CN108485793A - A kind of preparation method of high-stability D HA algae oils - Google Patents
A kind of preparation method of high-stability D HA algae oils Download PDFInfo
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- CN108485793A CN108485793A CN201810278850.6A CN201810278850A CN108485793A CN 108485793 A CN108485793 A CN 108485793A CN 201810278850 A CN201810278850 A CN 201810278850A CN 108485793 A CN108485793 A CN 108485793A
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- green kernel
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Classifications
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
- A23D9/007—Other edible oils or fats, e.g. shortenings, cooking oils characterised by ingredients other than fatty acid triglycerides
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
- A23D9/02—Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
- A23D9/04—Working-up
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/025—Pretreatment by enzymes or microorganisms, living or dead
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
Abstract
The present invention provides a kind of preparation methods of high-stability D HA algae oils, include the following steps：(1) green kernel will be obtained after the shell removal of green fruit, is crushed after epidermis is removed and obtains green kernel powder；(2) green kernel powder is added in distilled water, constant temperature 1 hour at 55 DEG C, continues constant temperature 2 hours after papain is added, centrifuged after boiling sterilization, freeze-drying obtains green kernel extract after adjusting pH；(3) by aubergine pigment enzyme deactivation, rinsed clean after taking-up crushes after drying and obtains aubergine pigment powder；(4) aubergine pigment powder is added in ammonium oxalate solution, is filtered after constant temperature extraction, centrifuged after filtrate decoloration, alcohol precipitation is precipitated after concentration, is dried after washing and is obtained eggplant bark extract；(5) DHA algal oil, green kernel extract, eggplant bark extract are added in material-compound tank, insulated and stirred 2 hours stands, filters out foam, drying.The oxidation-stabilized performance of DHA algal oil produced by the present invention is fine, and service life is longer.
Description
Technical field
The present invention relates to a kind of DHA algal oils, more particularly to a kind of preparation method of high-stability D HA algae oils.
Background technology
DHA, docosahexaenoic acid are commonly called as docosapentaenoic acid, are a kind of to the very important polyunsaturated fatty acid of human body, belong to
Important member in Omega-3 unsaturated fatty acids family.DHA is a kind of main member of nervous system cell growth and maintenance
Element is the important composition aliphatic acid of brain and retina, and content is up to 20% in human brain cortex, in eye retina
Proportion is maximum, accounts for about 50%, most important to infant intelligence and visual acuity, in addition, DHA also has preferable drop blood
Fat, improves the effects that immunity at norcholesterol.DHA algal oil extracts from marine microalgae, and the transmission without food chain is more pacified relatively
Entirely, EPA content is very low.
Disclose " a kind of non-solvent high-purity DHA algal oil application No. is the Chinese invention of CN201410099686.4
Preparation method ", the first pre-processing by the feedstock oil containing 30~65wt%DHA Jing Guo depickling, degumming, drying；After again will be dry
DHA algal oil heating be molten into homogeneous phase, then cool down, after 2~8h of growing the grain, plate compression filtering, gained filter liquid state oil
For room temperature oil, solid oil is collected；Then heating is carried out to room temperature oil and is molten into homogeneous phase, then cooled down, 2~12h of growing the grain
Afterwards, plate compression filters, and the filter liquid state oil of gained is low-temperature oil；Finally, the 1~10wt% for accounting for oily weight is added in low-temperature oil
The solid oil of two steps filtering gained carries out heating and is molten into homogeneous phase together, then cools down, after growing the grain 6~for 24 hours, plate compression mistake
The filter liquid state oil of filter, gained is winterized oil, and DHA content is purified to 70~90g/ by 30~65g/100g of feedstock oil at this time
100g.The invention the problem is that：The oxidation stability of its DHA algal oil being prepared is bad, is easy rancid rotten, influence
Its service life.
Invention content
The technical problem to be solved in the present invention is to provide a kind of preparation method of high-stability D HA algae oils, this method is made
DHA algal oil oxidation-stabilized performance it is fine, service life is longer.
In order to solve the above technical problems, the technical scheme is that：
A kind of preparation method of high-stability D HA algae oils, includes the following steps：
(1) green kernel will be obtained after the shell removal of green fruit, pulverizer will be put into after the epidermis removal of green kernel
In, green kernel powder is obtained after crushing；
(2) the green kernel powder obtained step (1) is added in distilled water, adjusts after pH value is 6 that constant temperature 1 is small at 55 DEG C
When, continue constant temperature 2 hours after papain is added, boiling sterilization centrifuged obtained mixing slurry after 15 minutes, will be upper
It is spare to obtain green kernel extract for freeze-drying after layer oil reservoir extracts；
(3) enzyme deactivation 20 minutes in boiling water are added in aubergine pigment, rinsed clean after taking-up is put into after drying in pulverizer, powder
Aubergine pigment powder is obtained after broken；
(4) the aubergine pigment powder for obtaining step (3) is added in ammonium oxalate solution, will after constant temperature extracts 2.5 hours at 75 DEG C
Obtained mixed liquor filters, and is centrifugally separating to obtain supernatant after obtained filtrate is decolourized, alcohol precipitation after supernatant concentration is obtained
Precipitation dries after washing precipitation absolute ethyl alcohol repeatedly and obtains eggplant bark extract；
(5) the eggplant bark extract that green kernel extract that DHA algal oil, step (2) obtain, step (4) obtain is added
Enter in material-compound tank, insulated and stirred 1 hour after being heated to 55 DEG C, stands to foam heat preservation after floating and filter out foam, obtained after drying
High-stability D HA algae oils.
Further, in step (1) of the present invention, the grain size of green kernel powder is 50 mesh.
Further, in step (2) of the present invention, the weight ratio of green kernel powder and distilled water is 1:6.
Further, in step (2) of the present invention, the weight ratio of papain and green kernel powder is 1:500.
Further, in step (2) of the present invention, the temperature of freeze-drying is -25 DEG C.
Further, in step (3) of the present invention, the grain size of aubergine pigment powder is 60 mesh.
Further, in step (4) of the present invention, the mass concentration of ammonium oxalate solution is 2%.
Further, in step (4) of the present invention, the weight ratio of aubergine pigment powder and ammonium oxalate solution is 1:27.
Further, in step (5) of the present invention, green kernel extract, step that DHA algal oil, step (2) obtain
(4) weight ratio of the eggplant bark extract obtained is (80-90):(5-10):(1-2), and green kernel extract, aubergine pigment carry
It is 5 to take the weight ratio of object:1.
Further, in step (5) of the present invention, the speed of insulated and stirred is 500rpm.
Compared with prior art, the invention has the advantages that：
1) green fruit (Carya illinoensis (Wangh.) koch) is called Longevity, and the present invention removes its shell
Green kernel is obtained, then green kernel powder is obtained by being crushed after the epidermis removal on green kernel, then by aqueous enzymatic method to green
Root kernel powder extracts to obtain green kernel extract, containing a large amount of unsaturated fatty acids, has reducing blood lipid, the work of norcholesterol
Property, synergy can be generated with DHA algal oil, to further increase reducing blood lipid, the norcholesterol performance of the present invention.
2) aubergine pigment is the skin portion of daily vegetables eggplant, and the present invention will crush after its enzyme deactivation and obtain aubergine pigment powder, then
Aubergine pigment powder is extracted to obtain eggplant bark extract using ammonium oxalate method, containing a large amount of pectin, has reducing blood lipid, drop courage solid
Alcohol acts on, and can generate synergy with DHA algal oil and Bi Gen kernel extracts, to further increase the present invention reducing blood lipid,
Norcholesterol performance, in addition, eggplant bark extract also have the function of remove halitosis, therefore can effectively improve the present invention remove halitosis
Performance.
3) green kernel extract and eggplant bark extract all have stronger antioxidant activity, and when the weight ratio of the two
It is 5:Best collaboration antioxidant effect can be generated when 1, to play preferable anti-oxidant stabilization to DHA algal oil, effectively
Delay its rancid metamorphic process, prolongs the service life.
Specific implementation mode
Below in conjunction with specific embodiment, the present invention will be described in detail, herein illustrative embodiments and their description of the invention
For explaining the present invention, but it is not as a limitation of the invention.
Embodiment 1
The preparation method of high-stability D HA algae oils, includes the following steps：
(1) green kernel will be obtained after the shell removal of green fruit, pulverizer will be put into after the epidermis removal of green kernel
In, it is green kernel powder of 50 purposes that grain size is obtained after crushing；
(2) green kernel powder for obtaining step (1) is added in distilled water, and the weight ratio of green kernel powder and distilled water is
1:6, adjust after pH value is 6 constant temperature 1 hour at 55 DEG C, continue constant temperature 2 hours after papain is added, papain with it is green
The weight ratio of root kernel powder is 1:500, boiling sterilization centrifuged obtained mixing slurry after 15 minutes, and upper layer oil reservoir is extracted
To obtain green kernel extract spare for freeze-drying at -25 DEG C after out；
(3) enzyme deactivation 20 minutes in boiling water are added in aubergine pigment, rinsed clean after taking-up is put into after drying in pulverizer, powder
The aubergine pigment powder that grain size is 60 mesh is obtained after broken；
(4) the aubergine pigment powder obtained step (3) is added in the ammonium oxalate solution that mass concentration is 2%, aubergine pigment powder with
The weight ratio of ammonium oxalate solution is 1:Obtained mixed liquor is filtered after constant temperature extracts 2.5 hours at 27,75 DEG C, the filter that will be obtained
It is centrifugally separating to obtain supernatant after liquid decoloration, alcohol precipitation after supernatant concentration is precipitated, precipitation is washed repeatedly with absolute ethyl alcohol
Drying obtains eggplant bark extract after washing；
(5) it is 85 by weight ratio:7.5:Green kernel extract that 1.5 DHA algal oil, step (2) obtain, step (4)
Obtained eggplant bark extract is added in material-compound tank, insulated and stirred 1 hour under 500rpm speed after being heated to 55 DEG C, stands to bubble
Heat preservation filters out foam after foam floats, and high-stability D HA algae oils are obtained after drying.
Embodiment 2
As different from Example 1, in step (5), green kernel extract, step that DHA algal oil, step (2) obtain
(3) weight ratio of the eggplant bark extract obtained is 80:10:2.
Embodiment 3
As different from Example 1, in step (5), green kernel extract, step that DHA algal oil, step (2) obtain
(3) weight ratio of the eggplant bark extract obtained is 90:5:1.
Embodiment 4
As different from Example 1, in step (5), green kernel extract, step that DHA algal oil, step (2) obtain
(3) weight ratio of the eggplant bark extract obtained is 84:6:1.2.
Comparative Examples 1
Do not include green kernel extract in component, other components and preparation method are same as Example 1.
Comparative Examples 2
Do not include eggplant bark extract in component, other components and preparation method are same as Example 1.
Comparative Examples 3
In step (5), aubergine pigment extraction that green kernel extract that DHA algal oil, step (2) obtain, step (3) obtain
The weight ratio of object is 80:9:2, i.e. green kernel extract, eggplant bark extract weight ratio be 4.5:1, other components and
Preparation method is same as Example 1.
Comparative Examples 4
In step (5), aubergine pigment extraction that green kernel extract that DHA algal oil, step (2) obtain, step (3) obtain
The weight ratio of object is 80:9.9:1.8, i.e. green kernel extract, eggplant bark extract weight ratio be 5.5:1, other components
And preparation method is same as Example 1.
Comparative Examples 5
In step (5), the temperature of insulated and stirred is 50 DEG C, and other components and preparation method are same as Example 1.
Comparative Examples 6
In step (5), the temperature of insulated and stirred is 60 DEG C, and other components and preparation method are same as Example 1.
Comparative Examples 7
In step (5), the time of insulated and stirred is 50 minutes, and other components and preparation method are same as Example 1.
Comparative Examples 8
In step (5), the temperature of insulated and stirred is 70 minutes, and other components and preparation method are same as Example 1.
Comparative example
Comparative example is the embodiment 1 of the Chinese patent application No. is CN201410099686.4.
Experimental example one：Reducing blood lipid, norcholesterol performance test
Test method is：Choose 61 adults, 12 hours serum total cholesterol TC ＞ 5.72mmolL on an empty stomach-1Hyperlipemia
Disease patient, three times, each 6g observes the clinical efficacy of patient to edible algae oil after 6 weeks daily：(1) effective：The TC range of decrease >=20%；
(2) effectively：The TC ranges of decrease are 10-20%；(3) invalid：The TC ranges of decrease are less than 10%.Reducing blood lipid effective percentage is calculated, reducing blood lipid is effective
Patient's number/patient populations × 100% of rate=(effective+effective), test result are as shown in table 1：
| Reducing blood lipid effective percentage (%) | |
| Embodiment 1 | 91.2 |
| Embodiment 2 | 91.0 |
| Embodiment 3 | 90.7 |
| Embodiment 4 | 90.9 |
| Comparative Examples 1 | 78.7 |
| Comparative Examples 2 | 79.5 |
| Comparative Examples 3 | 91.1 |
| Comparative Examples 4 | 90.8 |
| Comparative example | 75.4 |
Table 1
As seen from Table 1, the reducing blood lipid effective percentage of 1-4 of the embodiment of the present invention shows the present invention obviously higher than comparative example
With preferable reducing blood lipid, norcholesterol performance, the wherein reducing blood lipid of embodiment 1, norcholesterol performance is best.Comparative Examples
The constituent part or component ratio of 1-4 is different from embodiment 1, wherein the reducing blood lipid effective percentage of Comparative Examples 1,2 under
Drop, reducing blood lipid, norcholesterol performance can be effectively improved by illustrating green kernel extract and eggplant bark extract；Comparative Examples
3,4 reducing blood lipid effective percentage and embodiment 1-4 maintain an equal level, and illustrate the weight ratio of green kernel extract, eggplant bark extract to drop
Blood fat, norcholesterol performance do not influence substantially.
Experimental example two：Except halitosis performance test
Test method is：61 mouth source property halitosis patients are chosen, twice, each 6g is observed edible algae oil after 10 days daily
The clinical efficacy of patient：(1) effective：Substantially there is no halitosis；(2) effectively：There is slight halitosis；(3) invalid：Halitosis symptom is not bright
It is aobvious to improve.Patient's number/patient populations × 100% that halitosis effective percentage=(effective+effective) is removed except halitosis is efficient is calculated,
Test result is as shown in table 2：
Table 2
As seen from Table 2, the halitosis effective percentage that removes of 1-4 of the embodiment of the present invention is far above comparative example, shows tool of the present invention
Have preferably remove halitosis performance, wherein embodiment 1 except halitosis performance it is best.The constituent part or component of Comparative Examples 1-4
Ratio is different from embodiment 1, and wherein Comparative Examples 2 decline a lot except halitosis effective percentage, and Comparative Examples 3 have except halitosis
Efficiency rises a bit, and having dropped a little except halitosis effective percentage for Comparative Examples 4 illustrates that eggplant bark extract is to greatly improve
Except the key factor of halitosis performance；The halitosis effective percentage that removes of Comparative Examples 1 maintains an equal level with embodiment 1-4, illustrates that green kernel carries
Object is taken not influenced on removing halitosis performance substantially.
Experimental example three：Oxidation-stabilized performance test
Test method is：Algae oil is placed in 60 DEG C of constant temperature ovens and forces oxidation, after stirring in 24 hours 1 time, 12 days
It takes out, before climbing T, T=(TBA- forces TBA before oxidation after pressure oxidation)/the pressure oxidation for calculating malonaldehyde value TBA
TBA × 100%, T are smaller to show that oxidation stability is better, and test result is as shown in table 3：
Table 3
As seen from Table 3, the T of 1-4 of the embodiment of the present invention is significantly lower than comparative example, shows that the present invention has preferable oxygen
Change stability, the oxidation-stabilized performance of wherein embodiment 1 is best.The constituent part or component ratio of Comparative Examples 1-4 with
Embodiment 1 is different, and the T of wherein Comparative Examples 1,2 rises, and illustrates green kernel extract and eggplant bark extract
Oxidation-stabilized performance can be effectively improved；The ascensional range of the T of Comparative Examples 3,4 is smaller, illustrates to extract when green kernel
The weight ratio of object and eggplant bark extract is 4.5:1 and 5.5:Oxidation-stabilized performance when 1 is slightly worse than green kernel extract
Weight ratio with eggplant bark extract is 5:Oxidation-stabilized performance when 1；The ascensional range of the T of Comparative Examples 5,6 is also smaller,
Illustrate that the extremes of temperature of insulated and stirred can reduce oxidation-stabilized performance；The ascensional range of the T of Comparative Examples 7,8 also compared with
Small, oxidation-stabilized performance can be reduced by illustrating that the overlong time of insulated and stirred is too short.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology can all carry out modifications and changes to above-described embodiment without violating the spirit and scope of the present invention.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should by the present invention claim be covered.
Claims (10)
1. a kind of preparation method of high-stability D HA algae oils, it is characterised in that：Include the following steps：
(1) green kernel will be obtained after the shell removal of green fruit, will be put into pulverizer after the epidermis removal of green kernel, powder
Green kernel powder is obtained after broken；
(2) the green kernel powder obtained step (1) is added in distilled water, adjusts after pH value is 6 constant temperature 1 hour at 55 DEG C, adds
Continue constant temperature 2 hours after entering papain, boiling sterilization centrifuged obtained mixing slurry after 15 minutes, by upper layer oil reservoir
It is spare to obtain green kernel extract for freeze-drying after extracting；
(3) enzyme deactivation 20 minutes in boiling water are added in aubergine pigment, rinsed clean after taking-up is put into pulverizer after drying, after crushing
Obtain aubergine pigment powder；
(4) the aubergine pigment powder for obtaining step (3) is added in ammonium oxalate solution, and constant temperature will obtain after extracting 2.5 hours at 75 DEG C
Mixed liquor filter, will obtained filtrate decoloration after be centrifugally separating to obtain supernatant, alcohol precipitation after supernatant concentration is precipitated,
It is spare to obtain eggplant bark extract for drying after precipitation absolute ethyl alcohol is washed repeatedly；
(5) the eggplant bark extract addition that green kernel extract that DHA algal oil, step (2) obtain, step (4) obtain is matched
In batch can, insulated and stirred 1 hour after being heated to 55 DEG C stands to foam heat preservation after floating and filters out foam, is obtained after drying high steady
Qualitative DHA algal oil.
2. a kind of preparation method of high-stability D HA algae oils according to claim 1, it is characterised in that：The step (1)
In, the grain size of green kernel powder is 50 mesh.
3. a kind of preparation method of high-stability D HA algae oils according to claim 2, it is characterised in that：The step (2)
In, the weight ratio of green kernel powder and distilled water is 1:6.
4. a kind of preparation method of high-stability D HA algae oils according to claim 3, it is characterised in that：The step (2)
In, the weight ratio of papain and green kernel powder is 1:500.
5. a kind of preparation method of high-stability D HA algae oils according to claim 4, it is characterised in that：The step (2)
In, the temperature of freeze-drying is -25 DEG C.
6. a kind of preparation method of high-stability D HA algae oils according to claim 5, it is characterised in that：The step (3)
In, the grain size of aubergine pigment powder is 60 mesh.
7. a kind of preparation method of high-stability D HA algae oils according to claim 6, it is characterised in that：The step (4)
In, the mass concentration of ammonium oxalate solution is 2%.
8. a kind of preparation method of high-stability D HA algae oils according to claim 7, it is characterised in that：The step (4)
In, the weight ratio of aubergine pigment powder and ammonium oxalate solution is 1:27.
9. a kind of preparation method of high-stability D HA algae oils according to claim 8, it is characterised in that：The step (5)
In, the weight ratio for the eggplant bark extract that green kernel extract that DHA algal oil, step (2) obtain, step (4) obtain is
(80-90):(5-10):(1-2), and the weight ratio of green kernel extract, eggplant bark extract is 5:1.
10. a kind of preparation method of high-stability D HA algae oils according to claim 9, it is characterised in that：The step
(5) in, the speed of insulated and stirred is 500rpm.
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Cited By (1)
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| CN109938351A (en) * | 2019-04-09 | 2019-06-28 | 安徽济生元药业有限公司 | It is a kind of to enhance memory, the DHA algal fat capsule of raising intelligence and preparation method thereof |
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| CN109938351A (en) * | 2019-04-09 | 2019-06-28 | 安徽济生元药业有限公司 | It is a kind of to enhance memory, the DHA algal fat capsule of raising intelligence and preparation method thereof |
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