CN1597678A - Extraction method of hawthorn leaf total flarone - Google Patents
Extraction method of hawthorn leaf total flarone Download PDFInfo
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- CN1597678A CN1597678A CN 03133957 CN03133957A CN1597678A CN 1597678 A CN1597678 A CN 1597678A CN 03133957 CN03133957 CN 03133957 CN 03133957 A CN03133957 A CN 03133957A CN 1597678 A CN1597678 A CN 1597678A
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- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 abstract description 2
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- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
A process for extracting the hawthorn leaf flavone includes such steps as immersing the hawthorn leaves in water, decocting, filtering, vacuum concentrating, adsorbing by macroreticular resin, alcohol eluting, adding diatomite in eluting liquid, heating, reflux decoloring, removing impurities by exchange resin, recovering alcohol, and drying.
Description
Technical field
The present invention relates to the extracting method of plant total flavones, exactly is the extracting method of Folium Crataegi total flavones.
Background technology
Pharmacology activity research shows: the Folium Crataegi total flavones extract can reduce the blood pressure of Hypertensive Rats, and it is reduced to normal arterial pressure, to the almost not influence of blood pressure with normal arterial pressure rat; The Folium Crataegi total flavones extract has the effect of obvious reduction rat blood serum total cholesterol and triglyceride (TG) (P＜0.05), and is certain dose-effect relationship; Lipid-lowering test to bait hyperlipidemia rabbit shows that the Folium Crataegi total flavones extract can significantly reduce (TC) in the hyperlipidemia rabbit anteserum (P＜0.05), and simultaneously the Folium Crataegi total flavones extract has and prevents higher fatty acid disease effect preferably.The author carries out the antiplatelet aggregative activity experiment to separate 7 chromocor compounds that obtain from the Folium Crataegi total flavones extract.The result shows: the C-glycoside compound still is that the O-glycoside compound all has certain antiplatelet aggregative activity.Therefore, the Folium Crataegi total flavones extract is as a kind of physiologically active substance, uses very extensively, not only can be used as food but also can be used as the preparation raw material of multiple medicine, various healthcare products.Because the Folium Crataegi total flavones extract has high using value and prospect.So, in the last few years, comprised that the expert of many countries of China, scholar have carried out extensive and deep research to the method for extracting Fructus Crataegi total flavones from Howthorn Leaf, obtained gratifying achievements.But the most frequently used method of conclude is alcohol extract or the water extract with Howthorn Leaf to suspend in water, and uses the solvent extraction of opposed polarity successively, and solvent commonly used has chloroform, ethyl acetate and water-saturated n-butanol.Fructus Crataegi total flavones focuses mostly in n-butanol layer.The reclaim under reduced pressure propyl carbinol; Medicinal extract concentration is 95% dissolve with ethanol, and makes it pass through active carbon column; Collect effluent liquid and decompression recycling ethanol, make finished product.The subject matter of utilizing this method to produce the Fructus Crataegi total flavones existence is: (1) product cost is higher, (2) impurity in the product, particularly content of harmful is higher, wherein heavy metal content surpasses 5ppm, pesticide residue is greater than 10ppb, surpass prescribed limit, simultaneously residual toxicity solvent, n-butanol etc. inevitably also.
Summary of the invention
The objective of the invention is to provide for people a kind of extracting method of Folium Crataegi total flavones, so that make the Fructus Crataegi total flavones cost that utilizes this method to produce low, foreign matter content is few, and makes its production process environmentally safe.
The method for preparing Fructus Crataegi total flavones provided by the invention comprises following processing step:
A: Howthorn Leaf is soaked and is decocted
(A) be 1: 8～16 in Howthorn Leaf, to add entry by the ratio of weight and number of Howthorn Leaf and tap water, soak at room temperature 0.5～2 hour, then, the mixture heating up to 70 ℃～100 ℃ with both is incubated 1～3 hour, afterwards, residue obtained liquid;
(B) be 1: 6～10 in the slag that processing step (A) leaches, to add entry by the ratio of weight and number of described Howthorn Leaf and water, and, be incubated 1～2.5 hour both mixture heating up to 70 ℃～100 ℃, afterwards, residue obtained liquid;
(C) be 1: 6～8 in the slag that processing step (B) leaches, to add entry by the ratio of weight and number of described Howthorn Leaf and water, and, be incubated 1～1.5 hour both mixture heating up to 70 ℃～100 ℃, afterwards, residue obtained liquid;
B: liquid concentration
The liquid mixing that will be respectively produce by described each processing step (A), (B), (C) is the back concentrating under reduced pressure together, is to end at 1～3: 1 until the ratio of its weight and described Howthorn Leaf weight;
C: absorb-elute
Macroporous adsorptive resins after making liquid after concentrating by activated processing, total flavones in the liquid is adsorbed by resin column, and discard effluent liquid, be that 0.1～1: 1 ratio is taken the distilled water flushing resin column in distilled water and the ratio that concentrates the volume of back liquid again, discard effluent liquid, continuing with concentration is that 50～70% ethanol cleans resin column, absorption total flavones is thereon ended by wash-out fully, and collect elutriant;
D: decolouring
In the ratio of weight and number of medicinal diatomite and described Howthorn Leaf is that 2～6: 100 ratio is taken medicinal diatomite and added in the described elutriant, and reflux 20～60 minutes then, makes this mixture filter by clear slag plate, and collects filtrate;
E: impurity elimination
Described filtrate is passed through in the Zeo-karb that is one another in series and anionite-exchange resin, make wherein ion and heavy metal by filtering, and collection filtrate;
F: finished product reclaims, drying
Recovery process E makes the ethanol in the filtrate, after the remaining material drying, can obtain the Fructus Crataegi total flavones finished product.
Compared with the prior art the present invention has the following advantages after realizing: 1. product cost is low; 2. the heavy metal content in the finished product is less than 5ppm, and pesticide residue is less than 10ppb, thereby its foreign matter content is low; 3. eliminate the residual of toxic solvents propyl carbinol; 4. production process environmentally safe.
Specific embodiment
Embodiment 1
A: Howthorn Leaf is soaked and is decocted
(A) get Howthorn Leaf 1kg and put into container, in container, add 8 liters in tap water again, soak at room temperature 1 hour, then, the mixture heating up to 70 ℃ with both is incubated 3 hours, afterwards, residue obtained liquid;
(B) in the slag that processing step (A) leaches, add 6 liters in tap water, and, be incubated 2.5 hours both mixture heating up to 70 ℃, afterwards, residue obtained liquid;
(C) in the slag that processing step (B) leaches, add 6 liters in tap water, and, be incubated 1.5 hours both mixture heating up to 70 ℃, afterwards, residue obtained liquid;
B: liquid concentration
The back together concentrating under reduced pressure of liquid mixing that to produce by described each processing step (A), (B), (C) respectively is concentrated into about 3 until it and only is upgraded to;
C: absorption, wash-out
Macroporous adsorptive resins after making liquid after concentrating by activated processing, total flavones in the liquid is adsorbed by resin column, and discard effluent liquid, use 3 liters of distilled water flushing resin columns again, discard effluent liquid, continuing with concentration is that 70% ethanol cleans resin column, absorption total flavones is thereon ended by wash-out fully, and collect elutriant;
D: decolouring
Medicinal diatomite 0.03kg is added in the described elutriant, be heated to 70 ℃, and both mixtures were refluxed 45 minutes, then, this mixture is filtered by clear slag plate, and collect filtrate at this temperature condition;
E: impurity elimination
Described filtrate is passed through in the 732 type Zeo-karbs that are one another in series and 717 type anionite-exchange resin, make wherein ion and heavy metal by filtering, and collection filtrate;
F: finished product reclaims, drying
Recovery process E makes the ethanol in the filtrate, after the remaining material drying, can obtain the Folium Crataegi total flavones finished product.
Embodiment 2
A: Howthorn Leaf is soaked and is decocted
(A) get Howthorn Leaf 1kg and put into container, in container, add 16 liters of entry again, soak at room temperature 2 hours, then, the mixture heating up to 80 ℃ with both is incubated 2 hours, afterwards, residue obtained liquid;
(B) in the slag that processing step (A) leaches, add 10 liters of entry, and, be incubated 2 hours both mixture heating up to 80 ℃, afterwards, residue obtained liquid;
(C) in the slag that processing step (B) leaches, add 8 liters of entry, and, be incubated 1.2 hours both mixture heating up to 80 ℃, afterwards, residue obtained liquid;
B: liquid concentration
The back together concentrating under reduced pressure of liquid mixing that to produce by described each processing step (A), (B), (C) respectively is concentrated into about 1 until it and only is upgraded to;
C: absorption, wash-out
Macroporous adsorptive resins after making liquid after concentrating by activated processing, total flavones in the liquid is adsorbed by resin column, and discard effluent liquid, use 0.5 liter of distilled water flushing resin column again, discard effluent liquid, continuing with concentration is that 50% ethanol cleans resin column, absorption total flavones is thereon ended by wash-out fully, and collect elutriant;
D: decolouring
Medicinal diatomite 0.06kg is added in the described elutriant, be heated to 80 ℃, and both mixtures were refluxed 60 minutes, then, this mixture is filtered by clear slag plate, and collect filtrate at this temperature condition;
E: impurity elimination
Described filtrate is passed through in the 732 type Zeo-karbs that are one another in series and 717 type anionite-exchange resin, make wherein ion and heavy metal by filtering, and collection filtrate;
F: finished product reclaims, drying
Recovery process E makes the ethanol in the filtrate, after the remaining material drying, can obtain the Folium Crataegi total flavones finished product.
Embodiment 3
A: Howthorn Leaf is soaked and is decocted
(A) get Howthorn Leaf 1kg and put into container, in container, add 12 liters of entry again, soak at room temperature 0.5 hour, then, the mixture heating up to 100 ℃ with both is incubated 1 hour, afterwards, residue obtained liquid;
(B) in the slag that processing step (A) leaches, add 8 liters of entry, and, be incubated 1 hour both mixture heating up to 100 ℃, afterwards, residue obtained liquid;
(C) in the slag that processing step (B) leaches, add 7 liters of entry, and, be incubated 1 hour both mixture heating up to 100 ℃, afterwards, residue obtained liquid;
B: liquid concentration
The back together concentrating under reduced pressure of liquid mixing that to produce by described each processing step (A), (B), (C) respectively is concentrated into about 2 until it and only is upgraded to;
C: absorption, wash-out
Macroporous adsorptive resins after making liquid after concentrating by activated processing, total flavones in the liquid is adsorbed by resin column, and discard effluent liquid, use 0.2 liter of distilled water flushing resin column again, discard effluent liquid, continuing with concentration is that 70% ethanol cleans resin column, absorption total flavones is thereon ended by wash-out fully, and collect elutriant;
D: decolouring
Medicinal diatomite 0.02kg is added in the described elutriant, be heated to 75 ℃, and both mixtures were refluxed 20 minutes, then, this mixture is filtered by clear slag plate, and collect filtrate at this temperature condition;
E: impurity elimination
Described filtrate is passed through in the 732 type Zeo-karbs that are one another in series and 717 type anionite-exchange resin, make wherein ion and heavy metal by filtering, and collection filtrate;
F: finished product reclaims, drying
Recovery process E makes the ethanol in the filtrate, after the remaining material drying, can obtain the Folium Crataegi total flavones finished product.
The Folium Crataegi total flavones product of producing by the present embodiment method:
1. yield (weight percent) is 4.8～5.5%.
2. detect the content of this product 〉=80% by colorimetry.
3. pressing the HPLC method detects: (1) Folium Crataegi extract after acid hydrolysis, the content of Vitexin be 5.44% (2) Folium Crataegi extract after acid hydrolysis, the content of Quercetin is 2.30%
4. composition: isolation identification 20 kinds of flavone components, be respectively PinnatifidaA; PinnatifidaB; PinnatifidaC; PinnatifidaD; PinnatifidaE; PinnatifidaF; 8-C-β-D-(2 "-the O-ethanoyl) the glucofuranose apigenin; 3 "-ethanoyl Vitexin; Vitexin; 6 "-O-ethanoyl Vitexin; 2 "-O-ethanoyl Vitexin; 2 "-O-rhamanopyranosyl Vitexin; Quercetin; 3-O-β-D-glucopyranosyl Quercetin; 3-O-β-D-galactopyranose base Quercetin; 3-O-β-D-glucopyranosyl (6 → 1) 1)-a-L-rhamnosyl Quercetin; 3-O-β-D-galactopyranose (6 → 1) 1)-a-L-rhamnosyl Quercetin; kaempferol; 7-O-a-L-rhamnosyl-3-O-β-D-Glucopyranose kaempferol; icarin.
5. foreign matter content: heavy metal≤5ppm, pesticide residue, both: the residual quantity of " 666 ", " DDT ", " 5 chloronitrobenzene " all≤10ppb
Colorimetry of the present invention can be referring to pharmaceutical analysis magazines such as study of the Song Dynasty China, 1992; 12 (1): 28.
HPLC method of the present invention can be referring to Zhang Peicheng Shenyang Pharmaceutical University doctorate paper: the research of hawthorn chemical ingredients and pharmacologically active thereof (in September, 1999).
Claims (1)
1. the extracting method of a Folium Crataegi total flavones is characterized in that it is made up of following processing step:
A: Howthorn Leaf is soaked and is decocted
(A) ratio of weight and number of Howthorn Leaf and water is 1: 8～16, adds entry in Howthorn Leaf, soak at room temperature 0.5～2 hour, and then, the mixture heating up to 70 ℃～100 ℃ with both is incubated 1～3 hour, afterwards, residue obtained liquid;
(B) ratio of weight and number of described Howthorn Leaf and water is 1: 6～10 to add entry in the slag that processing step (A) leaches, and with both mixture heating up to 70 ℃～100 ℃, is incubated 1～2.5 hour, afterwards, and residue obtained liquid;
(C) be 1: 6～8 in the slag that processing step (B) leaches, to add entry by the ratio of weight and number of described Howthorn Leaf and water, and, be incubated 1～1.5 hour both mixture heating up to 70 ℃～100 ℃, afterwards, residue obtained liquid;
B: liquid concentration
The liquid mixing that will be respectively produce by described each processing step (A), (B), (C) is the back concentrating under reduced pressure together, is to end at 1～3: 1 until the ratio of its weight and described Howthorn Leaf weight;
C: absorb-elute
Macroporous adsorptive resins after making liquid after concentrating by activated processing, total flavones in the liquid is adsorbed by resin column, and discard effluent liquid, be that 0.1～1: 1 ratio is taken the distilled water flushing resin column in distilled water and the ratio that concentrates the volume of back liquid again, discard effluent liquid, continuing with concentration is that 50～70% ethanol cleans resin column, absorption total flavones is thereon ended by wash-out fully, and collect elutriant;
D: decolouring
In the ratio of weight and number of medicinal diatomite and described Howthorn Leaf is that 2～6: 100 ratio is taken medicinal diatomite and added in the described elutriant, and reflux 20～60 minutes then, makes this mixture filter by clear slag plate, and collects filtrate;
E: impurity elimination
Described filtrate is passed through in the Zeo-karb that is one another in series and anionite-exchange resin, make wherein ion and heavy metal by filtering, and collection filtrate;
F: finished product reclaims, drying
Recovery process E makes the ethanol in the filtrate, after the remaining material drying, can obtain the Fructus Crataegi total flavones finished product.
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| CN102755405A (en) * | 2012-07-02 | 2012-10-31 | 吉林金麦通制药有限公司 | Fructus crataegi leaf water extract, preparation containing same and preparation method pf fructus crataegi leaf water extract |
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| CN103242279A (en) * | 2013-05-16 | 2013-08-14 | 陕西科技大学 | Method for extracting and purifying flavonoid substances in hawthorn |
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| CN103181959A (en) * | 2013-03-27 | 2013-07-03 | 张宗升 | Traditional chinese medicine composition and preparation method thereof |
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| CN103405534A (en) * | 2013-07-08 | 2013-11-27 | 马洪兵 | Technique for extracting hawthorn leaf extract from hawthorn leaf |
| CN106831892A (en) * | 2017-03-20 | 2017-06-13 | 山东省分析测试中心 | The preparation method of flavones monomer in a kind of leaves of Hawthorn |
| CN106831892B (en) * | 2017-03-20 | 2020-05-15 | 山东省分析测试中心 | A kind of preparation method of flavonoid monomer in hawthorn leaves |
| CN108191762A (en) * | 2018-01-24 | 2018-06-22 | 湖南华诚生物资源股份有限公司 | A kind of extracting method of pure natural heavy metal free Huperzine Serrate P.E |
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