CN102010402A - Method for preparing aloesin - Google Patents
Method for preparing aloesin Download PDFInfo
- Publication number
- CN102010402A CN102010402A CN2010105353853A CN201010535385A CN102010402A CN 102010402 A CN102010402 A CN 102010402A CN 2010105353853 A CN2010105353853 A CN 2010105353853A CN 201010535385 A CN201010535385 A CN 201010535385A CN 102010402 A CN102010402 A CN 102010402A
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- CN
- China
- Prior art keywords
- amomicin
- preparation
- ultra
- polyamide
- aloesin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 0 CCC(C(*)C(C1O)N)OC1c(c(C)cc(C)c12)c1OC(CC(C)=C)=CC2=O Chemical compound CCC(C(*)C(C1O)N)OC1c(c(C)cc(C)c12)c1OC(CC(C)=C)=CC2=O 0.000 description 1
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- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention relates to a method for preparing aloesin, which is simple and convenient to operate and has low pollution and low energy consumption. The method comprises the following steps of: taking fresh aloe leaves, adding water, performing homogenization treatment, performing centrifugal separation on the homogenate, taking the supernate, performing ultra-filtration through an ultra-filtration membrane, collecting the filtrate, adding the filtrate onto a polyamide chromatographic column, diluting the chromatographic column by using methanol as eluant, performing mating detection by using polyamide films of the same category and the eluant, collecting fractions of Rf=4-4.5 corresponding to the polyamide films, reclaiming the solvent, adding absolute ethanol for crystallization, separating the crystal, and washing and drying the crystal. The method for preparing the aloesin has high product quality, and is easy to realize industrialized amplification.
Description
Technical field
The present invention relates to a kind of preparation method of Amomicin, especially a kind of preparation method who from plant, extracts Amomicin.
Background technology
Amomicin (Aloesin), molecular formula: C
19H
22O
9, molecular weight: 394.377, CAS accession number: 30861-27-9.Be present in the Liliaceae Aloe various plants, wherein content is higher in liliaceous plant aloe Aloe vera L. var.chinensis (Haw.) the Berger leaf, and its source is abundant.Its molecular formula is as follows:
Modern study shows that Amomicin has various active such as anti-pigmentation, irritation cell growth, and it is also as the raw material that synthesizes other reactive derivative simultaneously.
In the prior art, still be not applicable to preparation technology's report of high purity Amomicin industrialized production.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method who is beneficial to big production operation, Amomicin that product purity is high.
For solving the problems of the technologies described above, the present invention adopts following technical proposal:
Get Fresh leaf of aloe, add its quality 1-3 and doubly measure the water of volume, carry out homogenized, homogenate is through centrifugation, get supernatant liquor, by the molecular weight cutoff value is that the daltonian ultra-filtration membrane of 1000-3000 carries out ultrafiltration, collect filtrate, be added on the polymeric amide chromatography post, with methyl alcohol as the eluent wash-out, launch as supporting detection with stating eluent more than the class polyamide layer of the same race simultaneously, collection is reclaimed solvent corresponding to the stream part of Rf=4-4.5 on the polyamine film, adds the dehydrated alcohol crystallization, fractional crystallization washs, is drying to obtain.
The amount that adds entry is preferably 2 times of amount volumes of raw materials quality.
The molecular weight cutoff value of ultra-filtration membrane is preferably 2000 dalton.
Polymeric amide is selected from a kind of in polyamide fibre 66, the polyamide fibre 6.
Preparation gained Amomicin can adopt following method to detect:
Test routine 1HPLC method and measure Amomicin purity
Chromatographic condition
Chromatographic column: octadecylsilane bonding glue silica gel is weighting agent; Moving phase: acetonitrile-0.2% glacial acetic acid aqueous solution (20: 80); Flow velocity: 1.0mL/min; Detect wavelength: 295nm; Column temperature: 30 ℃.
Measuring method
Precision takes by weighing Amomicin 2mg, places the 50mL measuring bottle, adds people's methyl alcohol 20mL, and sonic oscillation makes dissolving, and methanol constant volume is drawn 10 μ L to scale, injects high performance liquid chromatograph, adopts normalization method working sample purity.
Adopt the present invention to prepare Amomicin, be beneficial to big production operation, energy consumption is little, pollutes little.
The present invention is further elaborated below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment
Embodiment 1
Get Fresh leaf of aloe 10Kg, add 10L water, carry out homogenized, homogenate is got supernatant liquor through centrifugation, is that 1000 daltonian ultra-filtration membranes carry out ultrafiltration by the molecular weight cutoff value, collect filtrate, be added on polyamide fibre 66 (polyhexamethylene adipamide) the polymeric amide chromatography post, as the eluent wash-out, launch as supporting detection with stating eluent more than the class polyamide layer of the same race simultaneously with methyl alcohol, collection is corresponding to the stream part of Rf=4-4.5 on the polyamine film, reclaim solvent, add the dehydrated alcohol crystallization, fractional crystallization, washing, be drying to obtain white needle-Amomicin 6.5g, detect through HPLC, purity is 96.2%, UV, IR, MS;
2HNMR,
13The data of its physical behavior of sign such as CNMR are consistent with prior art.
Embodiment 2
Get Fresh leaf of aloe 10Kg, add 30L water, carry out homogenized, homogenate is got supernatant liquor through centrifugation, is that 3000 daltonian ultra-filtration membranes carry out ultrafiltration by the molecular weight cutoff value, collect filtrate, be added on polyamide fibre 66 (polyhexamethylene adipamide) the polymeric amide chromatography post, as the eluent wash-out, launch as supporting detection with stating eluent more than the class polyamide layer of the same race simultaneously with methyl alcohol, collection is corresponding to the stream part of Rf=4-4.5 on the polyamine film, reclaim solvent, add the dehydrated alcohol crystallization, fractional crystallization, washing, be drying to obtain white needle-Amomicin 7.3g, detect through HPLC, purity is 95.0%, UV, IR, MS;
2HNMR,
13The data of its physical behavior of sign such as CNMR are consistent with prior art.
Embodiment 3
Get Fresh leaf of aloe 10Kg, add 20L water, carry out homogenized, homogenate is got supernatant liquor through centrifugation, is that 2000 daltonian ultra-filtration membranes carry out ultrafiltration by the molecular weight cutoff value, collect filtrate, be added on the polyamide fibre 6 polymeric amide chromatography posts, as the eluent wash-out, launch as supporting detection with stating eluent more than the class polyamide layer of the same race simultaneously with methyl alcohol, collection is corresponding to the stream part of Rf=4-4.5 on the polyamine film, reclaim solvent, add the dehydrated alcohol crystallization, fractional crystallization, washing, be drying to obtain white needle-Amomicin 7.8g, detect through HPLC, purity is 97.7%, UV, IR, MS;
2HNMR,
13The data of its physical behavior of sign such as CNMR are consistent with prior art.
Claims (4)
1. the preparation method of an Amomicin, it is characterized in that described method is made up of the following step: get Fresh leaf of aloe, add its quality 1-3 and doubly measure the water of volume, carry out homogenized, homogenate is through centrifugation, getting supernatant liquor, is that the daltonian ultra-filtration membrane of 1000-3000 carries out ultrafiltration by the molecular weight cutoff value, collects filtrate, be added on the polymeric amide chromatography post,, launch as supporting detection with stating eluent more than the class polyamide layer of the same race simultaneously as the eluent wash-out with methyl alcohol, collect stream part corresponding to Rf=4-4.5 on the polyamine film, reclaim solvent, add the dehydrated alcohol crystallization, fractional crystallization, washing, be drying to obtain.
2. according to the preparation method of the described a kind of Amomicin of claim 1, it is characterized in that the described amount that adds entry is 2 times of amount volumes of raw materials quality.
3. according to the preparation method of the described a kind of Amomicin of claim 1, the molecular weight cutoff value that it is characterized in that described ultra-filtration membrane is 2000 dalton.
4. according to the preparation method of the described a kind of Amomicin of claim 1, it is characterized in that described polymeric amide is selected from a kind of in polyamide fibre 66, the polyamide fibre 6.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105353853A CN102010402A (en) | 2010-11-09 | 2010-11-09 | Method for preparing aloesin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105353853A CN102010402A (en) | 2010-11-09 | 2010-11-09 | Method for preparing aloesin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102010402A true CN102010402A (en) | 2011-04-13 |
Family
ID=43840755
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010105353853A Pending CN102010402A (en) | 2010-11-09 | 2010-11-09 | Method for preparing aloesin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102010402A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102584807A (en) * | 2012-02-06 | 2012-07-18 | 上海华震科技有限公司 | Ethanol liquid extraction process for aloesin |
| CN110437214A (en) * | 2019-09-10 | 2019-11-12 | 杨海鹰 | A kind of purification process of Aloesin |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1483451A (en) * | 2003-07-18 | 2004-03-24 | 王舒妍 | Method for extracting 50% aloetin |
| US20050164957A1 (en) * | 2002-05-03 | 2005-07-28 | Unigen Pharmaceuticals, Inc. | 7-Hydroxy chromones as potent antioxidants |
-
2010
- 2010-11-09 CN CN2010105353853A patent/CN102010402A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050164957A1 (en) * | 2002-05-03 | 2005-07-28 | Unigen Pharmaceuticals, Inc. | 7-Hydroxy chromones as potent antioxidants |
| CN1483451A (en) * | 2003-07-18 | 2004-03-24 | 王舒妍 | Method for extracting 50% aloetin |
Non-Patent Citations (1)
| Title |
|---|
| 杨宏健: "《天然药物化学》", 31 July 2007, article "河南科学技术出版社", pages: 35 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102584807A (en) * | 2012-02-06 | 2012-07-18 | 上海华震科技有限公司 | Ethanol liquid extraction process for aloesin |
| CN110437214A (en) * | 2019-09-10 | 2019-11-12 | 杨海鹰 | A kind of purification process of Aloesin |
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Application publication date: 20110413 |