CN102659736A - Preparation method of sudachitin - Google Patents
Preparation method of sudachitin Download PDFInfo
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- CN102659736A CN102659736A CN2012101159073A CN201210115907A CN102659736A CN 102659736 A CN102659736 A CN 102659736A CN 2012101159073 A CN2012101159073 A CN 2012101159073A CN 201210115907 A CN201210115907 A CN 201210115907A CN 102659736 A CN102659736 A CN 102659736A
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- soda
- booth
- extract
- sudachitin
- preparation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Medicines Containing Plant Substances (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention relates to a preparation method of sudachitin, which is simple to operate and has less pollution. The preparation method comprises the following process steps: (1) taking citrus sudachi, crushing, adding a proper amount of distilled water and biological enzymes for natural enzymolysis, adding an obtained enzymolysis raw material into a supercritical CO2 extractor and taking methanol as an entrainer for extraction to obtain an extract; (2) adding ethyl acetate into the extract to agitate and dissolve, filtering, and concentrating and drying a filtrate to obtain a crude extract; (3) separating and purifying sudachitin in the crude extract, wherein a two-phase solvent system of the sudachitin is petroleum ether-ethyl acetate-methanol-water, takes an upper phase as a fixed phase and a lower phase as a mobile phase and is used for collecting sudachitin components; and (4) carrying out vacuum concentration on the sudachitin components, separating out for crystallization, filtering out for crystallization and adding ethyl acetate-methanol for recrystallization. The sudachitin prepared by the invention has high product purity and the industrialization amplification is easy to realize.
Description
Technical field
The invention belongs to the traditional Chinese medicine extraction separation technology field, relate to a kind of method for preparing its booth of soda of from its citrus of soda, separating.
Background technology
The yellow needle of its booth of soda (Sudachitin) (ETHYLE ACETATE: methyl alcohol, 1:1), mp.239.5～240.5 ℃.Flavonoid substances mainly is present in composite family (Compositae), ancient heap chrysanthemum
Gutierrezia sarothraeOver-ground part, strumae Sunflower Receptacle
Helianthus strumosusHer watt chrysanthemum of over-ground part, needle-like
Iva acerosa(Nutt.) Jackson, the membranous chrysanthemum of husky living line leaf
Tetraneuris linearifolia var.arenicolaOver-ground part; Cyperaceae (Cyperaceae),
Trichophorum cespitosum(L.) Hartman subsp. stem; Labiatae (Labiatae), majoram
Majorana hortensisLeaf; . Rutaceae (Rutaceae), its citrus of soda
Citrus sudachiHort.ex Shirai fruit, its citrus of soda
Citrus sudachiHort.ex Shirai pericarp.Molecular formula: C
18H
16O
8, molecular weight: 360.32.When its booth of soda was 10 μ M in concentration, inhibited to the lens aldose reductase of rat, ox, inhibiting rate was respectively 66% and 56%; When concentration was 1 μ M, its inhibiting rate to both was all 19%.
At present, the sale of its booth reference substance of rare soda and related prods thereof on the market, scarcity of resources and cost are higher.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of its booth of soda.
The objective of the invention is to realize through following technical scheme:
(1) gets its citrus of soda,, add an amount of zero(ppm) water and enzyme natural enzymolysis, get the enzymolysis raw material and be added to supercritical CO through pulverization process
2In the extractor, as entrainment agent, extract, obtain extract with methyl alcohol;
(2) extract adding ETHYLE ACETATE stirs and makes dissolving, filters, and the filtrating concentrate drying gets crude extract;
(3) its booth of soda in the above-mentioned crude extract of employing high-speed countercurrent chromatography separation and purification; Its two-phase solvent system is petroleum ether-ethyl acetate-methanol-water, on to fill with the high speed adverse current chromatogram post mutually be stationary phase, rotate main frame; Pump into down and do moving phase mutually; Moving phase dissolving crude extract is by the sampling valve sample introduction, and the UV-detector on-line monitoring is collected its booth component of soda;
(4) its booth component of soda is carried out vacuum concentration, separate out crystallization, leach crystallization, add ETHYLE ACETATE-methyl alcohol (1:1) recrystallization, filtration, washing are drying to obtain its booth of soda.
The consumption of the enzyme in the said step (1) is 0.5-0.8%.
Supercritical CO in the said step (1)
2Extraction parameter condition is that extraction temperature is 30-45 ℃, and extracting pressure is 28-35MPa, and the extraction time is 1.5-3.5h, and separating still I temperature is 25-35 ℃, and pressure is 8-10MPa, and separating still II temperature is 20-28 ℃, and pressure is 5-8MPa, CO
2Flow is 2-4ml/g crude drug/min.
The volume ratio of said step (3) PetroChina Company Limited. ether-ETHYLE ACETATE-methanol-water solvent systems is 3-5:5-8:4-6:2-5.
Present method positively effect is:
(1) present method adopts supercritical CO
2Extraction, energy consumption is low, extraction agent CO
2Cleanliness without any pollution;
(2) present method adopts high-speed countercurrent chromatography, and yield is high, preparation amount is big, preparation cycle is short, has solved the low and with serious pollution technological deficiency of column chromatography efficient;
(3) operation of present method process step is simpler, easy to operate, and products obtained therefrom purity is high.
To combine embodiment to further specify the present invention below, but the scope that the present invention requires to protect is not limited to following embodiment.
Embodiment
Embodiment 1:
Get its citrus of 1kg soda,, add 5g enzyme and an amount of zero(ppm) water natural enzymolysis, get the enzymolysis raw material and be added to supercritical CO through pulverization process
2In the extractor, setting extraction temperature is 45 ℃, and extracting pressure is 28MPa, and separating still I temperature is 25 ℃, and pressure is 10MPa, and separating still II temperature is 20 ℃, and pressure is 5MPa, CO
2Feeding flow is 4ml/g crude drug/min, and feeding methyl alcohol extracts 3.5h as entrainment agent, in separating still, obtains extract, adds the ETHYLE ACETATE stirring and makes dissolving, filters, and the filtrating concentrate drying gets crude extract; Adopt its booth of soda in the high-speed countercurrent chromatography separation and purification crude extract, measure petroleum ether-ethyl acetate-methanol-water by the 3:8:6:2 volume ratio, mixing leaves standstill; Getting and filling with the high speed adverse current chromatogram post mutually is stationary phase, rotates main frame, pumps into down and does moving phase mutually; Moving phase dissolving crude extract is by the sampling valve sample introduction, and the UV-detector on-line monitoring is collected its booth component of soda; Vacuum concentration is separated out crystallization, leaches crystallization; Add ETHYLE ACETATE-methyl alcohol (1:1) recrystallization, filtration, washing are drying to obtain its booth of soda, content 96.5%.
Embodiment 2:
Get its citrus of 1kg soda,, add 8g enzyme and an amount of zero(ppm) water natural enzymolysis, get the enzymolysis raw material and be added to supercritical CO through pulverization process
2In the extractor, setting extraction temperature is 30 ℃, and extracting pressure is 35MPa, and separating still I temperature is 25 ℃, and pressure is 8MPa, and separating still II temperature is 20 ℃, and pressure is 5MPa, CO
2Feeding flow is 2ml/g crude drug/min, and feeding methyl alcohol extracts 1.5h as entrainment agent, in separating still, obtains extract, adds the ETHYLE ACETATE stirring and makes dissolving, filters, and the filtrating concentrate drying gets crude extract; Adopt its booth of soda in the high-speed countercurrent chromatography separation and purification crude extract, measure petroleum ether-ethyl acetate-methanol-water by the 5:5:4:5 volume ratio, mixing leaves standstill; Getting and filling with the high speed adverse current chromatogram post mutually is stationary phase, rotates main frame, pumps into down and does moving phase mutually; Moving phase dissolving crude extract is by the sampling valve sample introduction, and the UV-detector on-line monitoring is collected its booth component of soda; Vacuum concentration is separated out crystallization, leaches crystallization; Add ETHYLE ACETATE-methyl alcohol (1:1) recrystallization, filtration, washing are drying to obtain its booth of soda, content 97.8%.
Embodiment 3:
Get its citrus of 10kg soda,, add 60g enzyme and an amount of zero(ppm) water natural enzymolysis, get the enzymolysis raw material and be added to supercritical CO through pulverization process
2In the extractor, setting extraction temperature is 35 ℃, and extracting pressure is 35MPa, and separating still I temperature is 35 ℃, and pressure is 10MPa, and separating still II temperature is 28 ℃, and pressure is 7MPa, CO
2Feeding flow is 3ml/g crude drug/min, and feeding methyl alcohol extracts 3h as entrainment agent, in separating still, obtains extract, adds the ETHYLE ACETATE stirring and makes dissolving, filters, and the filtrating concentrate drying gets crude extract; Adopt its booth of soda in the high-speed countercurrent chromatography separation and purification crude extract, measure petroleum ether-ethyl acetate-methanol-water by the 4:7:5:3 volume ratio, mixing leaves standstill; Getting and filling with the high speed adverse current chromatogram post mutually is stationary phase, rotates main frame, pumps into down and does moving phase mutually; Moving phase dissolving crude extract is by the sampling valve sample introduction, and the UV-detector on-line monitoring is collected its booth component of soda; Vacuum concentration is separated out crystallization, leaches crystallization; Add ETHYLE ACETATE-methyl alcohol (1:1) recrystallization, filtration, washing are drying to obtain its booth of soda, content 97.3%.
Embodiment 4:
Get its citrus of 10kg soda,, add 70g enzyme and an amount of zero(ppm) water natural enzymolysis, get the enzymolysis raw material and be added to supercritical CO through pulverization process
2In the extractor, setting extraction temperature is 38 ℃, and extracting pressure is 30MPa, and separating still I temperature is 28 ℃, and pressure is 10MPa, and separating still II temperature is 25 ℃, and pressure is 7MPa, CO
2Feeding flow is 4ml/g crude drug/min, and feeding methyl alcohol extracts 2h as entrainment agent, in separating still, obtains extract, adds the ETHYLE ACETATE stirring and makes dissolving, filters, and the filtrating concentrate drying gets crude extract; Adopt its booth of soda in the high-speed countercurrent chromatography separation and purification crude extract, measure petroleum ether-ethyl acetate-methanol-water by the 4:7:5:3 volume ratio, mixing leaves standstill; Getting and filling with the high speed adverse current chromatogram post mutually is stationary phase, rotates main frame, pumps into down and does moving phase mutually; Moving phase dissolving crude extract is by the sampling valve sample introduction, and the UV-detector on-line monitoring is collected its booth component of soda; Vacuum concentration is separated out crystallization, leaches crystallization; Add ETHYLE ACETATE-methyl alcohol (1:1) recrystallization, filtration, washing are drying to obtain its booth of soda, content 98.1%.
Claims (4)
1. the preparation method of its booth of soda is characterized in that may further comprise the steps:
(1) gets its citrus of soda,, add an amount of zero(ppm) water and enzyme natural enzymolysis, get the enzymolysis raw material and be added to supercritical CO through pulverization process
2In the extractor, as entrainment agent, extract, obtain extract with methyl alcohol;
(2) extract adding ETHYLE ACETATE stirs and makes dissolving, filters, and the filtrating concentrate drying gets crude extract;
(3) above-mentioned crude extract adopts the high-speed countercurrent chromatography separation and purification; Its two-phase solvent system is petroleum ether-ethyl acetate-methanol-water, on to fill with the high speed adverse current chromatogram post mutually be stationary phase, rotate main frame; Pump into down and do moving phase mutually; Moving phase dissolving crude extract is by the sampling valve sample introduction, and the UV-detector on-line monitoring is collected its booth component of soda;
(4) its booth component of soda is carried out vacuum concentration, separate out crystallization, leach crystallization, add ETHYLE ACETATE-methyl alcohol (1:1) recrystallization, filtration, washing are drying to obtain its booth of soda.
2. the preparation method of a kind of its booth of soda according to claim 1 is characterized in that: the consumption of the enzyme in the said step (1) is 0.5-0.8%.
3. the preparation method of a kind of its booth of soda according to claim 1 is characterized in that: the supercritical CO in the said step (1)
2Extraction parameter condition is that extraction temperature is 30-45 ℃, and extracting pressure is 28-35MPa, and the extraction time is 1.5-3.5h, and separating still I temperature is 25-35 ℃, and pressure is 8-10MPa, and separating still II temperature is 20-28 ℃, and pressure is 5-8MPa, CO
2Flow is 2-4ml/g crude drug/min.
4. the preparation method of a kind of its booth of soda according to claim 1 is characterized in that: the volume ratio of said step (3) PetroChina Company Limited. ether-ETHYLE ACETATE-methanol-water solvent systems is 3-5:5-8:4-6:2-5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101159073A CN102659736A (en) | 2012-04-19 | 2012-04-19 | Preparation method of sudachitin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101159073A CN102659736A (en) | 2012-04-19 | 2012-04-19 | Preparation method of sudachitin |
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| CN102659736A true CN102659736A (en) | 2012-09-12 |
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| CN2012101159073A Pending CN102659736A (en) | 2012-04-19 | 2012-04-19 | Preparation method of sudachitin |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102827240A (en) * | 2012-09-20 | 2012-12-19 | 南京泽朗农业发展有限公司 | Method for extracting and separating thorn leaf pink glycosides A |
| WO2020090813A1 (en) * | 2018-10-30 | 2020-05-07 | 日立化成株式会社 | Method for producing flavonoid |
-
2012
- 2012-04-19 CN CN2012101159073A patent/CN102659736A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102827240A (en) * | 2012-09-20 | 2012-12-19 | 南京泽朗农业发展有限公司 | Method for extracting and separating thorn leaf pink glycosides A |
| WO2020090813A1 (en) * | 2018-10-30 | 2020-05-07 | 日立化成株式会社 | Method for producing flavonoid |
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Application publication date: 20120912 |