CN104513704A - Extraction method for odourless DHA oil - Google Patents

Extraction method for odourless DHA oil Download PDF

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Publication number
CN104513704A
CN104513704A CN201410752678.5A CN201410752678A CN104513704A CN 104513704 A CN104513704 A CN 104513704A CN 201410752678 A CN201410752678 A CN 201410752678A CN 104513704 A CN104513704 A CN 104513704A
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dha
concentrated solution
fermented liquid
membrane
water
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CN104513704B (en
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梁书俊
赵书林
夏德才
胡锐
杨齐华
李寰
闵征桥
龚于堞
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HUBEI FUXING BIOLOGICAL TECHNOLOGY Co Ltd
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HUBEI FUXING BIOLOGICAL TECHNOLOGY Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/02Pretreatment
    • C11B1/025Pretreatment by enzymes or microorganisms, living or dead
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/02Pretreatment
    • C11B1/04Pretreatment of vegetable raw material
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/10Production of fats or fatty oils from raw materials by extracting

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Biochemistry (AREA)
  • Microbiology (AREA)
  • Fats And Perfumes (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)

Abstract

The invention relates to an extraction method for odourless DHA oil. The method comprises the steps of: (1) fermentation: fermenting DHA containing Schizochytrium limacinum to obtain a fermentation broth; (2) fermentation broth dehydration: subjecting the fermentation broth to natural sedimentation, removing part of water in the fermentation broth, and taking the sedimentated concentrated liquid; (3) washing: using a ceramic membrane to conduct recirculating filtration on the concentrated liquid and performing washing; (4) cell wall breaking by a high pressure homogenizer; (5) dehydration treatment on the cell wall broken concentrated liquid; and (6) dissolution of the dehydrated concentrated liquid in an n-hexane solvent or a 95% ethanol solvent to perform extraction and desolvation so as to obtain DHA oil. The method provided by the invention greatly improves the taste and odor of DHA oil, reduces the wall breaking time, also improves the extraction efficiency and productivity of the extraction section, and is basically free of emulsification phenomenon, greatly saves the production cost, and improves production efficiency.

Description

A kind of extracting method without fishy smell DHA grease
Technical field
The invention belongs to the Study on extraction field of microbial oil, be specifically related to a kind of extracting method without fishy smell DHA grease.
Background technology
DHA is commonly called as " DHA (docosahexaenoic acid) ", Chinese is referred to as docosahexenoic acid, chemical name is 22 carbon-4,7,10,13,16,19-acid (all-cis formula), referred to as C22:6 (ω-3), belong to ω-3(n-3) serial long chain polyunsaturated fatty acids is a kind of to the very important polyunsaturated fatty acid of human body.
First, DHA is one of main moiety of human brain, mainly exists in phospholipid form, accounts for about 30% of brain cell lipid acid.At fetal period, DHA must obtain from parent, and women is at gestation time, if DHA intake is not enough, the brain cell g and D of fetus can be caused abnormal, and serious meeting produces retarded.In infant period, brain is in growth and development stage, and research shows, containing the baby that DHA is abundant in diet, thinking is quicker than general baby, and language ability and learning capacity are also strong than general baby, and the probability of suffering from nervous system disorders (as neurosis) is also much lower.Adolescent student, because learning tasks are heavy, take in DHA can memory, improve attention etc.To grownup, DHA maintains the requisite material of physiological function, particularly brain worker and the elderly, if DHA insufficiency of intake, then brain function can reduce, there will be absent minded, feel depressed and the situation such as inefficiency, more serious may cause senile dementia.
Secondly, DHA has anticoagulation, suppresses platelet aggregation and thrombotic effect, thus can prevent the generation of the cardiovascular disordeies such as myocardial infarction.
Three, DHA in the retina of people rich content, be the important composition composition of retinal tissue.Experiment proves, adds a certain amount of DHA, contribute to the growth of baby's eyes in food, baby's visual development and function maturation also earlier, and their quick-eyed than common children; Long-term lacking DHA, eyesight can reduce, due to DHA, this mainly can promote that optic nerve film extends, and maintains vision normal function.
Finally, DHA has and suppresses the effect of cancer, can the obviously generation of Tumor suppression, growth and transfer.Research shows, scientist makes DHA transfer to from neural system in medulloblastoma, when DHA is after endocellular metabolism, then analyzes the by product in cell.Scientist have studied DHA and derivative thereof to the impact of growth of cancer cells subsequently.Result of study shows, DHA kills all cancer cells, and the toxicity ratio DHA produced by DHA derivative itself more can kill cancer cells effectively.This shows, DHA can become the novel drugs of a kind of new treatment neuroblastoma or other cancers.
In current DHA grease production technique both domestic and external, most what adopt is Production by Enzymes, namely after employing biological means makes the somatic cells wall fragmentation in fermented liquid, with organic solvent by oil extraction in born of the same parents out.The oil yield of adopting gained is in this way higher, but, also relatively high for equipment requirements, fermentation liquor disk plate centrifuge concentrates, a part of frustule can be lost, and can add a large amount of water in concentrated solution in enzymolysis process, then need to adopt extractor and a large amount of organic solvents that respective volume is very large; Meanwhile, in enzyme process extraction, owing to containing a large amount of water in fermented liquid, when some colloidalmaterial and protein etc. stir in the presence of an organic, be easy to the emulsification causing whole system, once emulsification occurs, grease-contained organic layer is separated with water layer, just must add a large amount of ethanol breakdowns of emulsion, or add a large amount of salt breakdowns of emulsion, and breakdown of emulsion usually spends the plenty of time, so not only increase and control difficulty, also greatly increase production cost, reduce production efficiency, be difficult to realize continuous prodution; In addition, common enzymolysis time is 8h, and the long meeting of enzymolysis time brings acid smell to DHA grease, and this taste is that enzyme itself is subsidiary, DHA grease also can be made to darken simultaneously, bring difficulty, especially in summer to follow-up oil and fat refining.
Summary of the invention
The object of the invention is to solve large, the consuming time length of existing DHA grease extracting method rate of loss, power consumption is large, and the grease fishy smell the extracted problem such as heavily, and a kind of novel DHA grease extraction process is provided.
To achieve these goals, the extracting method without fishy smell DHA grease provided by the invention, comprises the following steps:
(1), ferment: the schizochytrium limacinum containing DHA is fermented, obtains fermented liquid;
(2), fermented liquid dewaters: fermented liquid obtained for step () is left standstill 1-2h and carries out natural subsidence, in removing fermented liquid, the water of 35-45%, gets sedimentation concentration liquid;
(3), wash: utilize ceramic membrane circulating filtration concentrated solution, then wash concentrated solution with water;
(4), cell walls is broken: utilize high pressure homogenizer that cell walls is carried out fragmentation;
(5), dewater: the method adopting ethanol dehydration or spraying dry dehydration, processed is carried out to the concentrated solution after cell walls fragmentation;
(6), oil extraction: the concentrated solution after processed is dissolved in normal hexane solvent or 95% alcohol solvent in carry out extracting, precipitation obtains DHA grease.
Preferably, in described step (three), ceramic membrane diameter is 0.1-1um; Wash water temperature used and be 25-30 DEG C, washing time is 30min, washes 2-3 times that water consumption used is concentrated solution.Water temperature is on the impact of this step, and be mainly manifested in fermentation broth viscosity and filtering velocity, water temperature controls at 25-30 DEG C, and fermentation broth viscosity is lower, and filtering velocity is fast.
Preferably, described ceramic membrane comprises first step filtering membrane and second stage filtering membrane, and the diameter of described first step filtering membrane is 0.5-1um; The diameter of described second stage filtering membrane is 0.1-0.5um; In first step membrane filtration removing fermented liquid after impurity, enter second stage membrane filtration.Find when after the washing of fermentation liquor first ceramic membrane circulating filtration through experimental study, some macromole impurity and waste water remove substantially, now when second ceramic membrane, filtering velocity can accelerate, make cell content material more effective through, and the frustule cell walls of microscopy 90% breaks because of osmotic pressure reason.
Preferably, in described step (four), the pressure of high pressure homogenizer is 10-40MPa, and homogenization cycles is 1-3 times.Homogenization pressure and homogenization cycles can be regulated according to the particular case of cell wall rupture.
The invention has the beneficial effects as follows:
(1) the present invention is first by fermented liquid natural subsidence, and then utilize ceramic membrane circulating filtration to wash concentrated solution, technological design is reasonable, and reaction conditions is easy to get, and loss cell rate is zero substantially, also reduces extractor volume simultaneously, is easy to realize industrialization.
(2) the present invention greatly improves the gas flavour of DHA grease, utilizes ceramic membrane circulating filtration to wash and removes some water miscible fishy smell material, micromolecular polysaccharide and impurity in cell, solves that DHA grease color is dark, the fishy smell problem such as heavily.
(3) the present invention selects high-pressure homogeneous replacement enzymolysis broken wall, the DHA grease lighter color obtained, without the acid smell that enzymolysis process is brought into, and consuming time short, consume energy low, greatly saved production cost, enhanced productivity.
The inventive method utilizes the washing of ceramic membrane circulating filtration, high pressure homogenizer broken wall, greatly improves the taste smell of DHA grease, decreases broken time.In addition, ceramic membrane circulating filtration eliminates a large amount of waste water, fermentating liquid volume is reduced, greatly reduce the usage quantity of organic solvent, reduce extractor volume simultaneously, also improve the production capacity of extraction efficiency and extraction workshop section, and substantially do not have the generation of emulsion, greatly save production cost, enhanced productivity.
Embodiment
Be clearly and completely described 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.
The plant and instrument that each embodiment uses is all commercial conventional equipment, and the reagent that each embodiment uses is all commercial conventional reagent.
Embodiment 1:
Without the extracting method of fishy smell DHA grease, comprise the following steps:
(1), ferment: the schizochytrium limacinum containing DHA is fermented, obtains fermented liquid;
(2), fermented liquid dewaters: the fermented liquid that step () is obtained is left standstill 2h and carries out natural subsidence, remove the water of in fermented liquid 43%, get sedimentation concentration liquid;
(3), wash: utilize ceramic membrane circulating filtration concentrated solution, ceramic membrane comprises first step filtering membrane and second stage filtering membrane, and the diameter of first step filtering membrane is 1um; The diameter of described second stage filtering membrane is 0.5um; In first step membrane filtration removing fermented liquid after impurity, enter second stage membrane filtration, then wash concentrated solution with water, washing water temperature used is 30 DEG C, and washing time is 30min, washes 3 times that water consumption used is concentrated solution.
(4), cell walls is broken: utilize high pressure homogenizer that cell walls is carried out fragmentation, the pressure of high pressure homogenizer is 10MPa, and homogenization cycles is 3 times;
(5), dewater: the method adopting ethanol dehydration or spraying dry dehydration, processed is carried out to the concentrated solution after cell walls fragmentation;
(6), oil extraction: the concentrated solution after processed is dissolved in the alcohol solvent of 95% carry out extracting, precipitation must without fishy smell DHA grease.
Embodiment 2:
Without the extracting method of fishy smell DHA grease, comprise the following steps:
(1), ferment: the schizochytrium limacinum containing DHA is fermented, obtains fermented liquid;
(2), fermented liquid dewaters: the fermented liquid that step () is obtained is left standstill 1.5h and carries out natural subsidence, remove the water of in fermented liquid 40%, get sedimentation concentration liquid;
(3), wash: utilize ceramic membrane circulating filtration concentrated solution, ceramic membrane comprises first step filtering membrane and second stage filtering membrane, and the diameter of first step filtering membrane is 0.8um; The diameter of described second stage filtering membrane is 0.2um; In first step membrane filtration removing fermented liquid after impurity, enter second stage membrane filtration, then wash concentrated solution with water, washing water temperature used is 25 DEG C, and washing time is 30min, washes 2 times that water consumption used is concentrated solution.
(4), cell walls is broken: utilize high pressure homogenizer that cell walls is carried out fragmentation, the pressure of high pressure homogenizer is 40MPa, and homogenization cycles is 1 time;
(5), dewater: the method adopting ethanol dehydration or spraying dry dehydration, processed is carried out to the concentrated solution after cell walls fragmentation;
(6), oil extraction: the concentrated solution after processed is dissolved in normal hexane solvent carry out extracting, precipitation must without fishy smell DHA grease.
Embodiment 3:
Without the extracting method of fishy smell DHA grease, comprise the following steps:
(1), ferment: the schizochytrium limacinum containing DHA is fermented, obtains fermented liquid;
(2), fermented liquid dewaters: the fermented liquid that step () is obtained is left standstill 1h and carries out natural subsidence, remove the water of in fermented liquid 35%, get sedimentation concentration liquid;
(3), wash: utilize ceramic membrane circulating filtration concentrated solution, ceramic membrane comprises first step filtering membrane and second stage filtering membrane, and the diameter of first step filtering membrane is 0.5um; The diameter of described second stage filtering membrane is 0.1um; In first step membrane filtration removing fermented liquid after impurity, enter second stage membrane filtration, then wash concentrated solution with water, washing water temperature used is 28 DEG C, and washing time is 30min, washes 2 times that water consumption used is concentrated solution.
(4), cell walls is broken: utilize high pressure homogenizer that cell walls is carried out fragmentation, the pressure of high pressure homogenizer is 20MPa, and homogenization cycles is 3 times;
(5), dewater: the method adopting ethanol dehydration or spraying dry dehydration, processed is carried out to the concentrated solution after cell walls fragmentation;
(6), oil extraction: the concentrated solution after processed is dissolved in normal hexane solvent carry out extracting, precipitation must without fishy smell DHA grease.
Embodiment 4:
Without the extracting method of fishy smell DHA grease, comprise the following steps:
(1), ferment: the schizochytrium limacinum containing DHA is fermented, obtains fermented liquid;
(2), fermented liquid dewaters: the 120kg fermented liquid natural subsidence 1h obtained by step (), removes the water of 40%, obtain sedimentation concentration liquid 70kg;
(3), ceramic membrane circulating filtration washing: the first step filtering membrane utilizing diameter to be 0.1um and diameter are the second stage filtering membrane circulating filtration washing concentrated solution of 0. 6 um, water temperature is 25 DEG C, total amount of water is 140kg, the color and luster of filtrate, salty fishy smell, specific conductivity are successively decreased gradually with filtration washing time, washing time is 30min, now filtrate specific conductivity and pure water close, stop filter, finally obtain concentrated cleaning solution and be about 30Kg;
(4), high-pressure homogeneous cell walls is broken: utilize high pressure homogenizer that cell walls is carried out fragmentation, the pressure of high pressure homogenizer is 20MPa, and homogenization cycles is 3 times;
(5), dewater: the concentrated cleaning solution spraying dry after homogeneous is removed remaining moisture, and spray tower inlet temperature is 150-170 DEG C, and air outlet temperature is 60-90 DEG C;
(6), oil extraction: the concentrated solution after processed is dissolved in normal hexane solvent carry out extracting, precipitation must without fishy smell DHA grease.
Embodiment 1-4DHA oil extraction situation is in table 1.
Table 1DHA oil extraction situation
Show that the DHA grease extraction yield that the present invention obtains is high by table 1, lighter color, without fishy smell.
Above-described embodiment is several preferably scheme of the present invention, not any pro forma restriction is done to the present invention, other change is also had under the prerequisite not exceeding the technical scheme described in claim, although this specification sheets is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of specification sheets is only for clarity sake, those skilled in the art should by specification sheets integrally, technical scheme in each embodiment also can through appropriately combined, form other embodiments that it will be appreciated by those skilled in the art that.

Claims (4)

1., without an extracting method for fishy smell DHA grease, it is characterized in that comprising the following steps:
(1), ferment: the schizochytrium limacinum containing DHA is fermented, obtains fermented liquid;
(2), fermented liquid dewaters: fermented liquid obtained for step () is left standstill 1-2h and carries out natural subsidence, in removing fermented liquid, the water of 35-45%, gets sedimentation concentration liquid;
(3), wash: utilize ceramic membrane circulating filtration concentrated solution, then wash concentrated solution with water;
(4), cell walls is broken: utilize high pressure homogenizer that cell walls is carried out fragmentation;
(5), dewater: the method adopting ethanol dehydration or spraying dry dehydration, processed is carried out to the concentrated solution after cell walls fragmentation;
(6), oil extraction: the concentrated solution after processed is dissolved in normal hexane solvent or 95% alcohol solvent in carry out extracting, precipitation obtains DHA grease.
2. the extracting method without fishy smell DHA grease according to claim 1, is characterized in that: in described step (three), and ceramic membrane diameter is 0.1-1um; Wash water temperature used and be 25-30 DEG C, washing time is 30min, washes 2-3 times that water consumption used is concentrated solution.
3. the extracting method without fishy smell DHA grease according to claim 2, is characterized in that: described ceramic membrane comprises first step filtering membrane and second stage filtering membrane, and the diameter of described first step filtering membrane is 0.5-1um; The diameter of described second stage filtering membrane is 0.1-0.5um; In first step membrane filtration removing fermented liquid after impurity, enter second stage membrane filtration.
4. the extracting method without fishy smell DHA grease according to claim 1, is characterized in that: in described step (four), and the pressure of high pressure homogenizer is 10-40MPa, and homogenization cycles is 1-3 times.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106398857A (en) * 2016-11-29 2017-02-15 广东省生物工程研究所(广州甘蔗糖业研究所) Method for extracting Schizochytrium limacinum oil and application thereof

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106398857A (en) * 2016-11-29 2017-02-15 广东省生物工程研究所(广州甘蔗糖业研究所) Method for extracting Schizochytrium limacinum oil and application thereof
CN106398857B (en) * 2016-11-29 2020-02-14 广东省生物工程研究所(广州甘蔗糖业研究所) Method for extracting schizochytrium limacinum grease and application thereof

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