CN103450299A - Method for simultaneously preparing esculoside and esculetin - Google Patents
Method for simultaneously preparing esculoside and esculetin Download PDFInfo
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- CN103450299A CN103450299A CN 201310425575 CN201310425575A CN103450299A CN 103450299 A CN103450299 A CN 103450299A CN 201310425575 CN201310425575 CN 201310425575 CN 201310425575 A CN201310425575 A CN 201310425575A CN 103450299 A CN103450299 A CN 103450299A
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- ethyl acetate
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- cichorigenin
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Abstract
The invention relates to a method for simultaneously preparing esculoside and esculetin, and in particular relates to a continuous countercurrent ultrasonic extraction method. The method comprises the following steps: adding ethanol liquor to ash bark crude powder; after carrying out continuous countercurrent ultrasonic extraction, carrying out solid-liquid separation to obtain leach liquor; carrying out solid-liquid separation to obtain supernate; concentrating under reduced pressure; adding distilled water to dissolve; firstly, extracting for 2 times by chloroform; extracting the water layer extracted by chloroform through ethyl acetate for times; combining the ethyl acetate extracting liquor; drying by anhydrous sodium sulfate; recovering the solvent under reduced pressure till dryness; adding methanol to separate out yellow acicular crystals; repeatedly crystallizing for many times by a recrystallization solvent to obtain the esculetin; partially concentrating water extracted by ethyl acetate to separate out yellowish crystals; repeatedly crystallizing for many times by the recrystallization solvent to obtain the esculoside. The method provided by the invention has the advantages of simplicity in process, short extraction time, high extraction rate and reasonable utilization of raw materials, and is environment-friendly and easy for industrial production.
Description
technical field:
The present invention relates to a kind of method that simultaneously prepares Vitamin C2 and Cichorigenin, relate in particular to a kind of method of utilizing the continuous countercurrent supersound extraction.
background technology:
Dry bark or trunk bark that the bark of ash is five kind of plant such as Oleaceae plants Chinese ash, it is China's conventional Chinese medicine simply, the successive dynasties book on Chinese herbal medicine is all on the books, containing Vitamin C2, Cichorigenin, fraxin, Fraxetin and resin, tannin and a small amount of starch etc., its cold nature, bitter, the function heat-clearing and damp-drying drug, be apt to control diarrhea due to damp-heat and dysentery, damp and hot rheumatism also had to the effect of clearing away damp-heat, suitable numbness pain relieving, modern study proves, the bark of ash has relieving inflammation and relaxing pain and reduces the effect of hematuria acid, is used for the treatment of gout excellent.Wherein Vitamin C2 and Cichorigenin have stronger oxidation-resistance.Find in recent years the great attention that the efficient natural antioxidant has been subject to people from herbal medicine, there is vast potential for future development.
Less about the research report of Vitamin C2 in the bark of ash and Cichorigenin at present, by the exploration to extracting method, for the industrialization of extracting Vitamin C2 and Cichorigenin from the bark of ash lays the foundation, meet the need of market.
summary of the invention:
The objective of the invention is fully to develop the value of the bark of ash, a kind of method of simultaneously extracting Vitamin C2 and Cichorigenin be provided, the method has advantages of that technique is simple, extraction efficiency is high, power consumption less, extraction time is short, is easy to realize suitability for industrialized production.
The present invention includes following steps:
A. get the bark of ash and pulverize, cross 100 mesh sieves;
B. add 95% ethanol of 5 ~ 10 times of bark of ash grain weight amounts in bark of ash powder, under 60 ~ 80 ℃, under 50 ~ 70KHz, solid-liquid separation after continuous countercurrent supersound extraction 2 ~ 3h, obtain supernatant liquor;
C. by the above-mentioned supernatant liquor concentrating under reduced pressure obtained, add distilled water to dissolve, first use chloroform extraction 2 times, the water layer that chloroform extraction is crossed is extracted with ethyl acetate 2 ~ 4 times, combined ethyl acetate extraction liquid, anhydrous sodium sulfate drying, decompression and solvent recovery is to dry, add methyl alcohol and separate out yellow needle-like crystal, 60 ~ 90% methanol aqueous solution periodic crystallisation 2 times, obtain Cichorigenin;
D. the stripped water section of ethyl acetate is concentrated, separate out micro-yellow crystals, the methanol aqueous solution periodic crystallisation with 60 ~ 90% 2 times, obtain Vitamin C2.
The present invention selects continuous countercurrent supersound extraction Vitamin C2 and Cichorigenin, uses minimum solvent to obtain maximum solubleness, has improved extraction effect, significantly reduced solvent load, reduced energy consumption, can realize continuous operation, be easy to realize suitability for industrialized production simultaneously.In addition, at present less to the extraction research of Vitamin C2 and Cichorigenin, the present invention has utilized raw material fully, has obtained two kinds of products of Vitamin C2 and Cichorigenin simultaneously, for the development and utilization of the bark of ash opens up a new way.
Further illustrate the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
embodiment:
Embodiment 1:
Get 100g through pulverizing, cross the bark of ash powder of 100 mesh sieves, 95% ethanol that adds 5 times of bark of ash grain weight amounts, solid-liquid separation after continuous countercurrent supersound extraction 2h under 70 ℃, under 60KHz, obtain supernatant liquor, concentrating under reduced pressure, add distilled water to dissolve, first use chloroform extraction 2 times, the water layer that chloroform extraction is crossed is extracted with ethyl acetate 4 times, the combined ethyl acetate extraction liquid, anhydrous sodium sulfate drying, decompression and solvent recovery, to dry, adds methyl alcohol and separates out yellow needle-like crystal, 60% methanol aqueous solution periodic crystallisation 2 times, obtain Cichorigenin, productive rate is 3.58%; The stripped water section of ethyl acetate is concentrated, separate out micro-yellow crystals, the methanol aqueous solution periodic crystallisation with 60% 2 times, obtain Vitamin C2, and productive rate is 2.01%.
Embodiment 2:
Get 100g through pulverizing, cross the bark of ash powder of 100 mesh sieves, 95% ethanol that adds 10 times of bark of ash grain weight amounts, solid-liquid separation after continuous countercurrent supersound extraction 3h under 80 ℃, under 50KHz, obtain supernatant liquor, concentrating under reduced pressure, add distilled water to dissolve, first use chloroform extraction 2 times, the water layer that chloroform extraction is crossed is extracted with ethyl acetate 3 times, the combined ethyl acetate extraction liquid, anhydrous sodium sulfate drying, decompression and solvent recovery, to dry, adds methyl alcohol and separates out yellow needle-like crystal, 80% methanol aqueous solution periodic crystallisation 2 times, obtain Cichorigenin, productive rate is 4.01%; The stripped water section of ethyl acetate is concentrated, separate out micro-yellow crystals, the methanol aqueous solution periodic crystallisation with 80% 2 times, obtain Vitamin C2, and productive rate is 2.24%.
Embodiment 3:
Get 100g through pulverizing, cross the bark of ash powder of 100 mesh sieves, 95% ethanol that adds 8 times of bark of ash grain weight amounts, solid-liquid separation after continuous countercurrent supersound extraction 2.5h under 60 ℃, under 70KHz, obtain supernatant liquor, concentrating under reduced pressure, add distilled water to dissolve, first use chloroform extraction 2 times, the water layer that chloroform extraction is crossed is extracted with ethyl acetate 2 times, the combined ethyl acetate extraction liquid, anhydrous sodium sulfate drying, decompression and solvent recovery, to dry, adds methyl alcohol and separates out yellow needle-like crystal, 90% methanol aqueous solution periodic crystallisation 2 times, obtain Cichorigenin, productive rate is 3.79%; The stripped water section of ethyl acetate is concentrated, separate out micro-yellow crystals, the methanol aqueous solution periodic crystallisation with 90% 2 times, obtain Vitamin C2, and productive rate is 2.15%.
Claims (3)
1. a method that simultaneously prepares Vitamin C2 and Cichorigenin, is characterized in that, comprises the following steps:
A. get the bark of ash and pulverize, cross 100 mesh sieves;
B. add 95% ethanol of 5 ~ 10 times of bark of ash grain weight amounts in bark of ash powder, under 60 ~ 80 ℃, under 50 ~ 70KHz, solid-liquid separation after continuous countercurrent supersound extraction 2 ~ 3h, obtain supernatant liquor;
C. by the above-mentioned supernatant liquor concentrating under reduced pressure obtained, add distilled water to dissolve, first use chloroform extraction 2 times, the water layer that chloroform extraction is crossed is extracted with ethyl acetate for several times, combined ethyl acetate extraction liquid, anhydrous sodium sulfate drying, decompression and solvent recovery is to dry, add methyl alcohol and separate out yellow needle-like crystal, recrystallization solvent periodic crystallisation 2 times, obtain Cichorigenin;
D. the stripped water section of ethyl acetate is concentrated, separate out micro-yellow crystals, with recrystallization solvent periodic crystallisation 2 times, obtain Vitamin C2.
2. a kind of method that simultaneously prepares Vitamin C2 and Cichorigenin according to claim 1 is characterized in that: the number of times of the ethyl acetate extraction described in step c is 2 ~ 4 times.
3. a kind of method that simultaneously prepares Vitamin C2 and Cichorigenin according to claim 1, is characterized in that: the methanol aqueous solution that the recrystallization solvent described in step c and steps d is 60 ~ 90%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201310425575 CN103450299A (en) | 2013-09-18 | 2013-09-18 | Method for simultaneously preparing esculoside and esculetin |
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| CN 201310425575 CN103450299A (en) | 2013-09-18 | 2013-09-18 | Method for simultaneously preparing esculoside and esculetin |
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| CN103450299A true CN103450299A (en) | 2013-12-18 |
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| CN 201310425575 Pending CN103450299A (en) | 2013-09-18 | 2013-09-18 | Method for simultaneously preparing esculoside and esculetin |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106905279A (en) * | 2017-01-19 | 2017-06-30 | 中国农业大学 | A kind of extracting method of Chinese herbaceous peony antioxidation composition |
| CN107501220A (en) * | 2017-08-23 | 2017-12-22 | 佛山市三水区嘉华化学研究院（普通合伙） | A kind of aesculetin and preparation method and application with antioxidant and anti-aging activity |
| CN109134562A (en) * | 2018-10-26 | 2019-01-04 | 宁县恒瑞康生物科技有限公司 | A kind of aesculin purification process |
-
2013
- 2013-09-18 CN CN 201310425575 patent/CN103450299A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106905279A (en) * | 2017-01-19 | 2017-06-30 | 中国农业大学 | A kind of extracting method of Chinese herbaceous peony antioxidation composition |
| CN106905279B (en) * | 2017-01-19 | 2019-03-22 | 中国农业大学 | A kind of extracting method of Chinese herbaceous peony antioxidation ingredient |
| CN107501220A (en) * | 2017-08-23 | 2017-12-22 | 佛山市三水区嘉华化学研究院（普通合伙） | A kind of aesculetin and preparation method and application with antioxidant and anti-aging activity |
| CN109134562A (en) * | 2018-10-26 | 2019-01-04 | 宁县恒瑞康生物科技有限公司 | A kind of aesculin purification process |
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Application publication date: 20131218 |
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| WD01 | Invention patent application deemed withdrawn after publication |