CN103694300A - Method for extracting oryzanol from waste bran meal grease - Google Patents
Method for extracting oryzanol from waste bran meal grease Download PDFInfo
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- CN103694300A CN103694300A CN201310659297.8A CN201310659297A CN103694300A CN 103694300 A CN103694300 A CN 103694300A CN 201310659297 A CN201310659297 A CN 201310659297A CN 103694300 A CN103694300 A CN 103694300A
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Abstract
The invention provides a method for extracting oryzanol from waste bran meal grease. The method comprises the following steps of: 1) adding a high temperature resistant enzyme to the waste bran meal grease, wherein the added high temperature resistant enzyme is 0.5 to 5% the mass of the waste bean meal grease; agitating to digest for 60 to 120min under a temperature of 70 to 95 DEG C; and filtering to obtain clear grease; 2) alkali dissolution, namely, mixing an alkaline methanol solution and the clear grease obtained in step 1) based on the mass ratio of (1: 5)-(1: 8); heating to reach 60 DEG C; agitating; standing until two phases are separated; and extracting; 3) acidification: heating the extract liquor obtained in step 2) to 40 to 60 DEG C; adding acid to regulate the pH (Power of Hydrogen) to be 3.0 to 6.0; standing overnight; and centrifugally separating to obtain a coarse oryzanol product; and 4) refining oryzanol, namely, flushing the coarse oryzanol product obtained in step 3) with distilled water; and then drying to obtain the refined oryzanol. With the adoption of the method, the technical process is greatly reduced and simplified, and the yield of oryzanol is also greatly increased.
Description
Technical field
The present invention relates to extract in rice bran waste grease the method for thiaminogen.
Background technology
In recent years; along with the demand of people to healthy living; the effect of thiaminogen causes extensive concern, and thiaminogen is as a kind of newer medicine, and known pharmacological action at present mainly contains regulating plant nerve; promote growth of animal; adjusting improves functions of intestines and stomach, stops autologous synthetic cholesterol and reduces serum cholesterol, promotes skin capillary blood vessel circulating function; protection skin, has weak class sex hormone function.Due to the essentially no side effect of thiaminogen, thereby be subject to the favor of clinical medicine.In addition thiaminogen, also for makeup, has significant curative effect to face's exfoliation eczema, freckle etc.Also be used as foodstuff additive, to resist the absorption of cholesterol, prevent lipid oxidation etc.Thereby market constantly increases the demand of thiaminogen.
In the refining of Rice pollard oil, produce a large amount of waste greases, in the past, they are often used as extraction croude fatty acids, then, in fact, in these waste greases, contain thiaminogen.Along with the recycling to waste grease, from rice bran waste grease, extract the concern that thiaminogen causes people.
Present method is utilized the character of thiaminogen different pH state different solubilities in polar solvent, has simplified the complicated technologies such as alkali refining, saponification, adopts methyl alcohol directly to extract, and obtains higher thiaminogen yield.
Summary of the invention
The technical problem to be solved in the present invention is the method for thiaminogen of extracting from rice bran waste grease, makes a large amount of waste grease in Rice pollard oil refinement obtain higher value application.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
A method of extracting thiaminogen from chaff dregs of rice waste grease, comprises the following steps:
1) in chaff dregs of rice waste grease, add high temperature resistant enzyme, add-on is the 0.5-5% of chaff dregs of rice waste grease quality, stirs digestion 60-120min at 70-95 ℃, filters, and obtains grease clear liquid;
2) alkali is molten: by alkaline methanol solution and step 1) grease clear liquid in mass ratio routine 1:5 ~ 1:8 mix, heat to 60 ℃, stir, standingly treat that two are separated, extraction;
3) acid out: by step 2) extraction liquid is heated to 40-60 ℃, and adding acid to be adjusted to pH is 3.0-6.0, standing over night, and centrifugation, obtains thiaminogen crude product;
4) refining thiaminogen: the thiaminogen crude product that step 3) is obtained, with distilled water, rinse, then dry, obtain refining thiaminogen.
Described in step 1), high temperature resistant enzyme is α-amylase.
Step 2) collocation method of described alkaline methanol solution is: methyl alcohol is mixed with water, and being configured to volumetric concentration is the methanol solution between 65%-85%, and it is 11 ~ 13 that NaOH regulates pH.
Described in step 3), acid is hydrochloric acid.
Step 2) in, preparing alkaline methanol, to carry out alkali molten be the key of this technique, alkaline methanol can dissolve thiaminogen sodium salt and fatty acid soaps, and does not dissolve the unsaponifiables such as chaff wax, fatty alcohol, sterol, thereby can make thiaminogen sodium salt separated with unsaponifiables with thick substances.Therefore, the molten yield that is directly connected to thiaminogen of alkali.The principal element that affects the molten effect of alkali has the concentration of extraction agent methyl alcohol, the molten pH of the consumption of methyl alcohol and alkali.We have been determined by experiment optimal conditions, and the concentration of methyl alcohol and water configuration is between 65%-85%, and the pH of adjusting is between 11-14, and the ratio of mixing with grease clear liquid is between 1:5 ~ 1:8.
In step 3), acid out is to utilize weak organic acid to decompose thiaminogen sodium salt, reduction thiaminogen, and isolate from methanol solution middle reaches.Thereby the quality of acid out, can have a strong impact on the quality of thiaminogen.Extraction liquid main component has methyl alcohol, water, thiaminogen sodium salt, fatty acid sodium salt etc.If extraction liquid is hot solution state, carry out acid out, thiaminogen and lipid acid can be separated out simultaneously, have comprised lipid acid crystal in thiaminogen crystal, to aftertreatment, bring very large difficulty, will have a strong impact on the quality of thiaminogen.In order to address this problem, present method adopts extraction liquid is heated to 40-60 ℃, adds acid to be adjusted to certain pH value, standing over night, and centrifugation obtains thiaminogen crude product.Wherein, we are heated to extraction liquid between 40-60 ℃, to add acid for adjusting pH between 3.0-6.0.
In step 4), the thiaminogen crude product obtaining, rinses with distilled water, then carries out hollow and is dried, and obtains refining thiaminogen.
Beneficial effect: the present invention extracts thiaminogen from the chaff dregs of rice, adopt alkaline methanol extraction process to extract thiaminogen, the techniques such as oil alkali refining and saponification have been replaced, thereby avoided the loss of thiaminogen in oil alkali refining and saponification, greatly shorten, simplified technical process, also greatly improved thiaminogen yield.
Embodiment
According to following embodiment, can better understand the present invention.Yet, those skilled in the art will readily understand, the described concrete material proportion of embodiment, processing condition and result thereof be only for the present invention is described, and should also can not limit the present invention described in detail in claims.
Embodiment 1
Get rice bran waste grease 5kg, add amylase 2 5g, be heated to 70 ℃, digestion time 60min, with strainer, filter, obtaining grease 1.2kg, is 1.52% with measurement of ultraviolet-visible spectrophotometer containing thiaminogen, gets 65% methanol solution, with NaOH, regulate pH to 11, get 240g alkaline methanol and mix with grease, heat to 60 ℃ and fully stir, after standing for some time, two are separated.Extraction liquid is heated to 40 ℃, with acid, adjusts pH to 3.0, standingly treat that thiaminogen separates out, filter and obtain thiaminogen, through washing and drying, obtain thiaminogen 11.36g, the yield of thiaminogen is 62.28%.
Embodiment 2
Get rice bran waste grease 5kg, add amylase 150g, be heated to 80 ℃, digestion time 80min, with strainer, filter, obtaining grease 1.29kg, is 1.46% with measurement of ultraviolet-visible spectrophotometer containing thiaminogen, gets 75% methanol solution, with NaOH, regulate pH to 12, get 200g alkaline methanol and mix with grease, heat and fully stir, after standing for some time, two are separated.Extraction liquid is heated to 50 ℃, with acid, adjusts pH to 4.5, standingly treat that thiaminogen separates out, with filtration, obtain thiaminogen, through washing and drying, obtain thiaminogen 11.53g, the yield of thiaminogen is 61.23%.
Embodiment 3
Get rice bran waste grease 5kg, add amylase 2 50g, be heated to 95 ℃, digestion time 120min, with strainer, filter, obtaining grease 1.24kg, is 1.53% with measurement of ultraviolet-visible spectrophotometer containing thiaminogen, gets 85% methanol solution, with NaOH, regulate pH to 13, get 155g alkaline methanol and mix with grease, heat and fully stir, after standing for some time, two are separated.Extraction liquid is heated to 60 ℃, with acid, adjusts pH to 6.0, standingly treat that thiaminogen separates out, with filtration, obtain thiaminogen, through washing and drying, obtain thiaminogen 11.41g, the yield of thiaminogen is 60.15%.
Claims (4)
1. from chaff dregs of rice waste grease, extract a method for thiaminogen, it is characterized in that it comprises the following steps:
1) in chaff dregs of rice waste grease, add high temperature resistant enzyme, add-on is the 0.5-5% of chaff dregs of rice waste grease quality, stirs digestion 60-120min at 70-95 ℃, filters, and obtains grease clear liquid;
2) alkali is molten: by alkaline methanol solution and step 1) grease clear liquid in mass ratio routine 1:5 ~ 1:8 mix, heat to 60 ℃, stir, standingly treat that two are separated, extraction;
3) acid out: by step 2) extraction liquid is heated to 40-60 ℃, and adding acid to be adjusted to pH is 3.0-6.0, standing over night, and centrifugation, obtains thiaminogen crude product;
4) refining thiaminogen: the thiaminogen crude product that step 3) is obtained, with distilled water, rinse, then dry, obtain refining thiaminogen.
2. the method for extracting thiaminogen from chaff dregs of rice waste grease according to claim 1, is characterized in that: described in step 1), high temperature resistant enzyme is α-amylase.
3. the method for extracting thiaminogen from chaff dregs of rice waste grease according to claim 1, it is characterized in that: step 2) collocation method of described alkaline methanol solution is: methyl alcohol mixed with water, being configured to concentration is the methanol solution between 65%-85%, and it is 11 ~ 13 that NaOH regulates pH.
4. the method for extracting thiaminogen from chaff dregs of rice waste grease according to claim 1, is characterized in that: described in step 3), acid is hydrochloric acid.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310659297.8A CN103694300B (en) | 2013-12-10 | 2013-12-10 | A kind of method extracting thiaminogen from chaff dregs of rice waste grease |
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| CN201310659297.8A CN103694300B (en) | 2013-12-10 | 2013-12-10 | A kind of method extracting thiaminogen from chaff dregs of rice waste grease |
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| CN103694300A true CN103694300A (en) | 2014-04-02 |
| CN103694300B CN103694300B (en) | 2015-09-30 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5869708A (en) * | 1997-01-17 | 1999-02-09 | Das; Prashanta Kumar | Process for the isolation of oryzanols from crude dark acid oil (rice bran) |
| CN1485330A (en) * | 2002-09-27 | 2004-03-31 | 杜长安 | Solvent extraction process of oryzanol |
| US20040192948A1 (en) * | 2003-03-27 | 2004-09-30 | Council Of Scientific And Industrial Research | Process for the production of oryzanol enriched fraction from rice bran oil soapstock |
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2013
- 2013-12-10 CN CN201310659297.8A patent/CN103694300B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5869708A (en) * | 1997-01-17 | 1999-02-09 | Das; Prashanta Kumar | Process for the isolation of oryzanols from crude dark acid oil (rice bran) |
| CN1485330A (en) * | 2002-09-27 | 2004-03-31 | 杜长安 | Solvent extraction process of oryzanol |
| US20040192948A1 (en) * | 2003-03-27 | 2004-09-30 | Council Of Scientific And Industrial Research | Process for the production of oryzanol enriched fraction from rice bran oil soapstock |
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| CN103694300B (en) | 2015-09-30 |
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