CN101190919A - Method for extracting and preparing sesamin by using HZ816 modified resin - Google Patents
Method for extracting and preparing sesamin by using HZ816 modified resin Download PDFInfo
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- CN101190919A CN101190919A CNA2007100437579A CN200710043757A CN101190919A CN 101190919 A CN101190919 A CN 101190919A CN A2007100437579 A CNA2007100437579 A CN A2007100437579A CN 200710043757 A CN200710043757 A CN 200710043757A CN 101190919 A CN101190919 A CN 101190919A
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- sesamin
- resin
- sesame oil
- modified resin
- adsorption
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Abstract
The invention discloses a method of extracting and preparing sesamin by using HZ816 modified resin, which consists of the steps that dry resin and sesame oil are treated with countercurrent mixed adsorption on adsorption columns and then separated to remove ionized sesame oil; the residual sesame oil on the adsorption columns is then washed by n-hexane; finally methanol is used for eluting the sesamin adsorbed on the resin. Sesamin pastes with trace oil can be obtained by heating and recovering the methanol and products with the sesamin content of about 60 percent can be obtained after the trace oil of the sesamin pastes is removed. The invention improves the efficiency of the separation and extraction of the sesamin, simplifies the operation process and improves the economic value of the sesame oil after adsorption.
Description
Technical field
The present invention relates to the extracting method of sesamin, relate to adopt the method for HZ816 modified resin direct adsorbing and extracting sesamin from contain the sesamin raw material specifically.
Background technology
Sesamin is the natural constituents in the sesame, and molecular formula is C
20H
18O
6, molecular weight is 354.34.The fusing point of sesamin is fat-soluble cpds generally at 120～121 ℃, has the uv-absorbing of feature at 287nm and 236nm.Has opticity, [α]
20 D=-56 ° of (CHCl
3).
The early stage main auxiliary of sesamin as pyrethrum insecticide; along with further investigation to sesamin; find that it has many important physical active functions; as have anti-microbial activity, anti-oxidant activity, hypertension, adjusting fat and an alcohol metabolism, the protection liver, reduce cholesterol concentration in serum and the liver, antitumor etc.
The extracting method of existing sesamin mainly contains two classes, and first kind method is with United States Patent (USP) 5,209, and 826 are representative, and alkaline chemical precipitation separates sesamin from the sesame oil deodorization distillate; Second class methods were just implemented by people such as Allen L in 1949, extracted sesamin with the methyl alcohol equal solvent from sesame oil.In addition, China's number of patent application is that the method for adsorbing sesamin with neutral alumina from sesame oil has been reported in 03113181.6 research.
First kind method is suitable for having the production process of sesame oil deodorizing technology, and the domestic present technology of sesame oil manufacturing enterprise of China does not reach this level as yet, therefore, adopts this method separation and Extraction sesamin still not have feasibility in China.The edibleness that second class methods are extracted back sesame oil completely loses, and is difficult to make alcohol extract not to be with sesame oil, therefore, also needs saponification sesamin could be separated after extraction is finished, problems such as the separation of follow-up alkali in addition, moisture removal.Number of patent application is 03113181.6 research report, and when adopting alumina adsorption, 100 gram oil requires use 70～80 gram aluminum oxide, the originally all oxidized aluminium absorption of oil base during actually operating, the separation difficulty of sesame oil and aluminum oxide, and complicated operating process.
Summary of the invention
Sesame oil after technical problem to be solved by this invention is to provide a kind of and overcomes the extraction process complexity, the resid amount height that exist in the existing sesamin extraction and separation process, is extracted is worth a kind of method for preparing sesamin of extracting with HZ816 modified resin of serious degradation shortcoming down.
Technical problem solved by the invention can realize by the following technical solutions:
A kind of method for preparing sesamin of extracting with HZ816 modified resin, it is at first the exsiccant HZ816 resin adsorption column of packing into, in adverse current blended mode sesame oil is slowly injected from the column bottom, with HZ816 modified resin uniform mixing, after reaching adsorption equilibrium, with sesame oil residual on the normal hexane washing column, then with the sesamin that adsorbs on the methanol-eluted fractions resin; Heating recovery methyl alcohol obtains containing micro-greasy sesamin lotion; Add micro-ether and stir, standing demix promptly obtains the sesamin powder after the solid substance drying.
In the present invention, described HZ816 resin is packed into before the adsorption column, with dehydrated alcohol HZ816 modified resin is thoroughly cleaned earlier, gets rid of free ethanol, 55 ℃ of following vacuum-dryings 4 hours.
In the methods of the invention, the void volume of described adsorption column top is 2 times of HZ816 resin volume at least.
The present invention has improved the efficient of separation and Extraction sesamin, has simplified the operating procedure process, has improved the economic worth through the sesame oil after the absorption, and HZ816 modified resin can be reused through after the solvent cleaning.The stripping workshop that is rich in sesamin need not saponification, can directly adopt crystallization processes, obtains the sesamin product.Preliminary crystalline sesamin purity is about 60%.
Embodiment
For technique means, creation characteristic that the present invention is realized, reach purpose and effect is easy to understand, below in conjunction with embodiment, further set forth the present invention.
Embodiment 1
100 gram HZ816 modified resin dress posts, at room temperature the flow velocity with 2g/min flows through adsorption column by 1000ml sesame oil, sesamin content is 0.3289% in the original sesame oil, through sesamin concentration in the sesame oil behind the polymeric adsorbent is 0.3104%, and the adsorptive power of resin is the 1.85mg/g dried resin.The resin of finishing absorption at first needs emptying free sesame oil, uses the sesame oil of normal hexane flush away remnants then, uses the sesamin on the methanol-eluted fractions resin again.Boil off methyl alcohol after collecting the capacity meoh eluate, add micro-ether, stir, leave standstill hypsokinesis and go out the oil-containing ether, it is 59% powder that drying obtains sesamin content.
Embodiment 2
100 gram HZ816 modified resin dress posts, at room temperature the flow velocity with 2g/min flows through adsorption column by 1000ml sesame oil, sesamin content is 0.5424% in the original sesame oil, is 0.5074% through sesamin concentration in the sesame oil behind the polymeric adsorbent, and the adsorptive power of resin is the 3.5mg/g dried resin.The resin of finishing absorption at first needs emptying free sesame oil, uses the sesame oil of normal hexane flush away remnants then, uses the sesamin on the methanol-eluted fractions resin again.Boil off methyl alcohol after collecting the capacity meoh eluate, add ether, stir, leave standstill hypsokinesis and go out the oil-containing ether, it is 60% powder that drying obtains sesamin content.
Embodiment 3
20 gram HZ816 modified resin dress posts, at room temperature the flow velocity with 2g/min flows through adsorption column by 700ml sesame oil, sesamin content is 0.5424% in the original sesame oil, is 0.4970% through sesamin concentration in the sesame oil behind the polymeric adsorbent, and the adsorptive power of resin is the 15.9mg/g dried resin.The resin of finishing absorption at first needs emptying free sesame oil, uses the sesame oil of normal hexane flush away remnants then, uses the sesamin on the methanol-eluted fractions resin again.Boil off methyl alcohol after collecting the capacity meoh eluate, add micro-ether, stir, leave standstill hypsokinesis and go out the oil-containing ether, it is 58% powder that drying obtains sesamin content.
Embodiment 4
20 gram HZ816 modified resin dress posts, at room temperature the flow velocity with 2g/min flows through adsorption column by 1500ml sesame oil, sesamin content is 0.5424% in the original sesame oil, is 0.4984% through sesamin concentration in the sesame oil behind the polymeric adsorbent, and the adsorptive power of resin is the 33mg/g dried resin.The resin of finishing absorption at first needs emptying free sesame oil, uses the sesame oil of normal hexane flush away remnants then, uses the sesamin on the methanol-eluted fractions resin again.Boil off methyl alcohol after collecting the capacity meoh eluate, add micro-ether, stir, leave standstill hypsokinesis and go out the oil-containing ether, it is 61% powder that drying obtains sesamin content.
Embodiment 5
20 gram HZ816 modified resin dress posts, at room temperature cross adsorption column by 1500ml sesame oil cycling stream, co-adsorption 12 hours with the flow velocity of 2g/min.Sesamin content is 0.5424% in the original sesame oil, after the adsorption equilibrium in the sesame oil sesamin concentration be 0.4921%, the adsorptive power of resin is the 37.7mg/g dried resin.The resin of finishing absorption at first needs emptying free sesame oil, uses the sesame oil of normal hexane flush away remnants then, uses the sesamin on the methanol-eluted fractions resin again.Boil off methyl alcohol after collecting the capacity meoh eluate, add micro-ether, stir, leave standstill hypsokinesis and go out the oil-containing ether, it is 62% powder that drying obtains sesamin content.
More than show and described ultimate principle of the present invention, principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that describes in the foregoing description and the specification sheets just illustrates principle of the present invention; the present invention also has various changes and modifications without departing from the spirit and scope of the present invention, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is made up of appending claims and equivalent thereof.
Claims (4)
1. one kind is extracted the method prepare sesamin with HZ816 modified resin, it is characterized in that at first the exsiccant HZ816 resin adsorption column of packing into, sesame oil is slowly injected, with HZ816 modified resin uniform mixing, after reaching adsorption equilibrium, with sesame oil residual on the normal hexane washing column, then with the sesamin that adsorbs on the methanol-eluted fractions resin; Heating recovery methyl alcohol obtains containing micro-greasy sesamin lotion; Add micro-ether and stir, standing demix promptly obtains the sesamin powder after the solid substance drying.
2. a kind of method for preparing sesamin of extracting with HZ816 modified resin according to claim 1, it is characterized in that described HZ816 resin is packed into before the adsorption column, with dehydrated alcohol HZ816 modified resin is thoroughly cleaned earlier, get rid of free ethanol, 55 ℃ of following vacuum-dryings 4 hours.
3. a kind of HZ816 of using modified resin according to claim 1 extracts the method for preparing sesamin, it is characterized in that, the void volume of described adsorption column top is 2 times of HZ816 resin volume at least.
4. a kind of HZ816 of using modified resin as claimed in claim 1 extracts the method for preparing sesamin, it is characterized in that, described sesame oil injects from dry HZ816 modified resin adsorption column bottom is housed with reflux type.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100437579A CN100556907C (en) | 2007-07-13 | 2007-07-13 | A kind of method for preparing sesamin of extracting with HZ816 modified resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100437579A CN100556907C (en) | 2007-07-13 | 2007-07-13 | A kind of method for preparing sesamin of extracting with HZ816 modified resin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101190919A true CN101190919A (en) | 2008-06-04 |
| CN100556907C CN100556907C (en) | 2009-11-04 |
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ID=39486134
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|---|---|---|---|
| CNB2007100437579A Expired - Fee Related CN100556907C (en) | 2007-07-13 | 2007-07-13 | A kind of method for preparing sesamin of extracting with HZ816 modified resin |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102441018A (en) * | 2011-12-06 | 2012-05-09 | 湖南农业大学 | Method for separating and purifying eupatorium odoratum flavonoid substance by using HZ816 macroporous adsorption resin |
| CN104177370A (en) * | 2014-09-04 | 2014-12-03 | 陕西源邦生物技术有限公司 | Method for preparing high-content sesamin from sesame seed meal |
| CN105732652A (en) * | 2016-04-14 | 2016-07-06 | 滁州尹氏油脂有限公司 | Method for extracting sesamin from sesame meal |
-
2007
- 2007-07-13 CN CNB2007100437579A patent/CN100556907C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102441018A (en) * | 2011-12-06 | 2012-05-09 | 湖南农业大学 | Method for separating and purifying eupatorium odoratum flavonoid substance by using HZ816 macroporous adsorption resin |
| CN104177370A (en) * | 2014-09-04 | 2014-12-03 | 陕西源邦生物技术有限公司 | Method for preparing high-content sesamin from sesame seed meal |
| CN105732652A (en) * | 2016-04-14 | 2016-07-06 | 滁州尹氏油脂有限公司 | Method for extracting sesamin from sesame meal |
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| Publication number | Publication date |
|---|---|
| CN100556907C (en) | 2009-11-04 |
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Granted publication date: 20091104 Termination date: 20180713 |