CN102285976A - Method for extracting isoorientin from bamboo leaf flavones - Google Patents
Method for extracting isoorientin from bamboo leaf flavones Download PDFInfo
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- CN102285976A CN102285976A CN2011102978477A CN201110297847A CN102285976A CN 102285976 A CN102285976 A CN 102285976A CN 2011102978477 A CN2011102978477 A CN 2011102978477A CN 201110297847 A CN201110297847 A CN 201110297847A CN 102285976 A CN102285976 A CN 102285976A
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- isorientin
- folium bambosae
- bambosae flavone
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Abstract
The invention discloses a method for extracting isoorientin from bamboo leaf flavones, which comprises the following steps: (1) dissolving bamboo leaf flavones in anhydrous alcohol, and filtering to obtain a crude isoorientin extract; and (2) mixing the crude isoorientin extract with resin columns, eluting, separating and purifying, and recrystallizing. The isoorientin extracted by the method disclosed by the invention is a natural extract with high purity, has antioxidation myocardial, anti-myocardial ischemia and antihypoxic effects, and can be used in medicines, food and health products.
Description
Technical field
The invention belongs to the extracting and purifying method of isorientin, particularly a kind of method of from Folium Bambosae flavone, extracting isorientin.
Background technology
Folium Bambosae flavone is to be extracted by the leaf of bamboo, has anti-oxidant, the anti-ageing effect of waiting for a long time, and is emerging functional food additives; Be based on charcoal glycosides flavones in the Folium Bambosae flavone, wherein four kinds of main charcoal glycosides flavones are respectively orientin (Orientin), and isorientin (Isoorientin) is herded chaste tree glycosides (Vitexin) and the different chaste tree glycosides (Isoviextin) of herding.
Isorientin (Isoorientin) also claims Lutonaretin, is the isomers of orientin, yellow crystal, molecular formula: C21H20O11, molecular weight: 448.38, dissolve in organic solvents such as methyl alcohol, ethanol, Virahol, n-propyl alcohol, fusing point: 230 ℃～232 ℃.Modern study shows that isorientin has significant protective effect to myocardial ischemia, anoxic.
The common extraction source of isorientin is Polygonum orientale (the Gan Zao Guo Miho and the stem and branch with leaf of polygonaceae plant Polygonum knotweed (Polygonum orientale L.)); We discover in the Folium Bambosae flavone isorientin content generally more than 2%, and Folium Bambosae flavone derives from the leaf of bamboo, extract the safer cheapness of raw material, and natural resources can be utilized more fully.
Use the mixing of polyamide resin, two kinds of resins of silica gel, make isorientin be easier to separated purifying.
Summary of the invention
The objective of the invention is to make full use of the natural resources, a kind of method of extracting isorientin from Folium Bambosae flavone is provided.
Technical scheme of the present invention is summarized as follows:
From Folium Bambosae flavone, extract the method for isorientin, comprise the steps:
(1) with Folium Bambosae flavone, at 35 ℃, the feed liquid mass ratio is under the condition of 1:5～10, uses anhydrous alcohol solution, and the middling speed filter paper filtering gets the isorientin crude extract;
(2) with the isorientin crude extract, last hybrid resin post, concentration expressed in percentage by volume with 3 times of column volumes is 80% aqueous ethanolic solution, the concentration expressed in percentage by volume of 4 times of column volumes is 40%～60% Virahol ethanolic soln, the concentration expressed in percentage by volume of 5 times of column volumes is that 90% Virahol ethanolic soln carries out wash-out, the collected volume percentage concentration is 90% Virahol ethanolic soln elutriant, be evaporated to pol 30%, add isopyknic deionized water, stir evenly, crystallization is 7 hours under 20 ℃ of conditions, inhales and goes supernatant liquor, crystallization to add isopyknic anhydrous alcohol solution, be evaporated to pol 30%, add isopyknic deionized water, stir evenly, crystallization is 7 hours under 20 ℃ of conditions, filter, crystallization is washed till with deionized water does not have the alcohol flavor, and drying under reduced pressure under 60 ℃ of conditions promptly obtains the isorientin behind the purifying.Described hybrid resin is the mixing of polyamide resin, two kinds of resins of silica gel.
Described raw material Folium Bambosae flavone is the Folium Bambosae flavone of isorientin content 〉=0.5% that extracts in the leaf of bamboo.
Described solid-liquid ratio is 1:5～10.
Described hybrid resin is the mixing of polyamide resin, two kinds of resins of silica gel, and mixing quality is than being 2:8.
Described polyamide resin model is: the 30-60 order; The 60-100 order.
Described silica gel is column chromatography silica gel, and model is: the 60-100 order.
Embodiment
Extract the method for isorientin below by specific embodiment explanation the present invention from Folium Bambosae flavone, following description only is in order to make those skilled in the art understand the present invention better, but does not limit the present invention in any way.
Embodiment 1
From Folium Bambosae flavone, extract the method for isorientin, comprise the steps:
(1) with Folium Bambosae flavone, at 35 ℃, the feed liquid mass ratio is under the condition of 1:5, uses anhydrous alcohol solution, and the middling speed filter paper filtering gets the isorientin crude extract;
(2) with the isorientin crude extract, last hybrid resin post, hybrid resin is that polyamide resin 30-60 order and the column chromatography silica gel 60-100 order of 2:8 formed by mass ratio, concentration expressed in percentage by volume with 3 times of column volumes is 80% aqueous ethanolic solution, the concentration expressed in percentage by volume of 4 times of column volumes is 40% Virahol ethanolic soln, the concentration expressed in percentage by volume of 5 times of column volumes is that 90% Virahol ethanolic soln carries out wash-out, the collected volume percentage concentration is 90% Virahol ethanolic soln elutriant, be evaporated to pol 30%, add isopyknic deionized water, stir evenly, crystallization is 7 hours under 20 ℃ of conditions, supernatant liquor is removed in suction, crystallization adds isopyknic anhydrous alcohol solution, is evaporated to pol 30%, adds isopyknic deionized water, stir evenly, crystallization is 7 hours under 20 ℃ of conditions, filters, and crystallization is washed till with deionized water does not have the alcohol flavor, drying under reduced pressure under 60 ℃ of conditions promptly obtains the isorientin behind the purifying.Isorientin content is 97.3%.
Embodiment 2
From Folium Bambosae flavone, extract the method for isorientin, comprise the steps:
(1) with Folium Bambosae flavone, at 35 ℃, the feed liquid mass ratio is under the condition of 1:7, uses anhydrous alcohol solution, and the middling speed filter paper filtering gets the isorientin crude extract;
(2) with the isorientin crude extract, last hybrid resin post, hybrid resin is that polyamide resin 60-100 order and the column chromatography silica gel 60-100 order of 2:8 formed by mass ratio, concentration expressed in percentage by volume with 3 times of column volumes is 80% aqueous ethanolic solution, the concentration expressed in percentage by volume of 4 times of column volumes is 60% Virahol ethanolic soln, the concentration expressed in percentage by volume of 5 times of column volumes is that 90% Virahol ethanolic soln carries out wash-out, the collected volume percentage concentration is 90% Virahol ethanolic soln elutriant, be evaporated to pol 30%, add isopyknic deionized water, stir evenly, crystallization is 7 hours under 20 ℃ of conditions, supernatant liquor is removed in suction, crystallization adds isopyknic anhydrous alcohol solution, is evaporated to pol 30%, adds isopyknic deionized water, stir evenly, crystallization is 7 hours under 20 ℃ of conditions, filters, and crystallization is washed till with deionized water does not have the alcohol flavor, drying under reduced pressure under 60 ℃ of conditions promptly obtains the isorientin behind the purifying.Isorientin content is 98.6%.
Embodiment 3
From Folium Bambosae flavone, extract the method for isorientin, comprise the steps:
(1) with Folium Bambosae flavone, at 35 ℃, the feed liquid mass ratio is under the condition of 1:10, uses anhydrous alcohol solution, and the middling speed filter paper filtering gets the isorientin crude extract;
(2) with the isorientin crude extract, last hybrid resin post, hybrid resin is that polyamide resin 60-100 order and the column chromatography silica gel 60-100 order of 2:8 formed by mass ratio, concentration expressed in percentage by volume with 3 times of column volumes is 80% aqueous ethanolic solution, the concentration expressed in percentage by volume of 4 times of column volumes is 50% Virahol ethanolic soln, the concentration expressed in percentage by volume of 5 times of column volumes is that 90% Virahol ethanolic soln carries out wash-out, the collected volume percentage concentration is 90% Virahol ethanolic soln elutriant, be evaporated to pol 30%, add isopyknic deionized water, stir evenly, crystallization is 7 hours under 20 ℃ of conditions, supernatant liquor is removed in suction, crystallization adds isopyknic anhydrous alcohol solution, is evaporated to pol 30%, adds isopyknic deionized water, stir evenly, crystallization is 7 hours under 20 ℃ of conditions, filters, and crystallization is washed till with deionized water does not have the alcohol flavor, drying under reduced pressure under 60 ℃ of conditions promptly obtains the isorientin behind the purifying.Isorientin content is 98.4%.
Embodiment 4
From Folium Bambosae flavone, extract the method for isorientin, comprise the steps:
(1) with Folium Bambosae flavone, at 35 ℃, the feed liquid mass ratio is under the condition of 1:9, uses anhydrous alcohol solution, and the middling speed filter paper filtering gets the isorientin crude extract;
(2) with the isorientin crude extract, last hybrid resin post, hybrid resin is that polyamide resin 30-60 order and the column chromatography silica gel 60-100 order of 2:8 formed by mass ratio, concentration expressed in percentage by volume with 3 times of column volumes is 80% aqueous ethanolic solution, the concentration expressed in percentage by volume of 4 times of column volumes is 45% Virahol ethanolic soln, the concentration expressed in percentage by volume of 5 times of column volumes is that 90% Virahol ethanolic soln carries out wash-out, the collected volume percentage concentration is 90% Virahol ethanolic soln elutriant, be evaporated to pol 30%, add isopyknic deionized water, stir evenly, crystallization is 7 hours under 20 ℃ of conditions, supernatant liquor is removed in suction, crystallization adds isopyknic anhydrous alcohol solution, is evaporated to pol 30%, adds isopyknic deionized water, stir evenly, crystallization is 7 hours under 20 ℃ of conditions, filters, and crystallization is washed till with deionized water does not have the alcohol flavor, drying under reduced pressure under 60 ℃ of conditions promptly obtains the isorientin behind the purifying.Isorientin content is 97.4%.
Embodiment 5
From Folium Bambosae flavone, extract the method for isorientin, comprise the steps:
(1) with Folium Bambosae flavone, at 35 ℃, the feed liquid mass ratio is under the condition of 1:6, uses anhydrous alcohol solution, and the middling speed filter paper filtering gets the isorientin crude extract;
(2) with the isorientin crude extract, last hybrid resin post, hybrid resin is that polyamide resin 60-100 order and the column chromatography silica gel 60-100 order of 2:8 formed by mass ratio, concentration expressed in percentage by volume with 3 times of column volumes is 80% aqueous ethanolic solution, the concentration expressed in percentage by volume of 4 times of column volumes is 55% Virahol ethanolic soln, the concentration expressed in percentage by volume of 5 times of column volumes is that 90% Virahol ethanolic soln carries out wash-out, the collected volume percentage concentration is 90% Virahol ethanolic soln elutriant, be evaporated to pol 30%, add isopyknic deionized water, stir evenly, crystallization is 7 hours under 20 ℃ of conditions, supernatant liquor is removed in suction, crystallization adds isopyknic anhydrous alcohol solution, is evaporated to pol 30%, adds isopyknic deionized water, stir evenly, crystallization is 7 hours under 20 ℃ of conditions, filters, and crystallization is washed till with deionized water does not have the alcohol flavor, drying under reduced pressure under 60 ℃ of conditions promptly obtains the isorientin behind the purifying.Isorientin content is 98.7%.
Embodiment 6
From Folium Bambosae flavone, extract the method for isorientin, comprise the steps:
(1) with Folium Bambosae flavone, at 35 ℃, the feed liquid mass ratio is under the condition of 1:8, uses anhydrous alcohol solution, and the middling speed filter paper filtering gets the isorientin crude extract;
(2) with the isorientin crude extract, last hybrid resin post, hybrid resin is that polyamide resin 30-60 order and the column chromatography silica gel 60-100 order of 2:8 formed by mass ratio, concentration expressed in percentage by volume with 3 times of column volumes is 80% aqueous ethanolic solution, the concentration expressed in percentage by volume of 4 times of column volumes is 45% Virahol ethanolic soln, the concentration expressed in percentage by volume of 5 times of column volumes is that 90% Virahol ethanolic soln carries out wash-out, the collected volume percentage concentration is 50% Virahol ethanolic soln elutriant, be evaporated to pol 30%, add isopyknic deionized water, stir evenly, crystallization is 7 hours under 20 ℃ of conditions, supernatant liquor is removed in suction, crystallization adds isopyknic anhydrous alcohol solution, is evaporated to pol 30%, adds isopyknic deionized water, stir evenly, crystallization is 7 hours under 20 ℃ of conditions, filters, and crystallization is washed till with deionized water does not have the alcohol flavor, drying under reduced pressure under 60 ℃ of conditions promptly obtains the isorientin behind the purifying.Isorientin content is 97.7%.
Embodiment 7
From Folium Bambosae flavone, extract the method for isorientin, comprise the steps:
(1) with Folium Bambosae flavone, at 35 ℃, the feed liquid mass ratio is under the condition of 1:5, uses anhydrous alcohol solution, and the middling speed filter paper filtering gets the isorientin crude extract;
(2) with the isorientin crude extract, last hybrid resin post, hybrid resin is that polyamide resin 60-100 order and the column chromatography silica gel 60-100 order of 2:8 formed by mass ratio, concentration expressed in percentage by volume with 3 times of column volumes is 80% aqueous ethanolic solution, the concentration expressed in percentage by volume of 4 times of column volumes is 40% Virahol ethanolic soln, the concentration expressed in percentage by volume of 5 times of column volumes is that 90% Virahol ethanolic soln carries out wash-out, the collected volume percentage concentration is 90% Virahol ethanolic soln elutriant, be evaporated to pol 30%, add isopyknic deionized water, stir evenly, crystallization is 7 hours under 20 ℃ of conditions, supernatant liquor is removed in suction, crystallization adds isopyknic anhydrous alcohol solution, is evaporated to pol 30%, adds isopyknic deionized water, stir evenly, crystallization is 7 hours under 20 ℃ of conditions, filters, and crystallization is washed till with deionized water does not have the alcohol flavor, drying under reduced pressure under 60 ℃ of conditions promptly obtains the isorientin behind the purifying.Isorientin content is 98.1%.
Claims (7)
1. from Folium Bambosae flavone, extract the method for isorientin, it is characterized in that comprising the steps:
(1) with Folium Bambosae flavone, at 35 ℃, the feed liquid mass ratio is under the condition of 1:5～10, uses anhydrous alcohol solution, and the middling speed filter paper filtering gets the isorientin crude extract;
(2) with the isorientin crude extract, last hybrid resin post, concentration expressed in percentage by volume with 3 times of column volumes is 80% aqueous ethanolic solution, the concentration expressed in percentage by volume of 4 times of column volumes is 40%～60% Virahol ethanolic soln, the concentration expressed in percentage by volume of 5 times of column volumes is that 90% Virahol ethanolic soln carries out wash-out, the collected volume percentage concentration is 90% Virahol ethanolic soln elutriant, be evaporated to pol 30%, add isopyknic deionized water, stir evenly, crystallization is 7 hours under 20 ℃ of conditions, inhales and goes supernatant liquor, crystallization to add isopyknic anhydrous alcohol solution, be evaporated to pol 30%, add isopyknic deionized water, stir evenly, crystallization is 7 hours under 20 ℃ of conditions, filter, crystallization is washed till with deionized water does not have the alcohol flavor, and drying under reduced pressure under 60 ℃ of conditions promptly obtains the isorientin behind the purifying.
2. according to the described hybrid resin of claim 1 mixing of polyamide resin, two kinds of resins of silica gel.
3. from Folium Bambosae flavone, extract the method for isorientin according to claim 1, it is characterized in that described raw material Folium Bambosae flavone is the Folium Bambosae flavone of isorientin content 〉=0.5% that extracts in the leaf of bamboo.
4. according to the described method of from Folium Bambosae flavone, extracting isorientin of claim 1, it is characterized in that described solid-liquid ratio is 1:5～10.
5. according to the described method of extracting isorientin from Folium Bambosae flavone of claim 1, it is characterized in that described hybrid resin is the mixing of polyamide resin, two kinds of resins of silica gel, mixing quality is than being 2:8.
6. according to claim 1 or the 4 described methods of from Folium Bambosae flavone, extracting isorientin, it is characterized in that described polyamide resin model is: the 30-60 order; The 60-100 order.
7. according to claim 1 or the 4 described methods of extracting isorientin from Folium Bambosae flavone, it is characterized in that described silica gel is column chromatography silica gel, model is: the 60-100 order.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103044410A (en) * | 2012-12-14 | 2013-04-17 | 湘西自治州奥瑞克医药化工有限责任公司 | Production process for extracting isoorientin from bamboo product waste |
| CN104370895A (en) * | 2014-08-22 | 2015-02-25 | 江苏汉邦科技有限公司 | Orientin and homoorientin preparation method |
| CN104650052A (en) * | 2015-02-13 | 2015-05-27 | 宁波杰顺生物科技有限公司 | Method for preparing isoorientin extract from bamboo leaves |
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| CN103044410A (en) * | 2012-12-14 | 2013-04-17 | 湘西自治州奥瑞克医药化工有限责任公司 | Production process for extracting isoorientin from bamboo product waste |
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| CN104370895B (en) * | 2014-08-22 | 2016-06-29 | 江苏汉邦科技有限公司 | A kind of preparation method of orientin and Lutonaretin |
| CN104650052A (en) * | 2015-02-13 | 2015-05-27 | 宁波杰顺生物科技有限公司 | Method for preparing isoorientin extract from bamboo leaves |
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Application publication date: 20111221 |