CN110235989A - A kind of marine microalgae dregs of rice composite nutrient microcapsules and its preparation method and application - Google Patents
A kind of marine microalgae dregs of rice composite nutrient microcapsules and its preparation method and application Download PDFInfo
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Abstract
The invention belongs to marine microalgae dregs of rice secondary use field, a kind of marine microalgae dregs of rice composite nutrient microcapsules and its preparation method and application are disclosed.The preparation method of the marine microalgae dregs of rice composite nutrient microcapsules includes: S1, reaction is hydrolyzed in algae dregs of rice fine powder under acid condition, obtains hydrolysis feed liquid；S2, it the pH value for hydrolyzing feed liquid is adjusted to 7 or more carries out Maillard reaction, pH value is adjusted to neutrality and is concentrated and dried later, obtains maillard reaction product；S3, it is uniformly mixed by maillard reaction product, without acid-hydrolyzed algae dregs of rice fine powder, auxiliary wall material and water, forms water phase, then emulsified and dried after the water phase is mixed with grease.Nutrient stability is high in marine microalgae dregs of rice composite nutrient microcapsules provided by the invention, is made an addition in feed, can promote growth of animal, enhance the immunity function of animal, Systemic stress response ability is improved, antibiotic usage is reduced, improves survival rate and growth speed.
Description
Technical field
The invention belongs to marine microalgae dregs of rice secondary use fields, and in particular to a kind of micro- glue of marine microalgae dregs of rice composite nutrient
Capsule and its preparation method and application.
Background technique
There is abundant and unique structure primary or secondary metabolite in marine microalgae, chemical component is extremely complex,
With various physiological activity, such as containing polyunsaturated fatty acid, pigment, protein, polysaccharide etc., there is Important Economic value.
With the rapid development of ocean new industry, the algae dregs of rice enormous amount of the marine microalgae generated after target product, such as where extracted
It manages and efficiently uses these algae dregs of rice and have become a new issue.
Marine microalgae is mainly for the production of polyunsaturated fatty acid, except containing the more insatiable hungers of micro residue in the leftover bits and pieces algae dregs of rice
Outside fatty acid, protein also rich in, polysaccharide etc. are that a kind of medicine of food source extracts raw material, it is verified that
Its is nontoxic without side-effects.For example, protein accounts for about the 50% of biomass in purple ball frustule, meanwhile, purple ball frustule
The polysaccharide of 20%-50% biomass can be accumulated, which is the polymer being made of monosaccharide such as xylose, glucose, galactolipins；It mentions
After taking DHA splitting in the pot algae dregs of rice containing about 40% protein, about 5% polysaccharide and about 1.5% DHA, have very big benefit
With value；Chlorella is a kind of single celled eukaryotic microalgae, is the microalgae that the first is manually cultivated, since structure is simple, growth
Rapidly, toxigenic capacity is low for breeding, can heterotrophic mass culture, chlorella secondary metabolite is abundant, mainly rich in protein, more
The substances such as sugar, unsaturated fatty acid, carotenoid and growth factor.
In feed addictive, antibiotic is used as existing more than 50 years history of animal disease resistant epidemic disease, growth promotion drug, is supporting
Huge effect has been played in growing, and is greatly promoted the development of aquaculture.But the experimental results show that antibiotic exists
Drug resistance is generated using will cause harmful bacteria for a long time in feed, and medicament residue is generated in animal body.In recent years, with the mankind
The raising of living standard and health perception, food-safety problem concern increasingly extensive by global range, forbids antibiotic
The cry that additive is applied in aquaculture is higher and higher.A few days ago, European Union has prohibited uses antibiotic in animal feed,
Many countries including China are also considering ban as implementation of class.Therefore, natural, the green antibiosis of research and development
Plain substitute, it has also become one of the hot subject of Animal nutrition research field in global range.
Summary of the invention
The present invention is intended to provide one kind can be improved algae dregs of rice utilization rate and nutrient stability and reduce antibiotic usage
Marine microalgae dregs of rice composite nutrient microcapsules of amount and its preparation method and application.
In the prior art, mainly using the algae dregs of rice as the substitute of fish meal, or using the nutriment in the algae dregs of rice as
Feed addictive is applied in aquaculture.For example, " splitting application of the pot algae dregs of rice in litopenaeus vannamei compound feed " (2015
Chinese Fishery association Annual Conference thesis summary set) it has studied in mixed feed to split pot algae dregs of rice substitution Partial Fish Meal to South America
The influence of white shrimp cultivation survival rate and the speed of growth, the results showed that, that 20wt% is added in feed splits the pot algae dregs of rice, with substitution
The test group of protein in Partial Fish Meal and the survival rate and growth speed difference of control group are unobvious.For another example, " the pot algae dregs of rice are split
Application study in epinephelus akaara nursery " (science is breeded fish) have studied to split the pot algae dregs of rice instead of the part fish in mixed fodder
Starch the influence to epinephelus akaara survival rate of seedling and growth, the results showed that, replace epinephelus akaara seedling to cooperate with the pot algae dregs of rice are split
The fish slurry of half in feed, survival rate indifference, and the long growth rate of body and body weight growth rate increase.However, with top
Method is that the microalgae algae dregs of rice are added in feed directly as additive, and such nutrient stability is poor, and is promoting aquatic products
Effect in terms of animal growth and raising immunity is also poor.
The present inventor passes through further investigation and finds later, protein and polysaccharide rich in the microalgae algae dregs of rice,
The immunity function of animal can be enhanced, Systemic stress response ability is improved, reduce the usage amount of antibiotic, the microalgae algae dregs of rice are first existed
Maillard reaction is carried out after hydrolyzed under acidic conditions reaction again, gained maillard reaction product has anti-oxidant and increase fragrance
The effect of smell, can not only improve the holding time limit of nutrient core material, but also can enhance the feed wish of animal, promote
Animal growth；Using functional nutrient placental extract grease by over as core material, by the remnants after the above maillard reaction product, extraction grease
The collaboration of the object algae dregs of rice is used as wall material, and nutrient stability is high in gained microcapsules, and can be realized turns waste into wealth the algae dregs of rice, promotes algae
Dregs of rice utilization rate and added value improve the economic benefit and ecological benefits of marine microalgae new industry.Based on this, this hair is completed
It is bright.
Specifically, the present invention provides a kind of preparation methods of marine microalgae dregs of rice composite nutrient microcapsules, wherein the party
Method includes:
S1, it is that reaction is hydrolyzed in 15 μm of algae dregs of rice fine powders below under acid condition by partial size, obtains hydrolysis feed liquid；
S2, the pH value of the hydrolysis feed liquid is adjusted to 7 or more and carries out Maillard reaction, be later adjusted to neutrality pH value
And be concentrated and dried, obtain maillard reaction product；
S3, it is mixed by the maillard reaction product, without the acid-hydrolyzed algae dregs of rice fine powder, auxiliary wall material and water
It is even, water phase is formed, then emulsified and dried after the water phase is mixed with grease to get marine microalgae dregs of rice compound nutritional is arrived
Plain microcapsules.
Further, the algae dregs of rice are that marine microalgae extracts the residue after grease.
Further, the marine microalgae, which is selected from, splits pot algae (schizochytrium sp.), chlorella (chlorella
Sp.), purple ball algae (Porphyridium sp.), my Ken Shi pot algae (ulkenia sp.) and hidden dinoflagellate (crypthecodinium
At least one of sp.).
Further, in step S1, the mode of reaction is hydrolyzed under acid condition as past institute in the algae dregs of rice fine powder
It states and reaction is hydrolyzed again after acid is added in algae dregs of rice fine powder.
Further, the acid is selected from least one of hydrochloric acid, sulfuric acid, phosphoric acid, formic acid, acetic acid and trifluoroacetic acid.
Further, the amount ratio of the algae dregs of rice fine powder and acid is 1kg:(1-50) L, preferably 1kg:(1-10) it is L, more excellent
It is selected as 1kg:(2-5) L, the concentration of the acid is 0.1-5mol/L, preferably 0.5-2mol/L.
Further, in step S1, the condition of the hydrolysis includes that temperature is 80-160 DEG C, preferably 100-140
DEG C, the time is 2-16 hours, preferably 6-12 hours.
Further, the hydrolysis carries out in atmosphere of inert gases.
Further, in step S2, the pH value of the hydrolysis feed liquid is adjusted to 9-11 and carries out Maillard reaction.
Further, it is 60-120 DEG C, preferably 80-100 DEG C that the condition of the Maillard reaction, which includes temperature, and the time is
15-360min, preferably 45-150min.
Further, in step S3, the grease, maillard reaction product, without acid-hydrolyzed algae dregs of rice fine powder, supplementary wall
Mass parts ratio between material and water is (1-30): (1-40): (0.5-25): (0.5-25): (1-120), preferably (5-20):
(5-25):(2-15):(2-15):(10-80)。
Further, the auxiliary wall material is selected from converted starch, Sodium Caseinate, lactalbumin, soybean protein, malt paste
At least one of essence, malt syrup, cyclodextrin, sucrose, arabinose, glucose, lactose, trehalose and mannose.
Further, the grease in polyunsaturated fatty acid, vitamin, biostearin and carrier oil at least one
Kind.
Further, the polyunsaturated fatty acid is selected from docosahexaenoic acid, arachidonic acid, docosapentaenoic
At least one of acid, eicosapentaenoic acid, linoleic acid plus linolenic acid.
Further, the vitamin is selected from least one of vitamin A, vitamine D3 and vitamin E, the dimension life
Plain A includes retinol, vitamine A acetate and Retinol Palmitate.
Further, the biostearin be selected from beta carotene, astaxanthin, canthaxanthin, lutein, luteole, kind
At least one of Lycopene and Co-Q10.
Further, the carrier oil is selected from rapeseed oil, soybean oil, peanut oil, corn oil, sunflower oil, olive oil, castor
At least one of sesame oil, safflower oil and medium-chain fatty glyceride.
Further, the preparation method of marine microalgae dregs of rice composite nutrient microcapsules provided by the invention further includes in step
Antioxidant is added in S3, the antioxidant is oil-soluble inhibitor and/or water soluble antioxidant, the oil-soluble antioxygen
Agent makes an addition in grease, and the water soluble antioxidant makes an addition in water phase.
Further, the oil-soluble inhibitor is selected from Rosmarinus officinalis extract, BHA, BHT, TBHQ, tocopherol, dimension life
At least one of plain C palmitate and lecithin.
Further, it is more to be selected from ascorbic acid, sodium ascorbate, sodium isoascorbate and tea for the water soluble antioxidant
At least one of phenol.
Further, in step S3, before the drying step, further include the steps that lotion carrying out homogeneous.Preferably,
Matter pressure is 40-60MPa, and homogenization cycles are 1-3 times.
The present invention also provides marine microalgae dregs of rice composite nutrient microcapsules prepared by the above method.
In addition, the present invention also provides marine microalgae dregs of rice composite nutrient microcapsules the answering as feed addictive
With.
It is first carried out hydrolysis, then carries out Maillard reaction by the present invention using protein and polysaccharide in the algae dregs of rice,
Maillard reaction product and unhydrolysed algae dregs of rice fine powder compounding are prepared into microcapsules, the gained marine microalgae dregs of rice as wall material later
Nutrient stability is high in composite nutrient microcapsules, makes an addition in feed as additive, can promote animal
Growth enhances the immunity function of animal, improves Systemic stress response ability, and pre- disease prevention occurs, has no drug resistance, noresidue, nothing
Toxic side effect reduces cultivation medication, improves survival rate and growth speed.In a specific embodiment of the invention, this hair is utilized
Bright marine microalgae dregs of rice composite nutrient microcapsules obtained feed South America prawn, can reduce antibiotic usage amount reach 60% with
On.
Specific embodiment
In the present invention, term " the algae dregs of rice " refers to that marine microalgae extracts the residue after grease, wherein extracts the tool of grease
Body mode is known to the skilled person, and therefore not to repeat here.The specific example of the marine microalgae includes but is not limited to: splitting
Pot algae (schizochytrium sp.), chlorella (chlorella sp.), purple ball algae (Porphyridium sp.), I agrees
At least one of family name's pot algae (ulkenia sp.) and hidden dinoflagellate (crypthecodinium sp.), specific kind of above-mentioned microalgae
It is not particularly limited.There is no particular limitation in source of the present invention to the algae dregs of rice fine powder, the microalgae algae dregs of rice can be crushed and be obtained,
It may be commercially available algae dregs of rice fine powder.The partial size of the algae dregs of rice fine powder is for 15 μm hereinafter, preferably 10 μm hereinafter, more preferably 5 μ
M is hereinafter, most preferably 2 μm or less.
It in the present invention, is past by the mode that reaction is hydrolyzed in the algae dregs of rice fine powder under acid condition in step S1
Acid is added in the algae dregs of rice fine powder, reaction is hydrolyzed again later.It wherein, can when the acid can be existing various electrolysis
It generates hydrogen ion or is dissolved in water energy and enough discharge the substance that proton forms hydrogen ion, specific example includes but is not limited to:
At least one of hydrochloric acid, sulfuric acid, phosphoric acid, formic acid, acetic acid and trifluoroacetic acid.The acid is usually made in the form of its aqueous solution
With concentration can be 0.1-5mol/L, preferably 0.5-2mol/L.The amount ratio of the algae dregs of rice fine powder and acid is preferably 1kg:
(1-50) L, more preferably 1kg:(1-10) L, most preferably 1kg:(2-5) L.
In the present invention, in step S1, the condition of the hydrolysis, which generally includes temperature, to be 80-160 DEG C, preferably
It is 100-140 DEG C；Time can be 2-16 hours, preferably 6-12 hours.The hydrolysis is preferably in atmosphere of inert gases
Middle progress can be avoided oxygen in air in this way and interfere to hydrolysis reaction.Keep atmosphere of inert gases mode be
The usual inert gas into hydrolysis reaction system, for example, nitrogen or group 0 element gas.In addition, the hydrolysis feed liquid can be with
Maillard reaction is carried out after directly adjusting through pH value, moisture first can also be concentrated into 10-20wt% and is down to after room temperature
PH value is adjusted again, carries out Maillard reaction again later.
In the present invention, in step S2, the pH value of the Maillard reaction is 7 or more, preferably 9-11.The Mei Lade
The condition of reaction, which generally includes temperature, to be 60-120 DEG C, preferably 80-100 DEG C；Time can be 15-360min, preferably
For 45-150min.It after the Maillard reaction, needs that pH value is adjusted to neutrality and is concentrated and dried, wherein the concentration
Dry condition, which is subject to, is reduced to 5wt% or less for the moisture content in maillard reaction product.
In the present invention, in step S3, the inoxidizability of microcapsules is can be improved in the maillard reaction product, increases fragrance
Smell improves the feed wish of animal, to promote animal growth.It is described to cooperate Mei Lade without acid-hydrolyzed algae dregs of rice fine powder
Reaction product is used as wall material, and the algae dregs of rice are turned waste into wealth, and promotes algae dregs of rice utilization rate and added value, and it is emerging to improve marine microalgae
The economic benefit and ecological benefits of industry.Wherein, the grease, maillard reaction product, without acid-hydrolyzed algae dregs of rice fine powder, auxiliary
The mass parts ratio helped between wall material and water is preferably (1-30): (1-40): (0.5-25): (0.5-25): (1-120), more excellent
Be selected as (5-20): (5-25): (2-15): (2-15): (10-80), the stability for thus matching the microcapsules of formation are high.
In the present invention, in step S3, the specific example of the grease includes but is not limited to: polyunsaturated fatty acid, dimension
At least one of raw element, biostearin and carrier oil.Wherein, the polyunsaturated fatty acid is preferably selected from two dodecahexaenes
At least one of acid, arachidonic acid, clupanodonic acid, eicosapentaenoic acid, linoleic acid plus linolenic acid.The dimension life
Element is preferably selected from least one of vitamin A, vitamine D3 and vitamin E, and the vitamin A includes retinol, dimension life
Plain A acetate and Retinol Palmitate.It is yellow that the biostearin is preferably selected from beta carotene, astaxanthin, canthaxanthin, leaf
At least one of element, luteole, lycopene and Co-Q10.The carrier oil is preferably selected from rapeseed oil, soybean oil, flower
At least one of oil generation, corn oil, sunflower oil, olive oil, castor oil, safflower oil and medium-chain fatty glyceride.
In the present invention, in step S3, the specific example of the auxiliary wall material includes but is not limited to: converted starch, casein
Sour sodium, lactalbumin, soybean protein, maltodextrin, malt syrup, cyclodextrin, sucrose, arabinose, glucose, lactose, sea
At least one of algae sugar and mannose.
A preferred embodiment of the invention, the preparation method of the marine microalgae dregs of rice composite nutrient microcapsules
It further include that antioxidant is added in step s3, gained microcapsules have higher antioxygenic property at this time.The antioxidant can
Think oil-soluble inhibitor, or water soluble antioxidant.Wherein, the specific example packet of the oil-soluble inhibitor
It includes but is not limited to: at least one in Rosmarinus officinalis extract, BHA, BHT, TBHQ, tocopherol, vitamine C palmitate and lecithin
Kind.The specific example of the water soluble antioxidant includes but is not limited to: ascorbic acid, sodium ascorbate, sodium isoascorbate
At least one of with tea polyphenols.When adding oil-soluble antioxidants, made an addition in grease；When addition water soluble antioxidants
When, it is made an addition in water phase, i.e., with maillard reaction product, without the acid-hydrolyzed algae dregs of rice fine powder, auxiliary wall material and water
It is uniformly mixed together and forms water phase.In addition, relative to 100 parts by weight greases or wall material, the dosage of the antioxidant can be
0.2-5 parts by weight.
A preferred embodiment of the invention further includes carrying out lotion before the drying step in step S3
The step of homogeneous.Preferably, homogenization pressure 40-60MPa, homogenization cycles are 1-3 times.
The present invention also provides marine microalgae dregs of rice composite nutrient microcapsules prepared by the above method.
In addition, the present invention also provides marine microalgae dregs of rice composite nutrient microcapsules the answering as feed addictive
With.
The embodiment of the present invention is described below in detail, the examples of the embodiments are intended to be used to explain the present invention, and cannot
It is interpreted as limitation of the present invention.In the examples where no specific technique or condition is specified, described according to the literature in the art
Technology or conditions or carried out according to product description.Reagents or instruments used without specified manufacturer is that can lead to
Cross the conventional products of commercially available acquisition.
Embodiment 1
Take 130kg to extract the purple ball algae dregs of rice after ARA oil, after dry, using grinder by the algae dregs of rice be crushed to 5 μm hereinafter,
Obtain algae dregs of rice fine powder；80kg algae dregs of rice fine powder is taken, the sulfuric acid solution that 800L concentration is 0.5mol/L is added, vacuumizes benefit nitrogen, Yu Wendu
Back hydrolysis reacts 9 hours at 160 DEG C；Hydrolysis feed liquid is concentrated into moisture content to be about 15wt% and be down to room temperature, using hydrogen
Its pH value is adjusted to 9 by sodium oxide molybdena, then the back flow reaction 180min at 120 DEG C, and feed liquid is then down to room temperature, and by pH value
It is adjusted to neutrality, is concentrated and dried, obtains maillard reaction product；Take 40kg maillard reaction product, 25kg without acid-hydrolyzed algae
Each feed liquid is mixed and is added by dregs of rice fine powder, 15kg lactalbumin, 10kg maltodextrin, 1.8kg sodium ascorbate and 120kg purified water
Heat is uniformly dispersed to 55 DEG C, forms water phase；30kg vitamine A acetate (specification: 1.5MIU), 0.6kg TBHQ are mixed equal
It is even, it puts into water phase, 3000rpm high speed shearing emulsification 2min, 40-60MPa high-pressure homogeneous 2 times, lotion is sent into and is spray-dried
Tower is spray-dried, and the inlet temperature that spray drying tower is arranged is 185 DEG C and outlet temperature is 80 DEG C, spray-dried granulation
Afterwards to get purple ball algae dregs of rice multi-vitamins A acetate microcapsules.
Embodiment 2
The pot algae dregs of rice are split after taking 47kg to extract DHA oil, after dry, the algae dregs of rice are crushed to 2 μm hereinafter, obtaining using grinder
Algae dregs of rice fine powder；It takes 30kg algae dregs of rice fine powder, the acetic acid solution that 165L concentration is 1mol/L is added, vacuumize benefit nitrogen, 135 DEG C of Yu Wendu
Lower back hydrolysis reacts 10 hours；Hydrolysis feed liquid is concentrated into moisture content to be about 15wt% and be down to room temperature, using hydroxide
Its pH value is adjusted to 11 by sodium, then the back flow reaction 100min at 120 DEG C, and feed liquid is then down to room temperature, and by pH value tune
Section is concentrated and dried to neutrality, obtains maillard reaction product；Take 15kg maillard reaction product, 8.5kg without the acid-hydrolyzed algae dregs of rice
Fine powder, 5.5kg soybean protein, 3kg lactose and 45kg purified water are uniformly mixed, and it is equal that each feed liquid is mixed and heated to 55 DEG C of dispersions
It is even, form water phase；5.5kg vitamine D3 (specification: 4.0MIU), 7kg rapeseed oil, 0.25kg tocopherol are uniformly mixed, investment
In water phase, 3000rpm high speed shearing emulsification 2min, 40-60MPa high-pressure homogeneous 2 times, lotion feeding spray drying tower is sprayed
Mist is dry, and the inlet temperature that spray drying tower is arranged is 185 DEG C and outlet temperature is 80 DEG C, after spray-dried granulation to get
Split pot algae dregs of rice multi-vitamins D3 microcapsules.
Embodiment 3
It takes 80kg to extract the chlorella dregs of rice after DHA oil, after dry, the algae dregs of rice is crushed to 2 μm hereinafter, obtaining using grinder
Algae dregs of rice fine powder；50kg algae dregs of rice fine powder is taken, the formic acid solution that 2500L concentration is 0.1mol/L is added, vacuumizes benefit nitrogen, Yu Wendu
Back hydrolysis reacts 2 hours at 120 DEG C；Hydrolysis feed liquid is concentrated into moisture content to be about 15wt% and be down to room temperature, using hydrogen
Its pH value is adjusted to 11 by sodium oxide molybdena, then the back flow reaction 15min at 90 DEG C, and feed liquid is then down to room temperature, and by pH value
It is adjusted to neutrality, is concentrated and dried, obtains maillard reaction product；Take 25kg maillard reaction product, 15kg without acid-hydrolyzed algae
Each feed liquid is mixed and heated to 55 DEG C and is uniformly dispersed by dregs of rice fine powder, 15kg sucrose and 80kg purified water, forms water phase；5kg is tieed up and is given birth to
Plain D3 (specification: 4.0MIU), 15kg vitamine A acetate (specification: 1.5MIU), 0.2kg vitamine C palmitate, 0.2kg ovum
Phosphatide is uniformly mixed, and is put into water phase, 3000rpm high speed shearing emulsification 2min, 40-60MPa high-pressure homogeneous 2 times, lotion is sent
Enter spray drying tower to be spray-dried, the inlet temperature that spray drying tower is arranged is 185 DEG C and outlet temperature is 80 DEG C, through spraying
To get chlorella dregs of rice multi-vitamins A acetate/vitamine D3 microcapsules after mist drying-granulating.
Embodiment 4
Take 14kg to extract my Ken Shi pot algae dregs of rice after DHA oil, after dry, using grinder by the algae dregs of rice be crushed to 10 μm with
Under, obtain algae dregs of rice fine powder；10kg algae dregs of rice fine powder is taken, the phosphoric acid solution that 10L concentration is 5mol/L is added, vacuumizes benefit nitrogen, Yu Wendu
Back hydrolysis reacts 16 hours at 80 DEG C；Hydrolysis feed liquid is concentrated into moisture content to be about 15wt% and be down to room temperature, using hydrogen
Its pH value is adjusted to 7 by sodium oxide molybdena, and 360min is then reacted at 60 DEG C, feed liquid is then down to room temperature, and pH value is adjusted
To neutrality, it is concentrated and dried, obtains maillard reaction product；Take 5kg maillard reaction product, 2kg without acid-hydrolyzed algae dregs of rice fine powder,
Each feed liquid is mixed and heated to 55 DEG C and is uniformly dispersed by 1kg arabinose, 1kg glucose and 14kg purified water, forms water phase；Add
Enter 1.4kg beta carotene (specification: 98%), 3.6kg soybean oil, 3000rpm high speed shearing emulsification 2min, 40-60MPa high pressure
Homogeneous 2 times, lotion feeding spray drying tower is spray-dried, the inlet temperature that spray drying tower is arranged is 185 DEG C and goes out
Mouth temperature is 80 DEG C, to get my the compound beta carotene microcapsules of the Ken Shi pot algae dregs of rice after spray-dried granulation.
Embodiment 5
The pot algae dregs of rice are split after taking 6kg to extract DHA oil, after dry, the algae dregs of rice are crushed to 7 μm hereinafter, obtaining using grinder
Algae dregs of rice fine powder；4kg algae dregs of rice fine powder is taken, the trifluoroacetic acid solution that 20L concentration is 1mol/L is added, vacuumizes benefit nitrogen, Yu Wendu 140
Back hydrolysis reacts 6 hours at DEG C；Hydrolysis feed liquid is concentrated into moisture content to be about 15wt% and be down to room temperature, using hydroxide
Its pH value is adjusted to 10 by sodium, then the back flow reaction 45min at 100 DEG C, feed liquid is then down to room temperature, and pH value is adjusted
To neutrality, it is concentrated and dried, obtains maillard reaction product；Take 2kg maillard reaction product, 1kg without acid-hydrolyzed algae dregs of rice fine powder,
Each feed liquid is mixed and heated to 55 DEG C and is uniformly dispersed by 0.5kg converted starch and 6.5kg purified water, forms water phase；3kg is added
DHA algal oil (specification: docosahexenoic acid glyceride content is 40%), 3000rpm high speed shearing emulsification 2min, 40-60MPa
High-pressure homogeneous 2 times, lotion feeding spray drying tower is spray-dried, the inlet temperature that spray drying tower is arranged is 185 DEG C
And outlet temperature is 80 DEG C, splits the compound DHA microcapsules of the pot algae dregs of rice after spray-dried granulation.
Embodiment 6
The hidden dinoflagellate dregs of rice of 9kg Kou Shi are taken, after dry, the algae dregs of rice are crushed to 15 μm hereinafter, obtaining algae dregs of rice fine powder using grinder；It takes
6kg algae dregs of rice fine powder is added the hydrochloric acid solution that 12L concentration is 2mol/L, vacuumizes benefit nitrogen, back hydrolysis is anti-at 100 DEG C of Yu Wendu
It answers 12 hours；Hydrolysis feed liquid is concentrated into moisture content and is about 15wt% and is down to room temperature, using sodium hydroxide by its pH value tune
Section is to 8, and then the back flow reaction 150min at 80 DEG C, is then down to room temperature for feed liquid, and pH value is adjusted to neutrality, and concentration is dry
It is dry, obtain maillard reaction product；Take 3kg maillard reaction product, 1.5kg without acid-hydrolyzed algae dregs of rice fine powder, 1.5kg caseinic acid
Each feed liquid is mixed and heated to 55 DEG C and is uniformly dispersed by sodium and 9kg purified water, forms water phase；By 3kg ARA algae oil (specification: peanut
Tetraene acid glyceride content be 40%), 0.06kg Rosmarinus officinalis extract be uniformly mixed, put into water phase in, 3000rpm high speed shear
2min is emulsified, 40-60MPa high-pressure homogeneous 2 times, lotion feeding spray drying tower is spray-dried, spray drying tower is set
Inlet temperature be 185 DEG C and outlet temperature is 80 DEG C, it is micro- to get the hidden compound ARA of the dinoflagellate dregs of rice of Kou Shi after spray-dried granulation
Capsule.
Comparative example 1
Take 130kg to extract the purple ball algae dregs of rice after ARA oil, after dry, using grinder by the algae dregs of rice be crushed to 5 μm hereinafter,
Obtain algae dregs of rice fine powder；Take 65kg algae dregs of rice fine powder, 15kg lactalbumin, 10kg maltodextrin, 1.8kg sodium ascorbate and 120kg pure
Change water, each feed liquid is mixed and heated to 55 DEG C and is uniformly dispersed, forms water phase；By 30kg vitamine A acetate (specification:
1.5MIU), 0.6kg TBHQ is uniformly mixed, and is put into water phase, 3000rpm high speed shearing emulsification 2min, 40-60MPa high pressure is equal
Matter 2 times, lotion feeding spray drying tower is spray-dried, the inlet temperature that spray drying tower is arranged is 185 DEG C and exports
Temperature is 80 DEG C, to get purple ball algae dregs of rice multi-vitamins A acetate microcapsules after spray-dried granulation.
Comparative example 2
The pot algae dregs of rice are split after taking 47kg to extract DHA oil, after dry, the algae dregs of rice are crushed to 2 μm hereinafter, obtaining using grinder
Algae dregs of rice fine powder；Take 23.5kg without acid-hydrolyzed algae dregs of rice fine powder, 5.5kg soybean protein, 3kg lactose, 45kg purified water, by each material
Liquid is mixed and heated to 55 DEG C and is uniformly dispersed, and forms water phase；By 5.5kg vitamine D3 (specification: 4.0MIU), 7kg rapeseed oil,
0.25kg tocopherol is uniformly mixed, and is put into water phase, 3000rpm high speed shearing emulsification 2min, 40-60MPa high-pressure homogeneous 2 times,
Lotion feeding spray drying tower is spray-dried, the inlet temperature that spray drying tower is arranged is 185 DEG C and outlet temperature is
80 DEG C, pot algae dregs of rice multi-vitamins D3 microcapsules are split after spray-dried granulation.
Comparative example 3
It takes 80kg to extract the chlorella dregs of rice after DHA oil, after dry, the algae dregs of rice is crushed to 2 μm hereinafter, obtaining using grinder
Algae dregs of rice fine powder；It takes 40kg without acid-hydrolyzed algae dregs of rice fine powder, 15kg sucrose, 80kg purified water, each feed liquid is mixed and heated to 55
It DEG C is uniformly dispersed, forms water phase；By 5kg vitamine D3 (specification: 4.0MIU), 15kg vitamine A acetate (specification:
1.5MIU), 0.2kg vitamine C palmitate, 0.2kg lecithin are uniformly mixed, and are put into water phase, 3000rpm high speed shear cream
Change 2min, 40-60MPa high-pressure homogeneous 2 times, lotion feeding spray drying tower is spray-dried, spray drying tower is set
Inlet temperature is 185 DEG C and outlet temperature is 80 DEG C, to get chlorella dregs of rice multi-vitamins A acetic acid after spray-dried granulation
Ester/vitamine D3 microcapsules.
Comparative example 4
Take 14kg to extract my Ken Shi pot algae dregs of rice after DHA oil, after dry, using grinder by the algae dregs of rice be crushed to 10 μm with
Under, obtain algae dregs of rice fine powder；7kg algae dregs of rice fine powder, 1kg arabinose, 1kg glucose, 14kg purified water are taken, by each feed liquid Hybrid Heating
It is uniformly dispersed to 55 DEG C, forms water phase；1.4kg beta carotene, 3.6kg soybean oil, 3000rpm high speed shearing emulsification is added
2min, 40-60MPa high-pressure homogeneous 2 times, lotion feeding spray drying tower is spray-dried, entering for spray drying tower is set
Mouth temperature is 185 DEG C and outlet temperature is 80 DEG C, to get my the compound beta carotene of the Ken Shi pot algae dregs of rice after spray-dried granulation
Microcapsules.
Comparative example 5
Take 130kg to extract the purple ball algae dregs of rice after ARA oil, after dry, using grinder by the algae dregs of rice be crushed to 5 μm hereinafter,
Obtain algae dregs of rice fine powder；80kg algae dregs of rice fine powder is taken, the sulfuric acid solution that 800L concentration is 0.5mol/L is added, vacuumizes benefit nitrogen, Yu Wendu
Back hydrolysis reacts 9 hours at 160 DEG C；Hydrolysis feed liquid is concentrated into moisture content to be about 15wt% and be down to room temperature, using hydrogen
Its pH value is adjusted to 9 by sodium oxide molybdena, then the back flow reaction 180min at 120 DEG C, and feed liquid is then down to room temperature, and by pH value
It is adjusted to neutrality, is concentrated and dried, obtains maillard reaction product；Take 40kg maillard reaction product, 30kg lactalbumin, 20kg wheat
Each feed liquid is mixed and heated to 55 DEG C and is uniformly dispersed by bud dextrin, 1.8kg sodium ascorbate and 120kg purified water, forms water phase；
30kg vitamine A acetate (specification: 1.5MIU), 0.6kg TBHQ are uniformly mixed, put into water phase, 3000rpm high speed is cut
Emulsification 2min is cut, 40-60MPa high-pressure homogeneous 2 times, lotion feeding spray drying tower is spray-dried, setting spray drying
The inlet temperature of tower is 185 DEG C and outlet temperature is 80 DEG C, to get purple ball algae dregs of rice multi-vitamins A after spray-dried granulation
Acetate microcapsules.
Test case
(1) vitamin content stability test is tested
Embodiment 1-4 and the resulting microcapsules of comparative example 1-4 are vacuumized with aluminium foil bag and packed, then in temperature 50 C
± 2 DEG C, carry out the test of microcapsule stability under the conditions of humidity 75RH ± 5%RH, comparison the 2nd week, the 4th week and the 8th week steady
Qualitative, acquired results are shown in Table 1.
The content of vitamin A is according to GB/T 7292-1999 " feed addictive retinyl acetate particle " in microcapsules
Method detected, the content of vitamine D3 according to GB/T 9840-2006 " feed addictive vitamin d3 beadlet " method
Detected, the content of beta carotene according to GB 28310-2012 " food additives beta carotene (fermentation method) " side
Method is detected.
The vitamin stability test result of embodiment 1-4 and comparative example 1-4 is shown, is obtained using method provided by the invention
The microcapsules arrived stability with higher joined Mei Lade in the preparation process of the microcapsules of embodiment 1-4 in wall material
Reaction product, the 2nd week, the 4th week and the 8th week content drop range are obviously smaller than comparative example 1-4, it is seen that use side provided by the invention
Method is remarkably improved the stability of vitamin content in microcapsules.In addition, micro- glue can be assigned using method provided by the invention
The special burnt odor taste of capsule.
(2) to the Experiment on Function of cultured prawn growth and development, raising immunity
Control group and test group are feeds utilized as follows:
Compare 1 group: normal diet (No. 1 South America white shrimp feed purchased from Zhuhai Qiang Long Biotechnology Co., Ltd)；
Compare 2 groups: normal diet+0.5wt% Enrofloxacin is mixed bait and is fed；
Microcapsules prepared by 3 groups: normal diet+0.0025wt% comparative example 5 are compareed, bait is mixed and feeds；
Microcapsules prepared by 1 group: normal diet+0.0025wt% embodiment 1 are tested, bait is mixed and feeds；
Microcapsules+0.1wt% Enrofloxacin prepared by 2 groups: normal diet+0.0025wt% embodiment 1 is tested, bait is mixed
It feeds；
Microcapsules+0.2wt% Enrofloxacin prepared by 3 groups: normal diet+0.0025wt% embodiment 1 is tested, bait is mixed
It feeds；
Test microcapsules+0.3wt% Enrofloxacin prepared by 4 groups: normal diet+0.0025wt% embodiment 1, spice
It feeds.
The comparable South America prawn of individual head weight is tested on the comparable shrimp pool of environmental condition, wherein the shrimp of 1 group of control
The pool feeds normal diet, and the shrimp pool of 2 groups of control feeds with same normal diet and be mixed with the feed of 0.5wt% Enrofloxacin, right
The feed of microcapsules prepared by 0.0025wt% comparative example 5 is fed with same normal diet and be mixed with according to 3 groups of the shrimp pool, is tested
1 group of the shrimp pool feeds with same normal diet and is mixed with the feed of microcapsules prepared by 0.0025wt% embodiment 1, test 2
The shrimp pool of group feeds with same normal diet and is mixed with microcapsules prepared by 0.0025wt% embodiment 1 and 0.1wt% grace promise
The shrimp pool of the feed of Sha Xing, 3 groups of test feeds with same normal diet and is mixed with micro- glue prepared by 0.0025wt% embodiment 1
The feed of capsule and 0.2wt% Enrofloxacin, the shrimp pool of 4 groups of test feed with same normal diet and are mixed with 0.0025wt% implementation
The feed of microcapsules prepared by example 1 and 0.3wt% Enrofloxacin.It weighs within the 27th day after test, while according to the shrimp pool before testing
Prawn density and test after density, calculate prawn infectious age, the results are shown in Table 2.
As shown in Table 2, using being added to marine microalgae dregs of rice composite nutrient microcapsules prepared by the present invention
Feed is raised prawn (1 group of test), the prawn speed of growth ratio speed of growth fast 1 for being not added with above-mentioned microcapsules (1 group of control)
Times or more, the speed of growth of 3 groups than control is 0.5 times fast, and prawn growth is uniformly, and vigor is high, body colour health, and feed wish is obvious
Than feeding the high of normal diet, therefore the speed of growth is faster.It is shown according to the investigation result before test, when testing initial, each shrimp
The prawn germ infection rate on the pool is 45% or more, and it is dead to have a small amount of prawn daily, but tests 1 group of pair raised
Shrimp, the death rate of prawn starts to be decreased obviously after raising 3 days, it is possible thereby to illustrate, it is made that the present invention is added in normal diet
The immunity of prawn can be improved in standby microcapsules, reduces the usage amount of antibiotic.Further, from 2 groups of control and test 1-4
From the point of view of the test result of group, the usage amount of Enrofloxacin be the 40% of 2 groups of control in 3 groups of test, has been reached and to compare 2 groups same
Mortality level, it is seen then that feed South America prawn using the nutrient microcapsules that are prepared of the present invention, antibiotic can be reduced
Usage amount reaches 60% or more.And the shrimp pool (1 group of control) of normal diet is fed, the shrimp that dies of illness, and quantity can be salvaged per average daily
It is continuously increased, because the dead quantity of germ infection is more than 50% after 27 days, it is therefore seen that, the ocean that the present invention is prepared is micro-
Algae dregs of rice composite nutrient microcapsules have remarkable result in terms of promoting prawn growth and development and improving immunity.
Claims (10)
1. a kind of preparation method of marine microalgae dregs of rice composite nutrient microcapsules, which is characterized in that this method comprises:
S1, it is that reaction is hydrolyzed in 15 μm of algae dregs of rice fine powders below under acid condition by partial size, obtains hydrolysis feed liquid；
S2, the pH value of the hydrolysis feed liquid is adjusted to 7 or more and carries out Maillard reaction, be later adjusted to neutrality pH value and dense
Contracting drying, obtains maillard reaction product；
S3, it is uniformly mixed by the maillard reaction product, without the acid-hydrolyzed algae dregs of rice fine powder, auxiliary wall material and water, shape
It is emulsified and is dried at water phase, then after the water phase is mixed with grease to get micro- to marine microalgae dregs of rice composite nutrient
Capsule.
2. the preparation method of marine microalgae dregs of rice composite nutrient microcapsules according to claim 1, which is characterized in that described
The algae dregs of rice are that marine microalgae extracts the residue after grease；Preferably, the marine microalgae, which is selected from, splits pot algae (schizochytrium
Sp.), chlorella (chlorella sp.), purple ball algae (Porphyridium sp.), my Ken Shi pot algae (ulkenia sp.) and
At least one of hidden dinoflagellate (crypthecodinium sp.).
3. the preparation method of marine microalgae dregs of rice composite nutrient microcapsules according to claim 1 or 2, which is characterized in that
It is that acid is added into the algae dregs of rice fine powder by the mode that reaction is hydrolyzed in the algae dregs of rice fine powder under acid condition in step S1
Reaction is hydrolyzed again later；Preferably, it is described acid in hydrochloric acid, sulfuric acid, phosphoric acid, formic acid, acetic acid and trifluoroacetic acid extremely
Few one kind；Preferably, the algae dregs of rice fine powder and acid amount ratio be 1kg:(1-50) L, preferably 1kg:(1-10) L, more preferably
For 1kg:(2-5) L, the concentration of the acid is 0.1-5mol/L, preferably 0.5-2mol/L.
4. the preparation method of marine microalgae dregs of rice composite nutrient microcapsules according to claim 1 or 2, which is characterized in that
In step S1, the condition of the hydrolysis include temperature be 80-160 DEG C, preferably 100-140 DEG C, the time be 2-16 hours,
Preferably 6-12 hours；Preferably, the hydrolysis carries out in atmosphere of inert gases.
5. the preparation method of marine microalgae dregs of rice composite nutrient microcapsules according to claim 1 or 2, which is characterized in that
In step S2, the pH value of the hydrolysis feed liquid is adjusted to 9-11 and carries out Maillard reaction；The condition packet of the Maillard reaction
Including temperature is 60-120 DEG C, preferably 80-100 DEG C, time 15-360min, preferably 45-150min.
6. the preparation method of marine microalgae dregs of rice composite nutrient microcapsules according to claim 1 or 2, which is characterized in that
In step S3, the grease, maillard reaction product, without acid-hydrolyzed algae dregs of rice fine powder, auxiliary wall material and water between quality
Portion rate is (1-30): (1-40): (0.5-25): (0.5-25): (1-120), preferably (5-20): (5-25): (2-15):
(2-15):(10-80)。
7. the preparation method of marine microalgae dregs of rice composite nutrient microcapsules according to claim 1 or 2, which is characterized in that
The auxiliary wall material is selected from converted starch, Sodium Caseinate, lactalbumin, soybean protein, maltodextrin, malt syrup, ring
At least one of dextrin, sucrose, arabinose, glucose, lactose, trehalose and mannose；
Optional, the grease is selected from least one of polyunsaturated fatty acid, vitamin, biostearin and carrier oil；
Optional, the polyunsaturated fatty acid is selected from docosahexaenoic acid, arachidonic acid, clupanodonic acid, two
At least one of ten carbon 5 alkene acids, linoleic acid plus linolenic acid；
Optional, the vitamin is selected from least one of vitamin A, vitamine D3, vitamin E and vitamine A acetate；
Optional, the biostearin is selected from beta carotene, astaxanthin, canthaxanthin, lutein, luteole, lycopene
At least one of with Co-Q10；
It is optional, the carrier oil be selected from rapeseed oil, soybean oil, peanut oil, corn oil, sunflower oil, olive oil, castor oil,
At least one of safflower oil and medium-chain fatty glyceride.
8. the preparation method of marine microalgae dregs of rice composite nutrient microcapsules according to claim 1 or 2, which is characterized in that
This method further includes that antioxidant is added in step s3, and the antioxidant is oil-soluble inhibitor and/or water-soluble antioxygen
Agent, the oil-soluble inhibitor make an addition in grease, and the water soluble antioxidant makes an addition in water phase；Preferably, institute
It states oil-soluble inhibitor and is selected from Rosmarinus officinalis extract, BHA, BHT, TBHQ, tocopherol, vitamine C palmitate and lecithin
At least one of；Preferably, the water soluble antioxidant be selected from ascorbic acid, sodium ascorbate, sodium isoascorbate and
At least one of tea polyphenols.
9. the marine microalgae dregs of rice composite nutrient microcapsules that the method as described in any one of claim 1-8 is prepared.
10. application of the marine microalgae dregs of rice composite nutrient microcapsules as claimed in claim 9 as feed addictive.
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| WO2016029647A1 (en) * | 2014-08-26 | 2016-03-03 | 威海市世代海洋生物科技有限公司 | Active seaweed feed additive and preparation method therefor |
| CN105685770A (en) * | 2016-03-10 | 2016-06-22 | 厦门汇盛生物有限公司 | Method for preparing grease microcapsule powder from Maillard reaction product |
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| CN101978872A (en) * | 2010-10-25 | 2011-02-23 | 广东润科生物工程有限公司 | Microalgae seasonings and preparation method thereof |
| CN103937858A (en) * | 2014-04-11 | 2014-07-23 | 广东润科生物工程有限公司 | Method for preparing antioxidant by using schizochytrium limacinum algal meal |
| WO2016029647A1 (en) * | 2014-08-26 | 2016-03-03 | 威海市世代海洋生物科技有限公司 | Active seaweed feed additive and preparation method therefor |
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