CN103012351B - A kind of purifying technique of natural VE - Google Patents
A kind of purifying technique of natural VE Download PDFInfo
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- CN103012351B CN103012351B CN201210554975.XA CN201210554975A CN103012351B CN 103012351 B CN103012351 B CN 103012351B CN 201210554975 A CN201210554975 A CN 201210554975A CN 103012351 B CN103012351 B CN 103012351B
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Abstract
The invention discloses a kind of purifying technique of natural VE, it is that the crude product natural VE of 10% ~ 30% is for raw material with mass content, employing alcohols, varsol are extraction agent, with crude product natural VE by a certain percentage, at 40 DEG C ~ 60 DEG C after mixed dissolution extraction, be down to 0 DEG C ~ 10 DEG C, leave standstill after analysing solid and filter, filtrate decompression is steamed and desolventizes, obtain natural VE.Present method purification efficiency is high, and the standing cold analysis time shortens greatly, and the content of natural VE is improved 30 ~ 40 percentage points, has the higher rate of recovery simultaneously; In addition, this technical process is simple, low for equipment requirements, and solvent is easy to be recycled, the mobility of gained natural VE and clarity good.
Description
Technical field
The present invention relates to separation engineering technical field, particularly relate to a kind of purifying technique of natural VE.
Background technology
Vitamin-E (VE), have another name called tocopherol, it comprises 8 kinds of materials such as α, β, δ, γ type tocopherol and corresponding tocotrienols, belong to liposoluble vitamin, there is Green Tea Extract, anti-ageing, prevention skin keratin, the physical efficiency immunologic function improving human body and animal and the multiple important physiological function such as cellular immune function, control cardiovascular and cerebrovascular diseases.VE has natural VE and synthesis VE two to originate greatly, natural VE is the mixed tocopherol comprising various of monomer, but natural VE is all better than synthesizing VE from physiologically active or resistance of oxidation, and natural VE is to human non-toxic's side effect, therefore in industries such as food, dietary supplements and makeup, natural VE is subject to the favor of consumers in general.
Natural VE is extensively present in natural animal and plant body, dirty and relative rich can extract containing the material of tocopherol and tocotrienols from various plants grease, leafy vegetable, animal device.Current natural VE mainly comes from Vegetable oil lipoprotein and products thereof.
In prior art, the method for purification of natural VE is mainly divided into the methods such as solvent extration, molecular distillation method, method of chemical treatment and absorption method, but this several method respectively has relative merits.
As disclosed a kind of employing supercritical CO in patent CN1253951A
2the method of extraction and concentration natural VE, it comprises extraction and the multistage continuous separation technology of rectifying tower, and the content of vitamin E finally obtained is 40-70%, but the yield of present method is lower, is only 48% ~ 65%, and supercritical CO
2extraction process equipment requirements and costly.
In patent CN102584769A, disclose a kind of method utilizing polymeric adsorbent purification natural VE, although the method can obtain the natural VE of content more than 99%, the method requires that the content of lipid acid and sterol in raw material is low, and absorption regeneration is difficult.
A kind of method adopting mixed extractant solvent to extract natural VE is disclosed in patent CN147876A, comprise extraction, neutralize, dewater and the step such as distillation, the natural tocopherol level finally obtained and yield higher, but solvent for use system is more complicated, consumption of organic solvent is large, and produces waste water.
Disclosing a kind of in patent CN1263096A take content as the natural VE of 42% ~ 52% is raw material, through organic solvent extractions such as ketone, alcohol, hydrocarbon, cooling is separated out, filtering separation, the method of the step purification natural VEs such as concentrated mother liquor, although the content of natural VE can be improved 5 ~ 15 percentage points by the method, organic solvent consumption used large, the standing cold analysis time is long, purification efficiency is low.
Summary of the invention
The object of the invention is to there is the low problem of purification efficiency in the method for current organic solvent extractionprocess purification natural VE, a kind of purifying technique of natural VE is provided, the method is easy and simple to handle, cost is low, purification efficiency is high, the content of natural VE can be improved 30 ~ 40 percentage points, and have the higher rate of recovery.
Object of the present invention can be achieved through the following technical solutions:
A purifying technique for natural VE, described technique with mass content be the crude product natural VE of 10% ~ 30% for raw material, purification step comprises:
(1) by crude product natural VE and organic solvent, mixed dissolution at 40 DEG C ~ 60 DEG C extracts, upper strata extraction phase and lower floor's extracting phase is obtained after stratification, wherein said organic solvent is one or both in alcoholic solvent, varsol, described alcoholic solvent is one or both in methyl alcohol, ethanol, and described varsol is one or both in normal hexane, sherwood oil;
(2) temperature of above-mentioned extraction phase is down to 0 DEG C ~ 10 DEG C, leaves standstill after separating out solid and filter, filtrate and solid are separated;
(3), after above-mentioned filtrate decompression being steamed solvent, natural VE is obtained.
In the present invention, preferably, the lower floor's extracting phase in described step (1) with after described organic solvent extraction 1 ~ 2 time, merges the organic solvent phase that all extracting and separating obtain again.
In the present invention, preferably, in described step (1), organic solvent is the mixing of alcoholic solvent and varsol, and wherein the volume ratio of alcoholic solvent and varsol is 1:0.1 ~ 1:3, is more preferably 1:0.1 ~ 1:1.
In the present invention, in described step (1), dissolution extraction temperature is preferably 50 DEG C ~ 55 DEG C, and the cooling temperature in step (2) is preferably 5 DEG C ~ 8 DEG C.
In the present invention, preferably, the mass ratio of described crude product natural VE and organic solvent is 1:3 ~ 1:6, is more preferably 1:5.
In the present invention, preferably, the extraction time in described step (1) is 0.1 ~ 1 hour, is more preferably 30 ~ 40min.
In the present invention, preferably, 0.5 ~ 5 hour standing precipitation time in described step (2), 1 ~ 3 hour is more preferably.
In the present invention, preferably, described purification step also comprises the step of the natural VE obtained being carried out molecular distillation, and gained natural VE can obtain the natural VE of content more than 70% again through molecular distillation.
The purifying technique of natural VE of the present invention has the following advantages:
1, present method purification efficiency is high, and the standing cold analysis time shortens greatly, and the content of natural VE is improved 30 ~ 40 percentage points, and has the higher rate of recovery.
2, technical process is simple, low for equipment requirements, and solvent is easy to be recycled, the mobility of gained natural VE and clarity good.
Embodiment
Be clearly and completely described to the technical scheme in the embodiment of the present invention below, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
In the present invention, mass content be 10% ~ 30% crude product natural VE refer to the mass content of natural VE be 10% ~ 30% mixed tocopherols oil, described mixed tocopherol oil can be buied from market, and the T25 mixed tocopherols as Jiangsu Yue Hong Chemical Co., Ltd. or Ningbo Dahongying Bio-engineering Co., Ltd. is oily.
In the present invention, the method for filtrate and solid being separated can adopt customary filtration methods, as the method such as pressure filtration, vacuum filtration realizes.
Embodiment 1
Be crude product natural VE and the 200ml methanol mixed of 14.98% by 40g mass content, extraction stratification after 12 minutes is stirred at 45 DEG C, obtain upper strata extraction phase and lower floor's extracting phase, gained extraction phase is cooled to 5 DEG C, leaves standstill 1 hour, decompress filter after precipitation solid, filtrate is after vacuum distillation recovered solvent, obtain natural VE concentrated product 9.97g, wherein the content of natural VE is 51.57%, and total recovery is 85.8%.
Embodiment 2
By 40g mass content be 14.98% crude product natural VE mix with sherwood oil with 120ml methyl alcohol, wherein the volume ratio of methyl alcohol and sherwood oil is 1:3, extraction stratification after 30 minutes is stirred at 55 DEG C, obtain upper strata extraction phase and lower floor's extracting phase, gained extraction phase is cooled to 10 DEG C, leave standstill 5 hours, decompress filter after precipitation solid, filtrate is after vacuum distillation recovered solvent, obtain natural VE concentrated product 10.55g, wherein the content of natural VE is 50.41%, and total recovery is 88.74%.
Embodiment 3
By 40g mass content be 21.26% crude product natural VE mix with 240ml ethanol and normal hexane, wherein the volume ratio of ethanol and normal hexane is 1:0.1, extraction stratification after 1 hour is stirred at 50 DEG C, obtain upper strata extraction phase and lower floor's extracting phase, gained extraction phase is cooled to 0 DEG C, leave standstill 30 minutes, decompress filter after precipitation solid, filtrate is after vacuum distillation recovered solvent, obtain natural VE concentrated product 13.35g, wherein the content of natural VE is 55.31%, and total recovery is 86.82%.
Embodiment 4
By 40g mass content be 30.0% crude product natural VE mix with 200ml ethanol, extraction stratification after 10 minutes is stirred at 60 DEG C, obtain upper strata extraction phase and lower floor's extracting phase, gained extraction phase is cooled to 8 DEG C, leaves standstill 1 hour, decompress filter after precipitation solid, filtrate is after vacuum distillation recovered solvent, obtain natural VE concentrated product 16.08g, wherein the content of natural VE is 64.26%, and total recovery is 86.12%.By gained content be the natural VE concentrated product of 64.26% after molecular distillation, obtain the natural VE that content is 70.63%.
Embodiment 5
By 40g mass content be 25.8% crude product natural VE mix with 200ml methyl alcohol and normal hexane, wherein the volume ratio of methyl alcohol and normal hexane is 1:1, extraction stratification after 30 minutes is stirred at 55 DEG C, obtain upper strata extraction phase and lower floor's extracting phase, use 100ml methyl alcohol and normal hexane mixed solvent to lower floor's extracting phase extracting twice again, wherein the volume ratio of methyl alcohol and normal hexane is 1:1, standing separation obtains upper strata extraction phase, after merging the upper strata extraction phase that all extractions obtain, gained extraction phase is cooled to 8 DEG C, leave standstill 1 hour, decompress filter after precipitation solid, filtrate is after vacuum distillation recovered solvent, obtain natural VE concentrated product 15.31g, wherein the content of natural VE is 59.04%, total recovery is 87.59%.
The above; be only the better embodiment of the present invention, but protection scope of the present invention is not limited to therewith, be anyly familiar with those skilled in the art in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.
Claims (6)
1. a purifying technique for natural VE, described technique with mass content be the crude product natural VE of 10% ~ 30% for raw material, purification step comprises:
(1) by crude product natural VE and organic solvent, mixed dissolution at 40 DEG C ~ 60 DEG C extracts, upper strata extraction phase and lower floor's extracting phase is obtained after stratification, wherein said organic solvent is the mixing of alcoholic solvent and varsol, and wherein the volume ratio of alcoholic solvent and varsol is 1:0.1 ~ 1:3; Described alcoholic solvent is one or both in methyl alcohol, ethanol, and described varsol is one or both in normal hexane, sherwood oil;
(2) temperature of above-mentioned extraction phase is down to 0 DEG C ~ 10 DEG C, leaves standstill after separating out solid and filter, filtrate and solid are separated;
(3), after above-mentioned filtrate decompression being steamed solvent, natural VE is obtained.
2. the purifying technique of natural VE as claimed in claim 1, it is characterized in that, the lower floor's extracting phase in described step (1) with after described organic solvent extraction 1 ~ 2 time, merges the extraction phase that all extracting and separating obtain again.
3. the purifying technique of natural VE as claimed in claim 1, it is characterized in that, the mass ratio of described crude product natural VE and organic solvent is 1:3 ~ 1:6.
4. the purifying technique of natural VE as claimed in claim 1 or 2, it is characterized in that, the extraction time in described step (1) is 0.1 ~ 1 hour.
5. the purifying technique of natural VE as claimed in claim 1 or 2, is characterized in that, 0.5 ~ 5 hour standing precipitation time in described step (2).
6. the purifying technique of natural VE as claimed in claim 1 or 2, it is characterized in that, described purification step also comprises the step of the natural VE obtained being carried out molecular distillation.
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| CN201210554975.XA CN103012351B (en) | 2012-09-03 | 2012-12-19 | A kind of purifying technique of natural VE |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103323554B (en) * | 2013-07-03 | 2014-12-03 | 大连民族学院 | Analyzing and detecting method of vitamin E in deer product |
| CN103588744B (en) * | 2013-10-31 | 2016-01-13 | 宁波大红鹰生物工程股份有限公司 | Remove the method for fluidizer in natural VE |
| CN106480122B (en) * | 2016-09-05 | 2019-06-07 | 雄九（上海）医药技术股份有限公司 | The production method of vitamin E |
| CN106831922B (en) * | 2017-01-22 | 2018-11-23 | 山东圣地嘉禾生物工程有限公司 | The method of one-step method separating high-purity phytosterol and vitamin E |
| CN113121490B (en) * | 2019-12-31 | 2023-06-16 | 宜春大海龟生命科学有限公司 | Preparation method of sunflower oil-derived natural vitamin E |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3615029A1 (en) * | 1985-05-06 | 1986-11-06 | Henkel Corp., Minneapolis, Minn. | METHANOL EXTRACTION OF TOCOPHEROL |
| CN1263096A (en) * | 1999-12-24 | 2000-08-16 | 上海交通大学 | Method for raising natural vitamin E concentrate transparency and fluidity |
| CN1478776A (en) * | 2002-08-30 | 2004-03-03 | 宁波大红鹰生物工程股份有限公司 | Extraction and purification technology of natural vitamin E |
-
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- 2012-12-19 CN CN201210554975.XA patent/CN103012351B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3615029A1 (en) * | 1985-05-06 | 1986-11-06 | Henkel Corp., Minneapolis, Minn. | METHANOL EXTRACTION OF TOCOPHEROL |
| CN1263096A (en) * | 1999-12-24 | 2000-08-16 | 上海交通大学 | Method for raising natural vitamin E concentrate transparency and fluidity |
| CN1478776A (en) * | 2002-08-30 | 2004-03-03 | 宁波大红鹰生物工程股份有限公司 | Extraction and purification technology of natural vitamin E |
Non-Patent Citations (1)
| Title |
|---|
| 溶剂法纯化天然维生素E的试验研究;张倩等;《油脂工程.技术》;20081231;第69-71页 * |
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