CN107434816A - One kind extracts rutin method from Ilex Latifolia Thunb - Google Patents
One kind extracts rutin method from Ilex Latifolia Thunb Download PDFInfo
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- CN107434816A CN107434816A CN201610350584.4A CN201610350584A CN107434816A CN 107434816 A CN107434816 A CN 107434816A CN 201610350584 A CN201610350584 A CN 201610350584A CN 107434816 A CN107434816 A CN 107434816A
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- rutin
- ilex latifolia
- acetone
- latifolia thunb
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/06—Benzopyran radicals
- C07H17/065—Benzo[b]pyrans
- C07H17/07—Benzo[b]pyran-4-ones
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- Health & Medical Sciences (AREA)
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- Biotechnology (AREA)
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- Saccharide Compounds (AREA)
Abstract
The present invention relates to a kind of method that rutin is extracted from Ilex Latifolia Thunb, processing step is：By the Ilex Latifolia Thunb acetone after drying, crushing, continuous backflow is handled 2~4 hours in 50 DEG C~60 DEG C water-baths first, reclaims acetone, and sample dries, then using 70%~80% ethanol as Extraction medium, feed liquid w/v 1:20~30 carry out ultrasonic extractions, filtering, are recovered under reduced pressure ethanol, and mother liquor continues to be ultrasonically treated 1 hour, it is rear it is cold put crystallization, filter and obtain crude product rutin；Rutin crude product is handled about 0.5~1.0 hour with acetone continuous backflow again, recovery acetone, drying sample, then with w/v 1:100 add distilled water to dissolve by heating sample, filter while hot, cold to put crystallization, obtain rutin highly finished product.The present invention uses the technology of ultrasound assisted extraction, improves extraction efficiency and yield, and operating process is simple, and is sufficiently used the abundant Ilex latifolia resource in Southwestern China area, has opened up the frontier of Ilex Latifolia Thunb application, has solved the problems, such as rutin raw material anxiety.
Description
Technical field
The invention belongs to field of medicaments, is related to a kind of method of extraction and refined rutin from Ilex Latifolia Thunb.
Background technology
Rutin (Rutin), belongs to flavone compound, also known as rutin, citrin, rutin；It does not reduce capillary permeability and brittle effect only, it can also keep and recover the normal elasticity of capillary, available for preventing and treating hypertensive cerebral hemorrhage, diabetic retina bleeding and purpura haemorrhagica etc., it is also possible to make food antioxidant and pigment, moreover it is possible to the raw material as synthesis troxerutin.
At present, the method for producing rutin mainly has：1st, hot water extraction method, although this method technique is simple, equipment requirement is low, and product yield is relatively low, second-rate；2nd, the heavy method of alkali carries-acid, although product quality prepared by this method is slightly good, yield is relatively low；3rd, solvent extraction method, though this method yield is secure, product it is refined extremely difficult, product content is relatively low.As can be seen here, the above method cuts both ways.Find it is a kind of in high yield, the rutin of high-purity into production method, while Improving The Quality of Products reaches highest international standard DAB-10, take into account the utilization rate of raw material again, reduce production cost, it has also become the task of top priority of rutin production industry at present.
The content of the invention
The purpose of the present invention is that the defects of overcoming above-mentioned prior art, there is provided a kind of extraction time is short, and extraction efficiency is high, and purity is high, the low method that rutin is extracted from Ilex Latifolia Thunb of cost.
Technical scheme：
A kind of method that rutin is extracted from Ilex Latifolia Thunb, it is characterised in that its processing step is：By the Ilex Latifolia Thunb acetone after drying, crushing, continuous backflow is handled 2~4 hours in 50 DEG C~60 DEG C water-baths first, reclaims acetone, and sample dries, then using 70%~80% ethanol as Extraction medium, feed liquid w/v 1:20~30 carry out ultrasonic extractions, filtering, are recovered under reduced pressure ethanol, and mother liquor continues to be ultrasonically treated 1 hour, it is rear it is cold put crystallization, filter and obtain crude product rutin；
Above-mentioned drying refers at a temperature of 50 DEG C~70 DEG C dry Ilex Latifolia Thunb to constant weight；
Above-mentioned crushing refers to cross 50 mesh sieves after dried Ilex Latifolia Thunb is crushed；
The ultrasonic extraction of above-mentioned sample and the supersound process of mother liquor are handled using 80kHZ ultrasonic wave, and wherein the ultrasonic extraction of sample is 30 minutes every time three times；
The crude product rutin of above-mentioned gained is handled about 0.5~1.0 hour with acetone continuous backflow again, recovery acetone, drying sample, then with w/v 1:100 add distilled water to dissolve by heating sample, filter while hot, cold to put crystallization, obtain rutin highly finished product.
The present invention compares with the technology that rutin is obtained from other plants reported at present, mainly has the following advantages：
1）Using the technology of ultrasound assisted extraction, the production cycle greatly shortens, and by original several hours, or even longer time, shorten to 1.5h., and operating process is simple, and extraction efficiency improves.
2）In rutin subsidence stage, the effect of ultrasonic wave is also facilitated, so as to accelerate the speed of separating out of rutin, the production cycle is shortened, improves the yield of rutin.
3）The abundant Ilex latifolia resource in Southwestern China area is sufficiently used, has opened up the frontier of Ilex Latifolia Thunb application.
Embodiment
1) Ilex Latifolia Thunb be crushed into 50 mesh sieves in 50 DEG C~70 DEG C scope dryings to constant weight.
2) handled about 2~4 hours in 50 DEG C~60 DEG C water-bath continuous backflows with acetone, remove the oil-soluble impuritieses such as chlorophyll, reclaimed acetone, sample is dried.
3) using 70%~80% ethanol as Extraction medium, feed liquid w/v 1:Ilex Latifolia Thunb is carried out ultrasonic (80kHz) extraction three times by 20~30,30 minutes every time, filtering, merging filtrate, ethanol is recovered under reduced pressure.
4）Mother liquor continued ultrasound after 30 minutes, cold to put crystallization, and suction filtration obtains crude product rutin, dries.
5）Dry crude product rutin handles about 0.5~1.0h. with acetone continuous backflow again, removes the impurity such as the chlorophyll of attachment, reclaims acetone, drying sample.
6）With w/v 1:100 add distilled water to dissolve by heating sample, filter while hot, cold to put crystallization, obtain rutin essence
Product.
7）High performance liquid chromatography detection, rutin highly finished product purity>95%.
Claims (5)
1. a kind of method that rutin is extracted from Ilex Latifolia Thunb, is characterised by that its processing step is：By the Ilex latifolia tea-leaf acetone after drying, crushing, continuous backflow is handled 2~4 hours in 50~60 DEG C of water-baths first, reclaims acetone, sample is dried, then using 70~80% ethanol as Extraction medium, feed liquid w/v 1:20~30 carry out ultrasonic extractions, filtering, are recovered under reduced pressure ethanol, and mother liquor continues to be ultrasonically treated 1 hour, it is rear it is cold put crystallization, filter and obtain crude product rutin.The rutin crude product of gained is handled about 0.5~1.0 hour with acetone continuous backflow again, recovery acetone, drying sample, then with w/v 1:100 add distilled water to dissolve by heating sample, filter while hot, cold to put crystallization, obtain rutin highly finished product.
2. according to the method that rutin is extracted from Ilex Latifolia Thunb described in claim 1, it is characterized in that：Above-mentioned drying refers at a temperature of 50 DEG C~70 DEG C dry Ilex Latifolia Thunb to constant weight.
3. according to the method that rutin is extracted from Ilex Latifolia Thunb described in claim 1, it is characterized in that：Above-mentioned crushing refers to cross 50 mesh sieves after dried Ilex Latifolia Thunb is crushed.
4. according to the method that rutin is extracted from Ilex Latifolia Thunb described in claim 1, it is characterized in that：The ultrasonic extraction of above-mentioned sample and the supersound process of mother liquor are handled using 80kHZ ultrasonic wave, and wherein the ultrasonic extraction of sample is 30 minutes every time three times.
5. according to the method that rutin is extracted from Ilex Latifolia Thunb described in claim 1, it is characterized in that：The crude product rutin of above-mentioned gained is handled about 0.5~1.0 hour with acetone continuous backflow again, recovery acetone, drying sample, then with w/v 1:100 add distilled water to dissolve by heating sample, filter while hot, cold to put crystallization, obtain rutin highly finished product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610350584.4A CN107434816A (en) | 2016-05-25 | 2016-05-25 | One kind extracts rutin method from Ilex Latifolia Thunb |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610350584.4A CN107434816A (en) | 2016-05-25 | 2016-05-25 | One kind extracts rutin method from Ilex Latifolia Thunb |
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| CN107434816A true CN107434816A (en) | 2017-12-05 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610350584.4A Pending CN107434816A (en) | 2016-05-25 | 2016-05-25 | One kind extracts rutin method from Ilex Latifolia Thunb |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108659072A (en) * | 2018-04-23 | 2018-10-16 | 东北林业大学 | A kind of rutin-alcohol solvent compound crystal and preparation method thereof |
| CN109111493A (en) * | 2018-10-12 | 2019-01-01 | 河南精康制药有限公司 | A kind of feed purification method being used to prepare Troxerutin for Injection |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1410423A (en) * | 2001-09-28 | 2003-04-16 | 张杰克 | Technical method of extracting rutin |
| CN101818184A (en) * | 2010-05-04 | 2010-09-01 | 河南青纯生物科技有限公司 | Method for extracting rutin from sophora japonica |
-
2016
- 2016-05-25 CN CN201610350584.4A patent/CN107434816A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1410423A (en) * | 2001-09-28 | 2003-04-16 | 张杰克 | Technical method of extracting rutin |
| CN101818184A (en) * | 2010-05-04 | 2010-09-01 | 河南青纯生物科技有限公司 | Method for extracting rutin from sophora japonica |
Non-Patent Citations (2)
| Title |
|---|
| LI LI, ET AL.,: "Chemical constituents from Ligustrum robustum Bl.", 《BIOCHEMICAL SYSTEMATICS AND ECOLOGY》 * |
| 潘慧娟等，: "苦丁茶中黄酮类化合物的提取、鉴定和含量分析.", 《杭州医学高等专科学校学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108659072A (en) * | 2018-04-23 | 2018-10-16 | 东北林业大学 | A kind of rutin-alcohol solvent compound crystal and preparation method thereof |
| CN109111493A (en) * | 2018-10-12 | 2019-01-01 | 河南精康制药有限公司 | A kind of feed purification method being used to prepare Troxerutin for Injection |
| CN109111493B (en) * | 2018-10-12 | 2021-08-10 | 河南精康制药有限公司 | Raw material refining method for preparing troxerutin for injection |
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Application publication date: 20171205 |
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