CN108822176A - A kind of technique that enzyme process esterification free fatty acid extracts phytosterol - Google Patents
A kind of technique that enzyme process esterification free fatty acid extracts phytosterol Download PDFInfo
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- CN108822176A CN108822176A CN201810596234.5A CN201810596234A CN108822176A CN 108822176 A CN108822176 A CN 108822176A CN 201810596234 A CN201810596234 A CN 201810596234A CN 108822176 A CN108822176 A CN 108822176A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J9/00—Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of more than two carbon atoms, e.g. cholane, cholestane, coprostane
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Abstract
The present invention relates to phytosterol extractive technique fields, and in particular to a kind of technique that enzyme process esterification free fatty acid extracts phytosterol.Enzymatic treatment deodorization distillate technique of the present invention has the advantages such as reaction condition is mild, by-product is few compared with existing chemical catalyst method processing deodorization distillate technique at present.Meanwhile compared with enzyme process transesterification process deodorization distillate technique emerging at present, has the advantages that not use hazardous organic solvents, do not generate harmful side product.Solve the production security risk of raw material in phytosterol extraction process, meanwhile, it is phytosterol broader applications in field of food, provides more green safe process routes.
Description
Technical field
The present invention relates to phytosterol extractive technique fields, and in particular to a kind of enzyme process esterification free fatty acid extraction plant
The technique of sterol.
Background technique
Phytosterol (phytosterols) is primarily present in plant cell membrane, in each vegetable oil, nut and plant
Rich content in seed, especially content is higher in rice bran oil, rapeseed oil and corn oil.Phytosterol has good life
Manage function, have serum cholesterol-lowering, reducing blood lipid, it is antitumor, reduce heart disease incidence the effects of.As masses are to own health
More and more pay attention to, phytosterol is also increasingly favored by masses.
In vegetable oil industry, refining process causes a large amount of losses of phytosterol, such as in refining process generally
Deodorization procedures are needed, i.e., removes the impurity such as the fatty acid in vegetable oil by the way of high-temperature vacuum, extends vegetable oil products
Shelf life.And during vegetable oil deodorized, the byproduct of evaporative condenser is deodorization distillate, and main component is free-fat
Acid, neutral grease, phytosterol, natural VE and pigment etc..In the prior art, plant steroid is extracted from deodorization distillate
The process of alcohol, there are mainly two types of：
The first is to use strong acid or other chemicals as catalyst, by free fatty acid and neutral grease, in catalyst
Under effect, in the presence of excessive methanol, esterification occurs and generates fatty acid methyl ester, further plant steroid is isolated in cooling
Alcohol, referring to Chinese patent CN1074217A.Some Research Literatures and patent have carried out certain improvement in terms of acid catalyst, have adopted
With solid acid etc., referring to Chinese patent CN102229641B.The defect of such method is：One side strong acid and strong base, to equipment material
Matter is more demanding, tediously long to the reaction material liquid complex treatment process after the completion of esterification, meanwhile, processing soda acid, which can generate, largely to be contained
Oily brine waste can adversely affect environment；On the other hand this using chemicals such as strong acid as catalyst, it can be to locating
The raw material of reason --- original component in deodorization distillate causes centainly to destroy.
Second is enzyme reaction, replaces conventional strong acid transesterification anti-as catalyst progress using enzyme preparations such as lipase
Should after extract corresponding product, referring to Chinese patent CN1563399A.The above two classes technique, basic ideas are by strong acid or enzyme
Preparation generates fatty acid methyl ester as fatty acid in catalyst deodorization distillate and methanol, and then carries out point of target product
From extraction.On the one hand have the shortcomings that explosion danger and Health cost as solvent using methanol；On the other hand, in production work
During skill, there is the generation of fatty acid methyl ester by-product, and the fatty acid methyl ester generated has certain harm to human body, to plant
The safety of sterol will also result in potential risk, thus, the extracted plant sterol product of such technique is also not suitable for as food
Product additive use.
Summary of the invention
To solve problems of the prior art, the present invention proposes that a kind of technical process is easy, economically viable from plant
The method of object oil deodorization distillate extraction phytosterol.This method can succeed extracts plant steroid from plant oil deodorizing distillate
Alcohol, and the potential risk of fatty acid methyl ester is eliminated, specific technical solution is as follows.
A kind of enzyme process esterification free fatty acid extracts the technique of phytosterol, comprises the following steps that：
（1）Pretreatment of raw material：Deodorization distillate raw material is warming up to 60-80 DEG C, then adjusts its pH, controls the pH of reaction system
System is 6.0 ~ 7.5；
（2）Enzyme reaction：Glycerol or ethyl alcohol are added into step 1 gained deodorization distillate, are and the fatty acid in deodorization distillate
Reaction, provides required substrate, when temperature of reaction system is down to 50-70 DEG C, by 0.2 wt% -2 wt of deodorization distillate mass ratio
% is added lipase and stirs evenly, and temperature of reaction system is maintained 50-70 DEG C, mixing speed is 30-100 r/min, instead
Answering the period is 6-36 hours, until the acid value of reaction system no longer changes, terminates reaction；
（3）Depth depickling：Reaction system is warming up to 75 ~ 85 DEG C, adds the sig water that mass concentration is 8-22%, homogeneous, and tie up
It holds 75 ~ 85 DEG C of temperature 10 ~ 30 minutes, is centrifuged, discards precipitating；
（4）Decoloring reaction：Under vacuum conditions, temperature of reaction system is increased to 80-100 DEG C, addition decolorising agent stirring is decolourized
Filtering, obtains filtrate；
（5）(0-7 DEG C) of filtrate low temperature is stood（5-24 hours）, it is centrifuged, abandons supernatant, obtain crystal settling, as phytosterol
Crude product.
Preferably, adding the hydrogen that mass concentration is é -18 ° of B é of 10 ° of B into deodorization distillate raw material in the step 1
Sodium hydroxide solution, adjusts its pH, and the additive amount of sodium hydroxide solution is 100 ~ 300ppm of deodorization distillate quality.
Preferably, the additive amount of glycerol or ethyl alcohol is the 8 ~ 12% of deodorization distillate quality in the step 2.
Preferably, the additive amount of lipase is the 0.2 ~ 2% of deodorization distillate quality in the step 2.
Preferably, it is 40-70 DEG C that reaction system, which carries out temperature when enzyme reaction process, in the step 2.
Preferably, decolorising agent is active carbon in the step 4, the additive amount of active carbon is the 0.5- of reaction system quality
2%。
Preferably, adding the sodium hydroxide solution of mass concentration 8-22%, in terms of pure cerium hydroxide sodium, hydrogen in the step 3
Sodium oxide molybdena additive amount is 10 ~ 18% of fatty acid quality in reaction solution, homogeneous, and maintain 75-85 DEG C of temperature 10-30 minutes, from
The heart discards precipitating, obtains upper layer filtrate.
It is then centrifuged for preferably, standing 5 ~ 24 hours under the conditions of placing reaction liquid into 0 ~ 7 DEG C in the step 5.
Beneficial effect
The invention discloses a kind of technical process simplicity, the economically viable side that phytosterol is extracted from plant oil deodorizing distillate
Method.This method can succeed the potential risk extracted phytosterol from plant oil deodorizing distillate, and eliminate harmful side product.
Enzymatic treatment deodorization distillate technique of the present invention is deodorized with existing chemical catalyst method processing at present
Distillate technique is compared, and is had the advantage that：Reaction condition is mild, it is low to require equipment material, and technical process is easy, to environment
It is more friendly, it can retain that handled raw material --- original component in deodorization distillate, byproduct of reaction are few to greatest extent.
The present invention has the advantage that compared with enzyme process transesterification process deodorization distillate technique emerging at present：It does not adopt
With hazardous organic solvents --- methanol has technique friendly and safety, does not generate harmful by-product in technical process
Object --- fatty acid methyl ester, there is no the possibility of fatty acid methyl ester Pollution Plant sterol, whole process be not related to harmful material and
Intermediate product, and the advantages that reaction condition green is mild, and gained target product is safe and reliable.Solves phytosterol extraction process
The production security risk of middle raw material, meanwhile, it is phytosterol broader applications in field of food, provides more green safe
Process routes.
Specific embodiment
Embodiment 1
A kind of enzyme process esterification free fatty acid extracts the technique of phytosterol, includes the following steps：100g deodorization distillate is former
Material is warming up to 60 DEG C, adds the sodium hydroxide solution 0.2g of 10 % (w/w), stirs evenly, and measures reaction system pH at this time and is
6.0.The glycerol of deodorization distillate quality 8%, i.e. 8g are added into deodorization distillate.Lipase is added to stir evenly.60℃,
180rpm revolving speed is stirred to react 15 hours.Reaction terminates, and content of fatty acid is 10% in reaction system.10 are added into reaction solution
% (w/w) sodium hydroxide solution 14g, homogeneous, and maintain 75-85 DEG C of temperature 10-30 minutes.Centrifugation, discards precipitating.By supernatant
2g atlapulgite is added, vacuum decoloration 30 minutes at 95 DEG C, filtering stands 12-24 hours under the conditions of taking filtrate to be placed in 0-7 DEG C,
Supernatant is abandoned in centrifugation, and obtaining sample quality after crystal drying is 5g, i.e. phytosterol crude product, and content of phytosterol is after measured
65%。
Embodiment 2
A kind of enzyme process esterification free fatty acid extracts the technique of phytosterol, includes the following steps：100g deodorization distillate is former
Material is warming up to 60 DEG C, adds the sodium hydroxide solution 0.2g of 10 % (w/w), stirs evenly, and measures reaction system pH at this time and is
6.0.The glycerol of deodorization distillate quality 10%, i.e. 10g are added into deodorization distillate.Lipase is added to stir evenly.60℃,
180rpm revolving speed is stirred to react 15 hours.Reaction terminates, and content of fatty acid is 8.5% in reaction system.After decolorization filtering, to anti-
It answers and adds 10 % (w/w) sodium hydroxide solution 12.1g, homogeneous in liquid, and maintain 75-85 DEG C of temperature 10-30 minutes.Centrifugation is abandoned
It goes to precipitate.2g atlapulgite is added in supernatant, vacuum decoloration 30 minutes at 95 DEG C, filtering takes filtrate to be placed under the conditions of 0-7 DEG C
12-24 hour are stood, supernatant is abandoned in centrifugation, and obtaining sample quality after crystal drying is 5.5g, i.e. phytosterol crude product, after measured
Content of phytosterol is 63.5%.
Embodiment 3
A kind of enzyme process esterification free fatty acid extracts the technique of phytosterol, includes the following steps：100g deodorization distillate is former
Material is warming up to 60 DEG C, adds the sodium hydroxide solution 0.2g of 10 % (w/w), stirs evenly, and measures reaction system pH at this time and is
6.0.The glycerol of deodorization distillate quality 12%, i.e. 12g are added into deodorization distillate.Lipase is added to stir evenly.60℃,
180rpm revolving speed is stirred to react 15 hours.Reaction terminates, and content of fatty acid is 7.5% in reaction system.After decolorization filtering, to anti-
It answers and adds 10 % (w/w) sodium hydroxide solution, 10.7 g, homogeneous in liquid, and maintain 75-85 DEG C of temperature 10-30 minutes.Centrifugation is abandoned
It goes to precipitate.2g atlapulgite is added in supernatant, vacuum decoloration 30 minutes at 95 DEG C, filtering takes filtrate to be placed under the conditions of 0-7 DEG C
12-24 hour are stood, supernatant is abandoned in centrifugation, and obtaining sample quality after crystal drying is 6.1g, i.e. phytosterol crude product, after measured
Content of phytosterol is 62%.
Claims (8)
1. a kind of technique that enzyme process esterification free fatty acid extracts phytosterol, which is characterized in that comprise the following steps that：
（1）Pretreatment of raw material：Deodorization distillate raw material is warming up to 60-80 DEG C, then adjusts its pH, controls the pH of reaction system
System is 6.0 ~ 7.5；
（2）Enzyme reaction：Glycerol or ethyl alcohol are added into step 1 gained deodorization distillate, are down to 50-70 DEG C to temperature of reaction system
When, lipase is added and stirs evenly, reacts to the acid value of system and no longer changes, terminates reaction；
（3）Depth depickling：Reaction system is warming up to 75 ~ 85 DEG C, makes enzyme-deactivating, adds the sig water that mass concentration is 8-22%,
Homogeneous, and maintain 75 ~ 85 DEG C temperature 10 ~ 30 minutes, centrifugation discards precipitating；
（4）Decoloring reaction：Under vacuum conditions, temperature of reaction system is increased to 80-100 DEG C, addition decolorising agent stirs, mistake
Filter, obtains filtrate；
（5）Filtrate is stood, is centrifuged, supernatant is abandoned, obtains crystal settling, as phytosterol crude product.
2. the technique that enzyme process esterification free fatty acid according to claim 1 extracts phytosterol, which is characterized in that described
In step 1, the sodium hydroxide solution that mass concentration is é -18 ° of B é of 10 ° of B is added into deodorization distillate raw material, adjusts its pH, hydrogen
The additive amount of sodium hydroxide solution is 100 ~ 300ppm of deodorization distillate quality.
3. the technique that enzyme process esterification free fatty acid according to claim 1 extracts phytosterol, which is characterized in that described
Glycerol or ethyl alcohol additive amount are the 8 ~ 12% of deodorization distillate quality in step 2.
4. the technique that enzyme process esterification free fatty acid according to claim 1 extracts phytosterol, which is characterized in that described
The additive amount of lipase is the 0.2 ~ 2% of deodorization distillate quality in step 2.
5. the technique that enzyme process esterification free fatty acid according to claim 1 extracts phytosterol, which is characterized in that described
It is 50-70 DEG C that reaction system, which carries out temperature when enzyme reaction process, in step 2, and mixing speed is 30-100 r/min, reaction time
It is 6-36 hours.
6. the technique that enzyme process esterification free fatty acid according to claim 1 extracts phytosterol, which is characterized in that described
Decolorising agent is active carbon or atlapulgite in step 4, and the additive amount of active carbon or atlapulgite is the 0.5- of reaction system quality
2%。
7. the technique that enzyme process esterification free fatty acid according to claim 1 extracts phytosterol, which is characterized in that described
The sodium hydroxide solution that mass concentration 8-22% is added in step 3, in terms of pure cerium hydroxide sodium, sodium hydroxide additive amount is reaction solution
The 10 ~ 18% of middle fatty acid quality, homogeneous, and maintain 75-85 DEG C of temperature 10-30 minutes, it is centrifuged, discards precipitating, obtain upper layer filter
Liquid.
8. the technique that enzyme process esterification free fatty acid according to claim 1 extracts phytosterol, which is characterized in that described
5 ~ 24 hours are stood under the conditions of filtrate is placed in 0 ~ 7 DEG C in step 5 to be then centrifuged for.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112300238A (en) * | 2020-09-23 | 2021-02-02 | 福建福迩金生物科技有限公司 | Method for extracting phytosterol from soybeans |
Citations (6)
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|---|---|---|---|---|
| JPS49489A (en) * | 1972-04-17 | 1974-01-05 | ||
| CN1563399A (en) * | 2004-03-18 | 2005-01-12 | 清华大学 | New technique for extracting vitamin C and sterol from distillation of deodorizing vegetable oil |
| CN101225414A (en) * | 2008-01-09 | 2008-07-23 | 河南工业大学 | Novel method for extracting natural vitamin E, phytosterol, fatty acid methyl ester by enzyme catalysis and molecular distillation |
| CN103045664A (en) * | 2012-12-15 | 2013-04-17 | 华中科技大学 | Method for producing biodiesel, sterol and vitamin E from deodorized distillate |
| CN106977582A (en) * | 2017-05-10 | 2017-07-25 | 福建省格兰尼生物工程股份有限公司 | A kind of method of Hydrolysis kinetics phytosterol in deodorization distillate |
| CN107216253A (en) * | 2016-03-22 | 2017-09-29 | 浙江医药股份有限公司新昌制药厂 | A kind of utilization enzyme-chemically United Technologies extract the production method of VE, sterol from soybean oil deodorizer distillate |
-
2018
- 2018-06-11 CN CN201810596234.5A patent/CN108822176A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS49489A (en) * | 1972-04-17 | 1974-01-05 | ||
| CN1563399A (en) * | 2004-03-18 | 2005-01-12 | 清华大学 | New technique for extracting vitamin C and sterol from distillation of deodorizing vegetable oil |
| CN101225414A (en) * | 2008-01-09 | 2008-07-23 | 河南工业大学 | Novel method for extracting natural vitamin E, phytosterol, fatty acid methyl ester by enzyme catalysis and molecular distillation |
| CN103045664A (en) * | 2012-12-15 | 2013-04-17 | 华中科技大学 | Method for producing biodiesel, sterol and vitamin E from deodorized distillate |
| CN107216253A (en) * | 2016-03-22 | 2017-09-29 | 浙江医药股份有限公司新昌制药厂 | A kind of utilization enzyme-chemically United Technologies extract the production method of VE, sterol from soybean oil deodorizer distillate |
| CN106977582A (en) * | 2017-05-10 | 2017-07-25 | 福建省格兰尼生物工程股份有限公司 | A kind of method of Hydrolysis kinetics phytosterol in deodorization distillate |
Non-Patent Citations (1)
| Title |
|---|
| 肖勇生等: "脱臭馏出物中酶法合成脂肪酸甲酯及提取植物甾醇的研究", 《安徽农业科学》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112300238A (en) * | 2020-09-23 | 2021-02-02 | 福建福迩金生物科技有限公司 | Method for extracting phytosterol from soybeans |
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Application publication date: 20181116 |