood stasis dispelling, study of anti-atherogenic effect.(3) hypotensive effect; (4) resisting pathogenic microbes effect; (5) promote phagocytic activity of leukocytes; (6) other effects.Therefore, study now more mother chrysanthemum total flavone and have great clinical value and market development value as the medical active position.
At present, the preparation method of Flos Chrysanthemi Indici extract is a lot, but is applied to the industrial crude extract that mostly is, and general flavone content is low in the extract, can not satisfy the requirement of suitability for industrialized production.
Summary of the invention
The present invention is that the Flos Chrysanthemi Indici extract that will solve the preparation of the preparation method of existing Flos Chrysanthemi Indici extract is used for the industrial crude extract that mostly is, general flavone content is low in the extract, can not satisfy the problem of the requirement of suitability for industrialized production, and a kind of preparation method of Flos Chrysanthemi Indici extract is provided.
A kind of preparation method of Flos Chrysanthemi Indici extract specifically prepares according to following steps:
One, gets the Flos Chrysanthemi Indici Chinese crude drug, decoct 3 times with deionized water, each 1h, for the first time the quality of deionized water is 16 ~ 20 times of Flos Chrysanthemi Indici Chinese crude drug, for the second time the quality of deionized water is 12 ~ 16 times of Flos Chrysanthemi Indici Chinese crude drug, the quality of deionized water is 12 ~ 16 times of Flos Chrysanthemi Indici Chinese crude drug for the third time, merges 3 times decoction liquor, and reconcentration is to take the clear paste of 70 ℃ of relative densities as 1.10～1.14;
Two, in the clear paste of step 1 acquisition, add water, adding volume behind the water and the mass ratio of Flos Chrysanthemi Indici Chinese crude drug is 2L:1kg, be that 10% sodium hydroxide solution is regulated pH value to 6.5～7.0 with mass concentration again, leave standstill 12h ~ 24h, collect supernatant, regulate pH value to 2.0～3.0 with hydrochloric acid solution again, leave standstill again 12h ~ 24h, collect supernatant liquid;
Three, the supernatant liquid of step 2 being collected is crossed polyamide resin column, the mass ratio of polyamide and Flos Chrysanthemi Indici Chinese crude drug is 1:2.5, carry out eluting with deionized water again, the deionized water volume that eluting is used is 6 ~ 10 column volumes, it is 65% ~ 85% alcoholic solution eluting resin column that water lotion discards rear use volumetric concentration, the volumes of aqueous ethanol that eluting is used is 5 column volumes, collects ethanol elution;
Four, ethanol elution is carried out the distilling under reduced pressure Recycled ethanol, with sodium hydroxide solution adjust pH 6.0 ~ 7.0, concentrated, drying under reduced pressure namely obtains Flos Chrysanthemi Indici extract, finishes the preparation method of Flos Chrysanthemi Indici extract.
The invention has the beneficial effects as follows: adopt the method for acid treatment extracting solution to remove the larger tannin class material of molecular weight, the utilization polyamide is processed, adopting volumetric concentration is 80% ethanol elution, this technique is further removed macromolecular albumen, tannin and resinae material, so that the Flavonoid substances of enrichment molecular weight.The key point of this invention is to adopt before polyamide processes, and adopts first the acid treatment extracting solution, and flavone and organic acid in the extracting solution are all entered in the resin column under the non-salification, and can be more completely by resin absorption, and specific aim is better.Adopting simultaneously volumetric concentration is more completely desorbing flavone of 80% ethanol.This technique is except ethanol, do not use other organic solvents, so that technological process is simple, production equipment requires lower, manufacturing cost reduces, simultaneously the method extract yield highlyer surpass 2.5%, this extractive total flavone content surpasses 80%, reaches the specification requirement of national Chinese medicine raw material.The method makes the flavones ingredient enrichment and is applicable to suitability for industrialized production mainly in flavones ingredient.
General flavone content is with anhydrous rutin (C in the Flos Chrysanthemi Indici extract that the inventive method obtains
27H
30O
16) meter, surpass 80%; Monomer component linarin (C
28H
32O
14) content surpasses 15%.
The present invention is for the preparation of Flos Chrysanthemi Indici extract, and this extract can be used as the raw material of Chinese medicine raw material or oral formulations.
The specific embodiment
Technical solution of the present invention is not limited to the following cited specific embodiment, also comprises the combination in any between each specific embodiment.
The specific embodiment one: the preparation method of a kind of Flos Chrysanthemi Indici extract of present embodiment specifically prepares according to following steps:
One, gets the Flos Chrysanthemi Indici Chinese crude drug, decoct 3 times with deionized water, each 1h, for the first time the quality of deionized water is 16 ~ 20 times of Flos Chrysanthemi Indici Chinese crude drug, for the second time the quality of deionized water is 12 ~ 16 times of Flos Chrysanthemi Indici Chinese crude drug, the quality of deionized water is 12 ~ 16 times of Flos Chrysanthemi Indici Chinese crude drug for the third time, merges 3 times decoction liquor, and reconcentration is to take the clear paste of 70 ℃ of relative densities as 1.10～1.14;
Two, in the clear paste of step 1 acquisition, add water, adding volume behind the water and the mass ratio of Flos Chrysanthemi Indici Chinese crude drug is 2L:1kg, be that 10% sodium hydroxide solution is regulated pH value to 6.5～7.0 with mass concentration again, leave standstill 12h ~ 24h, collect supernatant, regulate pH value to 2.0～3.0 with hydrochloric acid solution again, leave standstill again 12h ~ 24h, collect supernatant liquid;
Three, the supernatant liquid of step 2 being collected is crossed polyamide resin column, the mass ratio of polyamide and Flos Chrysanthemi Indici Chinese crude drug is 1:2.5, carry out eluting with deionized water again, the deionized water volume that eluting is used is 6 ~ 10 column volumes, it is 65% ~ 85% alcoholic solution eluting resin column that water lotion discards rear use volumetric concentration, the volumes of aqueous ethanol that eluting is used is 5 column volumes, collects ethanol elution;
Four, ethanol elution is carried out the distilling under reduced pressure Recycled ethanol, with sodium hydroxide solution adjust pH 6.0 ~ 7.0, concentrated, drying under reduced pressure namely obtains Flos Chrysanthemi Indici extract, finishes the preparation method of Flos Chrysanthemi Indici extract.
Present embodiment adopts the method for acid treatment extracting solution to remove the larger tannin class material of molecular weight, the utilization polyamide is processed, adopting volumetric concentration is 80% ethanol elution, this technique is further removed macromolecular albumen, tannin and resinae material, so that the Flavonoid substances of enrichment molecular weight.The key point of this invention is to adopt before polyamide processes, and adopts first the acid treatment extracting solution, and flavone and organic acid in the extracting solution are all entered in the resin column under the non-salification, and can be more completely by resin absorption, and specific aim is better.Adopting simultaneously volumetric concentration is more completely desorbing flavone of 80% ethanol.This technique is except ethanol, do not use other organic solvents, so that technological process is simple, production equipment requires lower, manufacturing cost reduces, simultaneously the method extract yield highlyer surpass 2.5%, this extractive total flavone content surpasses 80%, reaches the specification requirement of national Chinese medicine raw material.The method makes the flavones ingredient enrichment and is applicable to suitability for industrialized production mainly in flavones ingredient.
General flavone content is with anhydrous rutin (C in the Flos Chrysanthemi Indici extract that present embodiment obtains
27H
30O
16) meter, surpass 80%; Monomer component linarin (C
28H
32O
14) content surpasses 15%.
The specific embodiment two: what present embodiment and the specific embodiment one were different is: the quality of deionized water is 18 ~ 19 times of Flos Chrysanthemi Indici Chinese crude drug for the first time, for the second time the quality of deionized water is 14 ~ 15 times of Flos Chrysanthemi Indici Chinese crude drug, and the quality of deionized water is 14 ~ 15 times of Flos Chrysanthemi Indici Chinese crude drug for the third time.Other is identical with the specific embodiment one.
The specific embodiment three: what present embodiment was different from the specific embodiment one or two is: the mass concentration of the described hydrochloric acid solution of step 2 is 5%.Other is identical with the specific embodiment one or two.
The specific embodiment four: what present embodiment was different from one of specific embodiment one to three is: the volumetric concentration of the described alcoholic solution of step 3 is 70% ~ 80%.Other is identical with one of specific embodiment one to three.
The specific embodiment five: what present embodiment was different from one of specific embodiment one to three is: the volumetric concentration of the described alcoholic solution of step 3 is 75%.Other is identical with one of specific embodiment one to three.
The specific embodiment six: what present embodiment was different from one of specific embodiment one to five is: the mass concentration of the described sodium hydroxide solution of step 4 is 10%.Other is identical with one of specific embodiment one to five.
The specific embodiment seven: what present embodiment was different from one of specific embodiment one to six is: adjust pH 6.5 ~ 6.8 in the step 4.Other is identical with one of specific embodiment one to six.
The specific embodiment eight: what present embodiment was different from one of specific embodiment one to seven is: the described drying under reduced pressure temperature of step 4 is 60 ℃ ~ 80 ℃, and the drying under reduced pressure time is 6h ~ 10h.Other is identical with one of specific embodiment one to seven.
The specific embodiment nine: what present embodiment was different from one of specific embodiment one to seven is: the described drying under reduced pressure temperature of step 4 is 65 ℃ ~ 75 ℃, and the drying under reduced pressure time is 7h ~ 9h.Other is identical with one of specific embodiment one to seven.
Adopt following examples to verify beneficial effect of the present invention:
Embodiment one:
The preparation method of a kind of Flos Chrysanthemi Indici extract of present embodiment specifically prepares according to following steps:
One, gets 100kg Flos Chrysanthemi Indici Chinese crude drug, decoct 3 times with deionized water, each 1h, for the first time the quality of deionized water is 20 times of Flos Chrysanthemi Indici Chinese crude drug, for the second time the quality of deionized water is 16 times of Flos Chrysanthemi Indici Chinese crude drug, the quality of deionized water is 16 times of Flos Chrysanthemi Indici Chinese crude drug for the third time, merges 3 times decoction liquor, and reconcentration is to take the clear paste of 70 ℃ of relative densities as 1.10～1.14;
Two, add water in the clear paste that obtains to step 1, the volume that adds behind the water is 200L, is 10% sodium hydroxide solution adjusting pH value to 6.5 again with mass concentration, leaving standstill 24h, collect supernatant, is 5% hydrochloric acid solution adjusting pH value to 2.0 again with mass concentration, leave standstill again 24h, collect supernatant liquid;
Three, the supernatant liquid of step 2 being collected is crossed polyamide resin column, the mass ratio of polyamide and Flos Chrysanthemi Indici Chinese crude drug is 1:2.5, carry out eluting with deionized water again, the deionized water volume that eluting is used is 8 column volumes, it is 80% alcoholic solution eluting resin column that water lotion discards rear use volumetric concentration, the volumes of aqueous ethanol that eluting is used is 5 column volumes, collects ethanol elution;
Four, ethanol elution being carried out the distilling under reduced pressure Recycled ethanol, is 10% sodium hydroxide solution adjust pH 6.5 with mass concentration, concentrated, drying under reduced pressure, drying under reduced pressure temperature are 80 ℃, and the drying under reduced pressure time is 9h, namely obtain Flos Chrysanthemi Indici extract, finish the preparation method of Flos Chrysanthemi Indici extract.
The extract yield of present embodiment is no less than 2.5%, and main component is flavone.The result of study of this extract components situation: general flavone content is with anhydrous rutin (C in the extract
27H
30O
16) meter, be no less than 80%; Monomer component linarin (C
28H
32O
14) content is no less than 15%.
The exploratory study of main component
1 material, test and reagent
High performance liquid chromatograph Agilent 1100 series liquid chromatograph instrument are furnished with online degasser; Quaternary gradient elution pump; Column oven.
Linarin chemical reference substance lot number: 111528-200605
Rutin chemical reference substance lot number: 110080-200707
Provided by Nat'l Pharmaceutical ﹠ Biological Products Control Institute
Chromatographic column C18250 * 4.6mm 5 μ m
Reagent: methanol, acetonitrile chromatographically pure (DIKMA)
The Flos Chrysanthemi Indici extract of reagent: embodiment one preparation
Lot number: 110601,110901,120401
2 test methods and result
2.1 test method
The Flos Chrysanthemi Indici extract quality control adopts determined by ultraviolet spectrophotometry total flavones, Syrups by HPLC linarin.
Large constituents in the Flos Chrysanthemi Indici extract mainly is the flavonoid composition, by document and standard substance location, tentatively think and adopt high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2010 D) to carry out assay by flavones ingredients such as containing linarin in the Flos Chrysanthemi Indici extract.Be filler with octadecylsilane chemically bonded silica; Acetonitrile-water-phosphoric acid system is mobile phase; The detection wavelength is 334nm.
2.2 result of the test
By the known composition of part is carried out assay, its content results sees Table 2-1
2-1 Flos Chrysanthemi Indici extract quality control assay result
| Lot number | The content of total flavones (%) | Determination of Linarin (%) |
| 110601 | 85.34 | 15.86 |
| 110901 | 88.46 | 16.54 |
| 120401 | 83.57 | 17.08 |
| Meansigma methods | 85.79 | 16.49 |
Flos Chrysanthemi Indici extract quality control index composition, general flavone content is with anhydrous rutin (C
27H
30O
16) meter, be no less than 80%; Monomer component linarin (C2
8H
32O
14) content is no less than 15%.
Claims (9)
1. the preparation method of a Flos Chrysanthemi Indici extract is characterized in that a kind of preparation method of Flos Chrysanthemi Indici extract, specifically according to the following steps preparation:
One, gets the Flos Chrysanthemi Indici Chinese crude drug, decoct 3 times with deionized water, each 1h, for the first time the quality of deionized water is 16 ~ 20 times of Flos Chrysanthemi Indici Chinese crude drug, for the second time the quality of deionized water is 12 ~ 16 times of Flos Chrysanthemi Indici Chinese crude drug, the quality of deionized water is 12 ~ 16 times of Flos Chrysanthemi Indici Chinese crude drug for the third time, merges 3 times decoction liquor, and reconcentration is to take the clear paste of 70 ℃ of relative densities as 1.10～1.14;
Two, in the clear paste of step 1 acquisition, add water, adding volume behind the water and the mass ratio of Flos Chrysanthemi Indici Chinese crude drug is 2L:1kg, be that 10% sodium hydroxide solution is regulated pH value to 6.5～7.0 with mass concentration again, leave standstill 12h ~ 24h, collect supernatant, regulate pH value to 2.0～3.0 with hydrochloric acid solution again, leave standstill again 12h ~ 24h, collect supernatant liquid;
Three, the supernatant liquid of step 2 being collected is crossed polyamide resin column, the mass ratio of polyamide and Flos Chrysanthemi Indici Chinese crude drug is 1:2.5, carry out eluting with deionized water again, the deionized water volume that eluting is used is 6 ~ 10 column volumes, it is 65% ~ 85% alcoholic solution eluting resin column that water lotion discards rear use volumetric concentration, the volumes of aqueous ethanol that eluting is used is 5 column volumes, collects ethanol elution;
Four, ethanol elution is carried out the distilling under reduced pressure Recycled ethanol, with sodium hydroxide solution adjust pH 6.0 ~ 7.0, concentrated, drying under reduced pressure namely obtains Flos Chrysanthemi Indici extract, finishes the preparation method of Flos Chrysanthemi Indici extract.
2. the preparation method of a kind of Flos Chrysanthemi Indici extract according to claim 1, the quality that it is characterized in that the deionized water first time is 18 ~ 19 times of Flos Chrysanthemi Indici Chinese crude drug, for the second time the quality of deionized water is 14 ~ 15 times of Flos Chrysanthemi Indici Chinese crude drug, and the quality of deionized water is 14 ~ 15 times of Flos Chrysanthemi Indici Chinese crude drug for the third time.
3. the preparation method of a kind of Flos Chrysanthemi Indici extract according to claim 2, the mass concentration that it is characterized in that the described hydrochloric acid solution of step 2 is 5%.
4. the preparation method of a kind of Flos Chrysanthemi Indici extract according to claim 3, the volumetric concentration that it is characterized in that the described alcoholic solution of step 3 is 70% ~ 80%.
5. the preparation method of a kind of Flos Chrysanthemi Indici extract according to claim 3, the volumetric concentration that it is characterized in that the described alcoholic solution of step 3 is 75%.
6. the preparation method of a kind of Flos Chrysanthemi Indici extract according to claim 5, the mass concentration that it is characterized in that the described sodium hydroxide solution of step 4 is 10%.
7. the preparation method of a kind of Flos Chrysanthemi Indici extract according to claim 6 is characterized in that adjust pH 6.5 ~ 6.8 in the step 4.
8. the preparation method of a kind of Flos Chrysanthemi Indici extract according to claim 7 is characterized in that the described drying under reduced pressure temperature of step 4 is 60 ℃ ~ 80 ℃, and the drying under reduced pressure time is 6h ~ 10h.
9. the preparation method of a kind of Flos Chrysanthemi Indici extract according to claim 7 is characterized in that the described drying under reduced pressure temperature of step 4 is 65 ℃ ~ 75 ℃, and the drying under reduced pressure time is 7h ~ 9h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104056342A (en) * | 2013-09-07 | 2014-09-24 | 福州力为康医药技术有限公司 | Physical cooling device |
| CN104177462A (en) * | 2014-09-01 | 2014-12-03 | 重庆工商大学 | Method for extracting refined rutin from magnolia petals |
| CN105062130A (en) * | 2015-08-11 | 2015-11-18 | 浙江理工大学 | Preparation method of wild chrysanthemum natural dye and preparation of anti-bacterial textiles adopting wild chrysanthemum natural dye |
-
2012
- 2012-11-23 CN CN 201210482811 patent/CN102920767A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104056342A (en) * | 2013-09-07 | 2014-09-24 | 福州力为康医药技术有限公司 | Physical cooling device |
| CN104056342B (en) * | 2013-09-07 | 2016-07-06 | 福州力为康医药技术有限公司 | Physical hypothermal device |
| CN104177462A (en) * | 2014-09-01 | 2014-12-03 | 重庆工商大学 | Method for extracting refined rutin from magnolia petals |
| CN104177462B (en) * | 2014-09-01 | 2016-04-13 | 重庆工商大学 | A kind of method of Hydrolysis kinetics rutin from yulan petal |
| CN105062130A (en) * | 2015-08-11 | 2015-11-18 | 浙江理工大学 | Preparation method of wild chrysanthemum natural dye and preparation of anti-bacterial textiles adopting wild chrysanthemum natural dye |
| CN105062130B (en) * | 2015-08-11 | 2018-05-22 | 浙江理工大学 | A kind of preparation method of wild chrysanthemum natural dye and its preparation of antimicrobial form textile |
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Application publication date: 20130213 |