CN104817566A - Sesamin separation extraction method - Google Patents
Sesamin separation extraction method Download PDFInfo
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- CN104817566A CN104817566A CN201510159296.6A CN201510159296A CN104817566A CN 104817566 A CN104817566 A CN 104817566A CN 201510159296 A CN201510159296 A CN 201510159296A CN 104817566 A CN104817566 A CN 104817566A
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- sesamin
- separating
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- growing
- extracting method
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/02—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains two hetero rings
- C07D493/04—Ortho-condensed systems
Abstract
The present invention discloses a sesamin separation extraction method, which comprises 5 steps such as water bath, evaporation, ether addition standing, crystal growing filtration, and secondary crystal growing, wherein the operation is simple, the process is reasonable, and the efficiency is high. According to the present invention, the crystal growing is performed in twice and comprises: adding dehydrated alcohol to a sesamin crude product, carrying out water bath heating to promote dissolving, placing into a refrigerator to grow the crystal, and filtering; the secondary crystal growing comprises: adding dehydrated alcohol to the sesamin crude product solution, dissolving, carrying out secondary crystal growing in the refrigerator, and repeating twice to obtain the purified sesamin crystal, wherein the sesamin crystal obtained with the operation is purified; and the extraction method has characteristics of simple process, complete extraction, and high production efficiency, and the prepared product has characteristics of high purity, green property, no addition, and quality assurance, and is the sesame product accepted and loved by the majority of people.
Description
Technical field
The present invention relates to a kind of separating and extracting method, particularly relate to a kind of separating and extracting method of sesamin.
Background technology
Sesamin, the root of Araliaceae Panax sessiliflorus, pedaliaceae plant sesame seed or seed oil, in the plants such as goatweed royal paulownia woody part.Sesamin infected by influenza, Sendai virus and tubercule bacillus have restraining effect.Agriculturally be used as the synergistic agent of pyrethrin, clinical observation has certain curative effect to trachitis, for antiviral, sterilant, antioxidant, insecticidal synergist, treatment trachitis.And preparation method's complex process of traditional sesame cake, inefficiency, inferior separating effect, extraction yield is low.In view of above-mentioned defect, be necessary the separating and extracting method designing a kind of sesamin in fact.
Summary of the invention
Technical problem to be solved by this invention is: the separating and extracting method providing a kind of sesamin, solves prior art processes complexity, inefficiency, inferior separating effect, the problem that extraction yield is low.
For solving the problems of the technologies described above, technical scheme of the present invention is: a kind of separating and extracting method of sesamin, it comprises the steps:
(1) water-bath: pulverized by sesame cake meal pulverizer, accurately take 450g, adds 1500ml normal hexane, carries out water-bath, and constantly stirs during water-bath;
(2) evaporate: then filter, filtrate is carried out evaporation with Rotary Evaporators and is removed normal hexane, then adds anhydrous methanol, stirs under temperature is 35 DEG C of-50 DEG C of conditions, after stratification, gets upper liquid and carries out rotary evaporation and remove methyl alcohol;
(3) add ether to leave standstill: add sherwood oil 20mL-30mL in gained material in step (2), leave standstill l h at 40 DEG C after, obtain sesamin crude product;
(4) growing the grain filters: sesamin crude product is added dehydrated alcohol, and heating in water bath is placed in refrigerator and carries out growing the grain, then filter after promoting dissolving;
(5) secondary growing the grain: carry out secondary growing the grain after adding anhydrous alcohol solution again in refrigerator, obtains sesamin purified crystals after repeating 2 times.
Further, described bath temperature is 50-60 DEG C, and the time is 2h.
Further, described churning time is 3h-5h.
Further, described refrigerator temperature is 5 DEG C.
Further, described refrigerator temperature is 4 DEG C.
Further, in described step (2), the ratio of dehydrated alcohol and the middle sesame seed meal crushed material of step (1) is 1:5.
Compared with prior art, the separating and extracting method of this sesamin, through water-bath, evaporate, add that ether leaves standstill, growing the grain filters, secondary growing the grain, altogether 5 procedures, simple to operate, rational technology, efficiency is high.Wherein growing the grain is divided into and carries out for twice, first time growing the grain be that sesamin crude product is added dehydrated alcohol, after heating in water bath promotes to dissolve, be placed in refrigerator and carry out growing the grain, then filter; Second time growing the grain in refrigerator, carries out secondary growing the grain after adding anhydrous alcohol solution again in sesamin crude product solution, obtains sesamin purified crystals after repeating 2 times, and it is purer that this operates the sesamin crystal making to obtain.This extracting method, technique is simple, and extract thoroughly, production efficiency is high, and obtained product purity is high, and green without adding, quality-guarantee is a sesame goods that numerous people accept and like.
Accompanying drawing explanation
Fig. 1 is the separating and extracting method schema of this sesamin
Following embodiment will further illustrate in conjunction with above-mentioned accompanying drawing.
Embodiment
Hereinafter, set forth multiple specific detail, to provide the thorough to the concept forming described embodiment basis.But to one skilled in the art, embodiment described obviously can be put into practice when not have in these specific detail some or all.In other cases, well-known treatment step is not specifically described.
Embodiment 1
As shown in Figure 1, a kind of separating and extracting method of sesamin, it comprises the steps:
(1) water-bath: pulverized by sesame cake meal pulverizer, accurately take 450g, adds 1500ml normal hexane, carries out water-bath, and constantly stirs during water-bath;
(2) evaporate: then filter, filtrate is carried out evaporation with Rotary Evaporators and is removed normal hexane, then adds anhydrous methanol, stirs under temperature is 35 DEG C of conditions, after stratification, gets upper liquid and carries out rotary evaporation and remove methyl alcohol;
(3) add ether to leave standstill: add sherwood oil 20mL in gained material in step (2), leave standstill l h at 40 DEG C after, obtain sesamin crude product;
(4) growing the grain filters: sesamin crude product is added dehydrated alcohol, and heating in water bath is placed in refrigerator and carries out growing the grain, then filter after promoting dissolving;
(5) secondary growing the grain: carry out secondary growing the grain after adding anhydrous alcohol solution again in refrigerator, obtains sesamin purified crystals after repeating 2 times.
Bath temperature of the present invention is 50 DEG C, time is 2h, and described churning time is 3h, and described refrigerator temperature is 5 DEG C, described refrigerator temperature is 4 DEG C, and in described step (2), the ratio of dehydrated alcohol and the middle sesame seed meal crushed material of step (1) is 1:5.
Embodiment 2
As shown in Figure 1, a kind of separating and extracting method of sesamin, it comprises the steps:
(1) water-bath: pulverized by sesame cake meal pulverizer, accurately take 450g, adds 1500ml normal hexane, carries out water-bath, and constantly stirs during water-bath;
(2) evaporate: then filter, filtrate is carried out evaporation with Rotary Evaporators and is removed normal hexane, then adds anhydrous methanol, stirs under temperature is 50 DEG C of conditions, after stratification, gets upper liquid and carries out rotary evaporation and remove methyl alcohol;
(3) add ether to leave standstill: add sherwood oil 30mL in gained material in step (2), leave standstill l h at 40 DEG C after, obtain sesamin crude product;
(4) growing the grain filters: sesamin crude product is added dehydrated alcohol, and heating in water bath is placed in refrigerator and carries out growing the grain, then filter after promoting dissolving;
(5) secondary growing the grain: carry out secondary growing the grain after adding anhydrous alcohol solution again in refrigerator, obtains sesamin purified crystals after repeating 2 times.
Bath temperature of the present invention is 60 DEG C, time is 2h, and described churning time is 5h, and described refrigerator temperature is 5 DEG C, described refrigerator temperature is 4 DEG C, and in described step (2), the ratio of dehydrated alcohol and the middle sesame seed meal crushed material of step (1) is 1:5.
Embodiment 3
As shown in Figure 1, a kind of separating and extracting method of sesamin, it comprises the steps:
(1) water-bath: pulverized by sesame cake meal pulverizer, accurately take 450g, adds 1500ml normal hexane, carries out water-bath, and constantly stirs during water-bath;
(2) evaporate: then filter, filtrate is carried out evaporation with Rotary Evaporators and is removed normal hexane, then adds anhydrous methanol, stirs under temperature is 42 DEG C of conditions, after stratification, gets upper liquid and carries out rotary evaporation and remove methyl alcohol;
(3) add ether to leave standstill: add sherwood oil 25mL in gained material in step (2), leave standstill lh at 40 DEG C after, obtain sesamin crude product;
(4) growing the grain filters: sesamin crude product is added dehydrated alcohol, and heating in water bath is placed in refrigerator and carries out growing the grain, then filter after promoting dissolving;
(5) secondary growing the grain: carry out secondary growing the grain after adding anhydrous alcohol solution again in refrigerator, obtains sesamin purified crystals after repeating 2 times.
Bath temperature of the present invention is 55 DEG C, time is 2h, and described churning time is 4h, and described refrigerator temperature is 5 DEG C, described refrigerator temperature is 4 DEG C, and in described step (2), the ratio of dehydrated alcohol and the middle sesame seed meal crushed material of step (1) is 1:5.
The present invention is not limited to above-mentioned concrete embodiment, and those of ordinary skill in the art is from above-mentioned design, and without performing creative labour, all conversion made, all drop within protection scope of the present invention.
Claims (6)
1. a separating and extracting method for sesamin, is characterized in that comprising the steps:
(1) water-bath: pulverized by sesame cake meal pulverizer, accurately take 450g, adds 1500ml normal hexane, carries out water-bath, and constantly stirs during water-bath;
(2) evaporate: then filter, filtrate is carried out evaporation with Rotary Evaporators and is removed normal hexane, then adds anhydrous methanol, stirs under temperature is 35 DEG C of-50 DEG C of conditions, after stratification, gets upper liquid and carries out rotary evaporation and remove methyl alcohol;
(3) add ether to leave standstill: add sherwood oil 20mL-30mL in gained material in step (2), leave standstill l h at 40 DEG C after, obtain sesamin crude product;
(4) growing the grain filters: sesamin crude product is added dehydrated alcohol, and heating in water bath is placed in refrigerator and carries out growing the grain, then filter after promoting dissolving;
(5) secondary growing the grain: carry out secondary growing the grain after adding anhydrous alcohol solution again in refrigerator, obtains sesamin purified crystals after repeating 2 times.
2. the separating and extracting method of a kind of sesamin as claimed in claim 1, it is characterized in that the bath temperature described in step (1) is 50-60 DEG C, the time is 2h.
3. the separating and extracting method of a kind of sesamin as claimed in claim 1, is characterized in that the churning time described in step (2) is 3h-5h.
4. the separating and extracting method of a kind of sesamin as claimed in claim 1, is characterized in that the refrigerator temperature described in step (4) is 5 DEG C.
5. the separating and extracting method of a kind of sesamin as claimed in claim 1, is characterized in that the refrigerator temperature described in step (5) is 4 DEG C.
6. the separating and extracting method of a kind of sesamin as claimed in claim 1, is characterized in that the ratio of dehydrated alcohol and the middle sesame seed meal crushed material of step (1) in described step (2) is 1:5.
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| CN201510159296.6A CN104817566A (en) | 2015-04-03 | 2015-04-03 | Sesamin separation extraction method |
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| CN201510159296.6A CN104817566A (en) | 2015-04-03 | 2015-04-03 | Sesamin separation extraction method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111205300A (en) * | 2020-01-22 | 2020-05-29 | 河南科技大学 | Method for efficiently extracting sesamin from sesame meal |
| CN112661767A (en) * | 2020-12-04 | 2021-04-16 | 武汉轻工大学 | Method for synchronously preparing sesame concentrated protein, sesame oil and sesamin from sesame cake meal |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040121058A1 (en) * | 2002-08-16 | 2004-06-24 | Ananthasankaran Jayalekshmy | Process for extraction of antioxidants from sesame seed/cake |
| CN1594310A (en) * | 2004-07-01 | 2005-03-16 | 江南大学 | Method for extracting sesamin from sesame oil root |
| JP2006056796A (en) * | 2004-08-18 | 2006-03-02 | J-Oil Mills Inc | Production method of sesame lignan |
| CN101007827A (en) * | 2007-02-01 | 2007-08-01 | 江苏大学 | Method of extracting sesamin from seasame cake |
| KR20100004492A (en) * | 2008-07-04 | 2010-01-13 | 대한민국(관리부서 : 산림청 국립산림과학원장) | Separation method of sesamin from magnolia kobus |
| CN101735234A (en) * | 2009-12-22 | 2010-06-16 | 中国人民解放军军事医学科学院卫生学环境医学研究所 | Preparation process for obtaining high purity sesamin from sesame cake meal |
-
2015
- 2015-04-03 CN CN201510159296.6A patent/CN104817566A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040121058A1 (en) * | 2002-08-16 | 2004-06-24 | Ananthasankaran Jayalekshmy | Process for extraction of antioxidants from sesame seed/cake |
| CN1594310A (en) * | 2004-07-01 | 2005-03-16 | 江南大学 | Method for extracting sesamin from sesame oil root |
| JP2006056796A (en) * | 2004-08-18 | 2006-03-02 | J-Oil Mills Inc | Production method of sesame lignan |
| CN101007827A (en) * | 2007-02-01 | 2007-08-01 | 江苏大学 | Method of extracting sesamin from seasame cake |
| KR20100004492A (en) * | 2008-07-04 | 2010-01-13 | 대한민국(관리부서 : 산림청 국립산림과학원장) | Separation method of sesamin from magnolia kobus |
| CN101735234A (en) * | 2009-12-22 | 2010-06-16 | 中国人民解放军军事医学科学院卫生学环境医学研究所 | Preparation process for obtaining high purity sesamin from sesame cake meal |
Non-Patent Citations (4)
| Title |
|---|
| 张燕飞 等: ""芝麻中芝麻素提取工艺研究进展"", 《粮食与油脂》 * |
| 许荣年 等: ""芝麻油中芝麻素、芝麻林素的研究"", 《食品科学》 * |
| 金青哲 等: ""芝麻油脚中芝麻素的提取与纯化研究"", 《粮油加工与食品机械》 * |
| 陈伟强 等: ""芝麻饼粕中芝麻素的分离提取与HPLC分析"", 《食品研究与开发》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111205300A (en) * | 2020-01-22 | 2020-05-29 | 河南科技大学 | Method for efficiently extracting sesamin from sesame meal |
| CN111205300B (en) * | 2020-01-22 | 2021-12-28 | 河南科技大学 | Method for extracting sesamin from sesame meal |
| CN112661767A (en) * | 2020-12-04 | 2021-04-16 | 武汉轻工大学 | Method for synchronously preparing sesame concentrated protein, sesame oil and sesamin from sesame cake meal |
| CN112661767B (en) * | 2020-12-04 | 2022-06-03 | 武汉轻工大学 | Method for synchronously preparing sesame concentrated protein, sesame oil and sesamin from sesame cake meal |
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Application publication date: 20150805 |