CN101606954A - From Herba Selaginellae, extract the method for purifying flavonoid substance - Google Patents
From Herba Selaginellae, extract the method for purifying flavonoid substance Download PDFInfo
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Abstract
The present invention relates to a kind of extracting method of effective components of Chinese medicinal, be specifically related to a kind ofly from Herba Selaginellae, to extract, the method for purifying flavonoid substance.After dry Herba Selaginellae pulverizing, sieving, use the ethanol water reflux, extract,, behind the filtered while hot extracting solution, ethanol is reclaimed in distilling under reduced pressure, and vacuum drying gets Herba Selaginellae extract to constant weight; Change the above-mentioned extract that obtains over to polyamide resin column, be that 10～60% ethanol aqueous wash removes decontamination earlier with volumetric concentration, the back is 70～90% ethanol water eluting with volumetric concentration, eluent flow rate is 0.5～2mL/min, collect eluent, ethanol is reclaimed in distilling under reduced pressure, and vacuum drying promptly gets the Herba Selaginellae Flavonoid substances to constant weight.General flavone content and yield that process of the present invention obtains are higher, and process safety is strong, and technology is simple, and production cost is low, is applicable to suitability for industrialized production.
Description
Technical field
The present invention relates to a kind of extracting method of effective components of Chinese medicinal, be specifically related to a kind ofly from Herba Selaginellae, to extract, the method for purifying flavonoid substance.
Background technology
Herba Selaginellae is a herbaceos perennial, belongs to the herb of fern Selaginaceae (Selaginellaceae) Selaginella (Selaginella) plant Herba Selaginellae, has another name called the grass of living forever and never die, nine dead Herba Hylothelephii Verticillatis, SHILIANHUA, Rohdea japonica Roth etc., is Chinese medicine.The version Pharmacopoeia of People's Republic of China recorded Herba Selaginellae [Selaginella tamariscina (Beauv.) Spring] and cushion Herba Selaginellae [Selaginella pulvinata (Hook et Grev.) Maxim.] in 2005, use as clinical standard medical material, its property is hot flat, have the promoting blood circulation to restore menstrual flow effect, be mainly used in the amenorrhea dysmenorrhea, injury from falling down, spit blood, metrorrhagia is had blood in stool, diseases such as proctoptosis.Modern pharmacology studies confirm that, the main effective ingredient of Herba Selaginellae is flavone compounds such as amentoflavone, hinokiflavone, Neocryptomerin, the effect that has anti peroxidation of lipid and remove free radical, can obviously reduce wastage of grain, etc. caused by rats oxygen speed and oxygen consumption, improve oxygen-resistant ability, coronary artery dilator; Improve hemorheological indexes, the inductive vascular endothelial cell damage of hemolytic phosphatidylcholine (LPC) is had protective effect.Therefore, the Herba Selaginellae total flavones is researched and developed as an effective site had important economic benefit and social benefit.Current, the single medicinal material effective ingredient just day by day comes into one's own as a kind of emerging product, and it is a support with modern extraction and separation technology, uses the quality controllable and stable extract and the preparation thereof of preparation technology's production of standard; Adopt by " Chinese crude drug quality of production management regulation " (GAP) requirement standardized planting and gather and the quality controllable Chinese crude drug processed is a raw material, use modern extractive technique, again by " Good Manufacturing Practice and Quality Control of Drug " (GMP) management mode improving the extract product of producing under the Quality Monitoring Control System with controlled quality standard, embodied the technological progress of Chinese medicine industry and the requirement of the modernization of Chinese medicine.
At present, domestic and international various document only is confined to the research to single component in the Herba Selaginellae, research to effective site is less, such as Zheng Xing etc. (cushion Herba Selaginellae The Chemical Constituents [J]. Chinese herbal medicine, 2001,32 (1): 17-18.) adopt alcohol heat reflux to extract and divide the position extraction then, with petroleum ether part and the ethyl acetate part that obtains, carry out silica gel column chromatography respectively, obtain 4 kinds of crystalline compounds.Dai Zhong etc. (chemical constitution study of Herba Selaginellae sinensis [J]. Chinese herbal medicine, 2001,32 (9): 784-785.) adopt 95% alcohol reflux, divide the position extraction then, the chloroform that obtains, ethyl acetate and n-butyl alcohol extract, each uses silica gel column chromatography after extracting partial concentration, obtains 4 kinds of crystalline compounds.These two kinds of methods all obtain single chemical constituent, are suitable for compound identification and research, be not suitable for the extraction of effective components of Chinese medicinal, and all use organic solvent in separation process, do not meet need of industrial production.
Chinese patent CN1562994A discloses a kind of amentoflavone preparation method of extract: dry Herba Selaginellae herb, alcohol reflux, vacuum concentration, utilize the styrene tyle macroporous adsorption resin adsorption and purification then promptly, the main component that the method obtains is an amentoflavone, final content 10～50%, and scope is wider, yield is low, makes troubles for the control and the stability of suitability for industrialized production content.Use macroporous adsorbent resin in this method separation process in addition, and do not relate to the mensuration residual to macroporous adsorbent resin, macroporous adsorbent resin is residual too much will to reduce safety greatly, be not suitable for being applied to suitability for industrialized production.
Summary of the invention
The yield that the objective of the invention is to solve total flavonoids substance in the Herba Selaginellae that exists in the existing extraction separation method to the Herba Selaginellae active ingredient is low, the residual extracting method that causes of the application of organic solvent, macroporous adsorbent resin is not suitable for technical problems such as suitability for industrialized production, and the free of contamination method that is suitable for the extracting of suitability for industrialized production, purifying flavonoid substance from Herba Selaginellae in a kind of yield height, production process of total flavonoids substance is provided.
The technical solution used in the present invention is as follows:
The method of extracting purifying flavonoid substance from Herba Selaginellae of the present invention is carried out according to the following steps:
(1) extracts: after dry Herba Selaginellae is pulverized, sieves, with volumetric concentration is 60～80% ethanol water reflux, extract, 2～3 times, merge ethanol extract, after the filtered while hot, ethanol is reclaimed in distillation under 0.05～0.1Mpa, in vacuum is 0.05～0.1Mpa, and temperature is to be dried to constant weight under 35～45 ℃, gets Herba Selaginellae extract;
(2) purification: the extract that step (1) is obtained changes polyamide resin column over to, be that 10～60% ethanol aqueous wash removes decontamination earlier with volumetric concentration, the back is 70～90% ethanol water eluting with volumetric concentration, eluent flow rate is 0.5～2mL/min, collect eluent, ethanol is reclaimed in distillation under 0.05～0.1Mpa, is 0.05～0.1Mpa in vacuum, temperature is to be dried to constant weight under 35～45 ℃, promptly gets the Herba Selaginellae Flavonoid substances.
In step (1), the consumption of ethanol water is 8～12 times of Herba Selaginellae weight, and the reflux, extract, temperature is 75～85 ℃, and extraction time is each 1.5～2.5h.
In step (2), the blade diameter length ratio of used polyamide resin column is 1: 4～8, and the polyamide particle size range is 60～100 orders; Applied sample amount is 45～55mg Herba Selaginellae extract on every 30mL polyamide; The consumption of ethanol water is 8～12 times of column volume amounts during the eluting remove impurity; The eluent consumption is 4～8 times of column volume amounts.
The present invention compared with prior art has following advantage:
(1) general flavone content and yield are higher: the Herba Selaginellae general flavone content that adopts the inventive method acquisition is greater than 60%, the total flavones yield is greater than 75%, the total flavones that is enriched to is except containing amentoflavone, also contain multiple flavone compounds such as Neocryptomerin, hinokiflavone, content is higher, good stability, productive rate is higher.
(2) process safety is strong: the whole technology solvent for use of the present invention is distilled water and ethanol, does not use poisonous organic reagent, has improved the safety of producing; In addition, this process using polyamide carries out separation and purification, and this resin is safe, is applicable to suitability for industrialized production.
(3) technology is simple, and production cost is low: the whole technology solvent for use of the present invention is distilled water and ethanol, and price is lower, has reduced production cost, is applicable to industrial mass production; In addition, this process using polyamide carries out separation and purification, this resin recycling rate of waterused height, and low price is applicable to suitability for industrialized production.
The specific embodiment
Below in conjunction with embodiment the present invention is elaborated, but therefore do not limit the present invention among the described scope of embodiments.
Embodiment 1
The method of extracting purifying flavonoid substance from Herba Selaginellae is carried out according to the following steps:
(1) extract: with dry Herba Selaginellae pulverize, sieve sieve for No. 3 after, with 8 times of Herba Selaginellae weight, volumetric concentration is 80% ethanol water reflux, extract, 3 times, and extracting temperature is 75 ℃, and extraction time is each 1.5h, merge ethanol extract, after the filtered while hot, ethanol is reclaimed in distillation under 0.05Mpa, at vacuum 0.05Mpa, temperature be 35 ℃ of following vacuum dryings to constant weight, Herba Selaginellae extract.
(2) purification: it is 1: 4 polyamide resin column that the extract that step (1) is obtained changes blade diameter length ratio over to, and the polyamide particle size range is 60～100 orders; Applied sample amount is a 45mg Herba Selaginellae extract on every 30mL polyamide.Be that 60% ethanol aqueous wash removes decontamination earlier with 8 times of column volume amount volumetric concentrations, the back is 90% ethanol water eluting with 4 times of column volume amount volumetric concentrations, eluent flow rate is 0.5mL/min, collect eluent, ethanol is reclaimed in distillation under 0.05Mpa, at vacuum 0.05Mpa, temperature be 35 ℃ of following vacuum dryings to constant weight, promptly get the Herba Selaginellae Flavonoid substances.
Adopt determined by ultraviolet spectrophotometry general flavone content and high effective liquid chromatography for measuring index composition amentoflavone content, general flavone content 62%, amentoflavone content 33.64%, total flavones yield 81.62%,
Embodiment 2
The method of extracting purifying flavonoid substance from Herba Selaginellae is carried out according to the following steps:
(1) extract: with dry Herba Selaginellae pulverize, sieve sieve for No. 3 after, with 12 times of Herba Selaginellae weight, volumetric concentration is 60% ethanol water reflux, extract, 2 times, and extracting temperature is 85 ℃, and extraction time is each 2.5h, merge ethanol extract, after the filtered while hot, ethanol is reclaimed in distillation under 0.1Mpa, at vacuum 0.1Mpa, temperature be 45 ℃ of following vacuum dryings to constant weight, Herba Selaginellae extract.
(2) purification: it is 1: 8 polyamide resin column that the extract that step (1) is obtained changes blade diameter length ratio over to, and the polyamide particle size range is 60～100 orders; Applied sample amount is a 55mg Herba Selaginellae extract on every 30mL polyamide.Be that 10% ethanol aqueous wash removes decontamination earlier with 12 times of column volume amount volumetric concentrations, the back is 70% ethanol water eluting with 8 times of column volume amount volumetric concentrations, eluent flow rate is 2mL/min, collect eluent, ethanol is reclaimed in distillation under 0.1Mpa, at vacuum 0.1Mpa, temperature be 45 ℃ of following vacuum dryings to constant weight, promptly get the Herba Selaginellae Flavonoid substances.
Adopt determined by ultraviolet spectrophotometry general flavone content and high effective liquid chromatography for measuring index composition amentoflavone content, general flavone content 66.65%, amentoflavone content 34.70%, the total flavones yield is greater than 82.56%.
Embodiment 3
The method of extracting purifying flavonoid substance from Herba Selaginellae is carried out according to the following steps:
(1) extract: with dry Herba Selaginellae pulverize, sieve sieve for No. 3 after, with 10 times of Herba Selaginellae weight, volumetric concentration is 70% ethanol water reflux, extract, 3 times, and extracting temperature is 80 ℃, and extraction time is each 2h, merge ethanol extract, after the filtered while hot, ethanol is reclaimed in distillation under 0.08Mpa, at vacuum 0.09Mpa, temperature be 40 ℃ of following vacuum dryings to constant weight, Herba Selaginellae extract.
(2) purification: it is 1: 6 polyamide resin column that the extract that step (1) is obtained changes blade diameter length ratio over to, and the polyamide particle size range is 60～100 orders; Applied sample amount is a 50mg Herba Selaginellae extract on every 30mL polyamide.Be that 50% ethanol aqueous wash removes decontamination earlier with 10 times of column volume amount volumetric concentrations, the back is 80% ethanol water eluting with 6 times of column volume amount volumetric concentrations, eluent flow rate is 1.0mL/min, collect eluent, ethanol is reclaimed in distillation under 0.08Mpa, at vacuum 0.09Mpa, temperature be 40 ℃ of following vacuum dryings to constant weight, promptly get the Herba Selaginellae Flavonoid substances.
Adopt determined by ultraviolet spectrophotometry general flavone content and high effective liquid chromatography for measuring index composition amentoflavone content, general flavone content 70.48%, amentoflavone content 34.88%, the total flavones yield is greater than 80.56%.
Embodiment 4
The method of extracting purifying flavonoid substance from Herba Selaginellae is carried out according to the following steps:
(1) extract: with dry Herba Selaginellae pulverize, sieve sieve for No. 3 after, with 11 times of Herba Selaginellae weight, volumetric concentration is 75% ethanol water reflux, extract, 3 times, and extracting temperature is 82 ℃, and extraction time is each 2.2h, merge ethanol extract, after the filtered while hot, ethanol is reclaimed in distillation under 0.06Mpa, at vacuum 0.09Mpa, temperature be 36 ℃ of following vacuum dryings to constant weight, Herba Selaginellae extract.
(2) purification: it is 1: 5 polyamide resin column that the extract that step (1) is obtained changes blade diameter length ratio over to, and the polyamide particle diameter is 600～100 orders; Applied sample amount is a 48mg Herba Selaginellae extract on every 30mL polyamide.Be that 20% ethanol aqueous wash removes decontamination earlier with 9 times of column volume amount volumetric concentrations, the back is 85% ethanol water eluting with 5 times of column volume amount volumetric concentrations, eluent flow rate is 1.5mL/min, collect eluent, ethanol is reclaimed in distillation under 0.06Mpa, at vacuum 0.08Mpa, temperature be 36 ℃ of following vacuum dryings to constant weight, promptly get the Herba Selaginellae Flavonoid substances.
Adopt determined by ultraviolet spectrophotometry general flavone content and high effective liquid chromatography for measuring index composition amentoflavone content, general flavone content 67.72%, amentoflavone content 33.67%, the total flavones yield is greater than 76.65%.
Claims (6)
1, a kind of method of from Herba Selaginellae, extracting purifying flavonoid substance, it is characterized in that: this method is carried out according to the following steps:
(1) extracts: after dry Herba Selaginellae is pulverized, sieves, with volumetric concentration is 60～80% ethanol water reflux, extract, 2～3 times, merge ethanol extract, after the filtered while hot, ethanol is reclaimed in distillation under 0.05～0.1Mpa, in vacuum is 0.05～0.1Mpa, and temperature is to be dried to constant weight under 35～45 ℃, gets Herba Selaginellae extract;
(2) purification: the extract that step (1) is obtained changes polyamide resin column over to, be that 10～60% ethanol aqueous wash removes decontamination earlier with volumetric concentration, the back is 70～90% ethanol water eluting with volumetric concentration, eluent flow rate is 0.5～2mL/min, collect eluent, ethanol is reclaimed in distillation under 0.05～0.1Mpa, is 0.05～0.1Mpa in vacuum, temperature is to be dried to constant weight under 35～45 ℃, promptly gets the Herba Selaginellae Flavonoid substances.
2, the method for from Herba Selaginellae, extracting purifying flavonoid substance according to claim 1, it is characterized in that: in step (1), the consumption of ethanol water is 8～12 times of Herba Selaginellae weight, and the reflux, extract, temperature is 75～85 ℃, and extraction time is each 1.5～2.5h.
3, the method for extracting purifying flavonoid substance from Herba Selaginellae according to claim 1 and 2, it is characterized in that: in step (2), the blade diameter length ratio of used polyamide resin column is 1: 4～8, and the polyamide particle diameter is 60～100 orders.
4, the method for extracting purifying flavonoid substance from Herba Selaginellae according to claim 3, it is characterized in that: in step (2), applied sample amount is 45～55mg Herba Selaginellae extract on every 30mL polyamide.
5, according to claim 1 or the 4 described methods of extracting purifying flavonoid substance from Herba Selaginellae, it is characterized in that: in step (2), the consumption of ethanol water is 8～12 times of column volume amounts during the eluting remove impurity.
6, the method for extracting purifying flavonoid substance from Herba Selaginellae according to claim 5, it is characterized in that: in step (2), the eluent consumption is 4～8 times of column volume amounts.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106692216A (en) * | 2016-11-15 | 2017-05-24 | 河南中医药大学 | Preparation method and application of selaginella tamariscina flavone and beta-cyclodextrin inclusion compound |
| CN107243016A (en) * | 2017-06-07 | 2017-10-13 | 中南大学湘雅医院 | Selaginella doederleinii extract and its application in terms of dull-witted disease drug is prepared |
| CN107382939A (en) * | 2017-07-31 | 2017-11-24 | 天津市泰通农业科技有限公司 | The method of flavone compound in supercritical carbon dioxide extracting selaginella doederleinii |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100451013C (en) * | 2004-04-21 | 2009-01-14 | 徐州技源天然保健品有限公司 | Producing technique for extracting extract products of amentoflavone |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106692216A (en) * | 2016-11-15 | 2017-05-24 | 河南中医药大学 | Preparation method and application of selaginella tamariscina flavone and beta-cyclodextrin inclusion compound |
| CN107243016A (en) * | 2017-06-07 | 2017-10-13 | 中南大学湘雅医院 | Selaginella doederleinii extract and its application in terms of dull-witted disease drug is prepared |
| CN107382939A (en) * | 2017-07-31 | 2017-11-24 | 天津市泰通农业科技有限公司 | The method of flavone compound in supercritical carbon dioxide extracting selaginella doederleinii |
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