CN101245359B - Method for producing alpha-linolenic acid subsection enzyme hydrolysis, molecular distillation from oil and fat enriched in linolenic acid - Google Patents
Method for producing alpha-linolenic acid subsection enzyme hydrolysis, molecular distillation from oil and fat enriched in linolenic acid Download PDFInfo
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- CN101245359B CN101245359B CN2008100493893A CN200810049389A CN101245359B CN 101245359 B CN101245359 B CN 101245359B CN 2008100493893 A CN2008100493893 A CN 2008100493893A CN 200810049389 A CN200810049389 A CN 200810049389A CN 101245359 B CN101245359 B CN 101245359B
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Abstract
The invention relates to a method for preparing Alpha-linolenic acid by graded enzyme hydrolysis and molecular distillation from linolenic acid-rich grease, which is characterized in that: the method comprises the following steps: (1) graded hydrolysis: a certain amount of water and lipozyme are added in the linolenic acid-rich grease to carry out the hydrolysis of the grease, then the materials undergo washing, and the hydrolysis and the washing processes are repeated; (2) drying: the obtained materials are dried and dewatered under certain pressure and temperature; (3) molecular distillation: the materials are distilled under certain temperature and pressure conditions, and the light phase is a product of the Alpha-linolenic acid. Compared with the prior art, the method has the advantages that: the linolenic acid-rich grease is firstly subject to one step of hydrolysis by the lipozyme, the most of the grease generates fatty acid by the hydrolysis, then the two step or three step hydrolysis is carried out to improve the hydrolysis degree of the grease. The process does not use acidic catalyst or alkaline catalyst, which can not produce the environmentally harmful waste acid waterand can improve the yield of the linolenic acid.
Description
Technical field
The present invention relates to the extracting method of alpha-linolenic acid, particularly a kind of from be rich in gamma-linolenic acid oil subsection enzyme hydrolysis, molecular distillation prepare the method for alpha-linolenic acid.
Background technology
Alpha-linolenic acid (Alpha-Linolenic Acid) is present in the green plants, is a kind of of N-3 system (being called ω-3 again) unsaturated fatty acids, and it is the necessary unsaturated fatty acids of human body.
Alpha-linolenic acid is of value to prevention and treatment coronary heart disease, diabetes, similar rheumatism, dermatitis disease, dysthymia disorders, psychotic disorder, dementia, allergy, asthma, ephrosis and chronic plug tuberculosis etc., in a single day human body lacks alpha-linolenic acid, promptly can cause the body lipid metabolism disorders, cause the generation of symptoms such as immunizing power reduces, forgetful, tired, visual deterioration, atherosclerosis.If especially infant, teenager lack alpha-linolenic acid, will have a strong impact on the normal development of its intelligence and eyesight.
Alpha-linolenic acid prolongs under the effect of enzyme at desaturase and carbochain after entering human body, and deriving in body metabolism is the precursor substance of EPA and DHA and prostaglandin(PG), has extensive physiologically active and obviously pharmacological action.
Alpha-linolenic acid extensively is present in occurring in nature, all contains a certain amount of linolenic acid in lower plant such as the leaf of animal milk, plant, root, stem and fruit, liverwort, fern and the planktonic organism, and wherein content is the highest in Semen Lini and the perillaseed, can reach more than 50%.But itself can not produce alpha-linolenic acid in the human body, can only from external source food, absorb.
Most of saponification, acidolysis, urea adduct method, silver ion complexation method, column chromatography, vacuum distillation method and the supercritical extraction method etc. of adopting of preparation method commonly used at present.
The patent of invention CN1219744C of Shanxi coal institute of the Chinese Academy of Sciences discloses to utilize and has been rich in the linolenic acid raw material, utilizes lipase-catalyzed esterification to produce ethyl linolenate, passes through supercritical extraction again, the method for purification of flax acetoacetic ester.
The patent CN1053010C of Beijing ten thousand rich secret service trade company application discloses and has utilized the linolenic acid raw material, produces linolenic method by saponification, acidolysis, urea clathrate method.
Cui of Anyang Chemical Idustry Group Co., Ltd. prepares linolenic acid for the patent CN1837179A of people such as people application utilizes perilla seed through squeezing, saponification, acidifying, urea complexation, freezing, extraction, molecular distillation.
Because fat hydrolysis is difficulty relatively, a hydrolysis can not make the grease complete hydrolysis, adopts the saponification acidolysis then can produce acid waste water and alkaline waste water, and therefore all there is weak point in above-mentioned these existing extractive techniques.
Summary of the invention
Purpose of the present invention is just at above-mentioned existing in prior technology problem, what provide is a kind of by being rich in the method that gamma-linolenic acid oil subsection enzyme hydrolysis, molecular distillation prepare alpha-linolenic acid, this method is utilized lipase segmentation catalytic hydrolysis reaction, can guarantee that not only grease fully obtains hydrolysis, and do not have spent acid, alkali waste water and produce, free from environmental pollution, the yield of alpha-linolenic acid has a more substantial increase.
The objective of the invention is to be achieved through the following technical solutions: the method that subsection enzyme hydrolysis, molecular distillation prepare alpha-linolenic acid from be rich in gamma-linolenic acid oil of the present invention may further comprise the steps:
(1) graded hydrolysis
In being rich in gamma-linolenic acid oil, add a certain amount of water and lipase, the weight ratio of grease and water is 1: 0.5-8.0, the add-on of lipase is the 0.5%-8% of grease weight, at temperature 20-85 ℃, reacted 2-10 hour, and made fat hydrolysis, the material that hydrolysis obtains is washed, material: water (volume ratio) is 1: 0.1-3, repeat above hydrolytic process 1-4 time;
(2) drying
The material that step (1) is obtained is under 0.02-0.06MPa, temperature 50-90 ℃ at pressure, drying and dehydrating;
(3) molecular distillation
The material of handling through step (2) distills under temperature 60-120 ℃, pressure 0.1-10Pa condition, gently is the product of alpha-linolenic acid mutually.
In the present invention, hydrolysis, water washing process preferably repeat 2-3 time; Described lipase can be any one in lipase Lipolase-100T, Lipolase-100L or the Candida lipolytica lipase, and the add-on of lipase is the 1%-5% of grease weight.
Temperature in step of the present invention (1) is preferably 30-60 ℃, water washing process, and the volume ratio of material and water is 1: 0.1-3.
Molecular distillation apparatus is selected single mode for use.
The described gamma-linolenic acid oil that is rich in is Purple Perilla Seed Oil, linseed oil or Oenothera oil.
The advantage that the present invention is compared with prior art possessed is: be at first to pass through lipase one-stage hydrolysis with being rich in gamma-linolenic acid oil, most of fat hydrolysis generates lipid acid, utilize lipase hydrolysed residual part grease once more then, improve greasy degree of hydrolysis, also can carry out for the third time, the 4th hydrolysis.This technology does not adopt acidity or basic catalyst, does not produce environmentally harmful spent acid, buck, but also has improved linolenic yield.
Embodiment
Example 1
A kind ofly extract linolenic method, comprise the steps: from Purple Perilla Seed Oil
(1) one-stage hydrolysis adds lipase Lipolase-100T in Purple Perilla Seed Oil, enzyme concn 1.0% (add-on that is lipase be grease weight 1%) adds the water of material equivalent, 55 ℃ of temperature of reaction, hydrolysis 6 hours.Record material acid value 110mgKOH/g.(this index is represented the fat hydrolysis degree, also is the indirect index of fatty acid content in the material).
(2) washing, in the material that obtains after handle (1) set by step, the adding volume ratio is 1: 0.3 a water, 85 ℃ of temperature, washing.
(3) two sections hydrolysis add lipase Lipolase-100L in the material that step (2) obtains, enzyme concn 1.0%, and the water of adding material equivalent, 55 ℃ of temperature of reaction in 6 hours reaction times, record material acid value 135mgKOH/g.
(4) washing after the material that obtains in (3) is set by step handled, adds volume ratio and is 1: 0.5 water, 85 ℃ of temperature, 30 minutes washing time.
(5) drying, the material that step (4) is obtained is under 0.02-0.06MPa, temperature 50-70 ℃ at pressure, drying and dehydrating.
(6) molecular distillation, the material through handle step (1), (2), (3), (4), (5) distills under 90 ℃ of temperature, pressure 2Pa condition, and gently mutually for containing linolenic product, heavy phase is returned step (1).
Example 2
A kind ofly extract linolenic method, comprise the steps: from Purple Perilla Seed Oil
(1) one-stage hydrolysis adds lipase Lipolase-100L in Purple Perilla Seed Oil, enzyme concn 2.0% (add-on that is lipase be grease weight 2%) adds the water of material equivalent, 55 ℃ of temperature of reaction, 4 hours reaction times.Record material acid value 106mgKOH/g.
(2) washing after the material that obtains in (1) is set by step handled, adds volume ratio and is 1: 0.4 water, 75 ℃ of temperature, washing.
(3) two sections hydrolysis add lipase Lipolase-100L in the material that step (2) obtains, enzyme concn 2.0%, the water of adding material equivalent, 55 ℃ of temperature of reaction, 6 hours reaction times.Record material acid value 139mgKOH/g.
(4) three sections hydrolysis
Add lipase Lipolase-100L in the material that in step (3), obtains, enzyme concn 3.0% (add-on that is lipase be grease weight 3%) adds the water of material equivalent, 55 ℃ of temperature of reaction, in 4 hours reaction times, record material acid value 160mgKOH/g.
(5) washing after the material that obtains in (1) (2) (3) (4) is set by step handled, adds volume ratio and is 1: 0.4 water, 75 ℃ of temperature, 30 minutes washing time.
(6) drying, the material that step (5) is obtained is under 0.02-0.06MPa, temperature 50-70 ℃ at pressure, drying and dehydrating.
(7) molecular distillation, the material through above-mentioned steps is handled distills for the first time under temperature (80-120 ℃), pressure (0.1-10Pa) condition, and gently mutually for being rich in linolenic product, heavy phase is returned step (1).
Example 3
A kind ofly extract linolenic method, comprise the steps: from linseed oil
(1) one-stage hydrolysis adds lipase Lipolase-100T in linseed oil, enzyme concn 4.0% (add-on that is lipase be grease weight 4%) adds the water of material equivalent, 55 ℃ of temperature of reaction, hydrolysis 6 hours.Record material acid value 97mgKOH/g.
(2) washing after the material that obtains in (1) is set by step handled, adds volume ratio and is 1: 0.5 water, 85 ℃ of temperature, washing.
(3) two sections hydrolysis add lipase Lipolase-100L in the material that step (2) obtains, enzyme concn 2.0%, the water of adding material equivalent, 55 ℃ of temperature of reaction, 6 hours reaction times.Record material acid value 134mgKOH/g.
(4) washing after the material that obtains in (3) is set by step handled, adds volume ratio and is 1: 0.6 water, 75 ℃ of temperature, 30 minutes washing time.
(4) three sections hydrolysis,
Add lipase Lipolase-100L in the material that in step (3), obtains, enzyme concn 2.0%, the water of adding material equivalent, 55 ℃ of temperature of reaction, hydrolysis 4 hours records material acid value 161mgKOH/g.
(5) washing after the material that obtains in (1) (2) (3) (4) is set by step handled, adds volume ratio and is 1: 0.6 water, 75 ℃ of temperature, 30 minutes washing time.
(6) drying, the material that step (5) is obtained is under 0.02-0.06MPa, temperature 50-70 ℃ at pressure, drying and dehydrating.
(7) molecular distillation, the material through above-mentioned steps is handled distills for the first time under temperature (80-120 ℃), pressure (0.1-10Pa) condition, and gently mutually for being rich in linolenic product, heavy phase is returned step (1).
Example 4
A kind ofly extract linolenic method, comprise the steps: from linseed oil
(1) one-stage hydrolysis adds Candida lipolytica lipase in linseed oil, enzyme concn 5.0% (add-on that is lipase be grease weight 5%) adds the water of material equivalent, 55 ℃ of temperature of reaction, 6 hours reaction times, hydrolysis.Record material acid value 108mgKOH/g.
(2) washing after the material that obtains in (1) is set by step handled, adds volume ratio and is 1: 0.5 water, 65 ℃ of temperature, 30 minutes washing time.
(3) two sections hydrolysis add lipase Lipolase-100L in the material that step (2) obtains, enzyme concn 3.0%, the water of adding material equivalent, 55 ℃ of temperature of reaction, 6 hours reaction times.Record material acid value 135mgKOH.
(4) washing after the material that obtains in (3) is set by step handled, adds volume ratio and is 1: 0.5 water, 65 ℃ of temperature, 30 minutes washing time.
(5) drying, the material that step (4) is obtained is under 0.02-0.06MPa, temperature 50-70 ℃ at pressure, drying and dehydrating.
(6) molecular distillation, the material through handle step (1), (2), (3), (4), (5) distills for the first time under temperature (80-120 ℃), pressure (0.1-10Pa) condition, and gently mutually for being rich in linolenic product, heavy phase is returned step (1).
Example 5
A kind ofly extract linolenic method, comprise the steps: from Oenothera oil
(1) one-stage hydrolysis adds lipase Lipolase-100L in Oenothera oil, enzyme concn 4.0%, the water of adding material equivalent, 45 ℃ of temperature of reaction, 6 hours reaction times.Record material acid value 103mgKOH/g
(2) washing after the material that obtains in (1) is set by step handled, adds volume ratio and is 1: 0.3 water, 85 ℃ of temperature, 30 minutes washing time.
(3) two sections hydrolysis add lipase Lipolase-100L in the material that step (2) obtains, enzyme concn 4.0%, the water of adding material equivalent, 45 ℃ of temperature of reaction, 6 hours reaction times.Record material acid value 136mgKOH/g.
(4) washing after the material that obtains in (3) is set by step handled, adds volume ratio and is 1: 0.5 water, 75 ℃ of temperature, 30 minutes washing time.
(5) drying, the material that step (4) is obtained is under 0.02-0.06MPa, temperature 50-70 ℃ at pressure, drying and dehydrating.
(6) molecular distillation, the material through handle step (1), (2), (3), (4), (5) distills for the first time under temperature (80-120 ℃), pressure (0.1-10Pa) condition, and gently mutually for being rich in linolenic product, heavy phase is returned step (1).
Claims (5)
1. a subsection enzyme hydrolysis from be rich in gamma-linolenic acid oil, molecular distillation prepare the method for alpha-linolenic acid, and it is characterized in that: it may further comprise the steps:
(1) graded hydrolysis
In being rich in gamma-linolenic acid oil, add a certain amount of water and lipase, described lipase is Lipolase-100T or Lipolase-100L, the add-on of lipase is the 1%-5% of grease weight, the water that adds material equivalent, at temperature 45-55 ℃, reacted 2-10 hour, make fat hydrolysis, the material that hydrolysis obtains is washed, and the hydrolysis water washing process repeats 1-4 time;
(2) drying
The material that step (1) is obtained under pressure 0.02-0.06MPa, temperature 50-90 ℃, drying and dehydrating;
(3) molecular distillation
The material of handling through step (2) distills under temperature 60-120 ℃, pressure 0.1-10Pa condition, gently is the product of alpha-linolenic acid mutually.
2. the method for preparing alpha-linolenic acid according to claim 1 is characterized in that: the hydrolysis in the step (1), water washing process repeat 2-3 time.
3. the method for preparing alpha-linolenic acid according to claim 1 is characterized in that: in the water washing process of step (1), the volume ratio of material and water is 1: 0.1-3.
4. the method for preparing alpha-linolenic acid according to claim 1, it is characterized in that: molecular distillation apparatus is selected single mode for use.
5. the method for preparing alpha-linolenic acid according to claim 1 is characterized in that: the described gamma-linolenic acid oil that is rich in is Purple Perilla Seed Oil, linseed oil or Oenothera oil.
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| 许松林等.短程蒸馏提纯胡麻籽油中α-亚麻酸的工艺研究.中草药.2004,35(3), * |
| 魏决等.酶法从紫苏子油中制取α-亚麻酸工艺研究——脂肪酶水解工艺的探讨.食品科学.2005,26(1), * |
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Assignee: State Grain Reserve Wuhan Scientific Research and Design Institute Assignor: Henan Industry University Contract record no.: 2011420000067 Denomination of invention: Method for producing alpha-linolenic acid subsection enzyme hydrolysis, molecular distillation from oil and fat enriched in linolenic acid Granted publication date: 20110316 License type: Exclusive License Open date: 20080820 Record date: 20110510 |
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