Using ovalbumin-inulin as the preparation method of the microcapsules of wall material
Technical field
It is specifically a kind of using ovalbumin-inulin as the micro- of wall material the present invention relates to a kind of microcapsule preparation method
The preparation method of capsule.
Background technique
Microencapsulation technology, abbreviation microcapsule method, is usually made of two parts, that is, the core material and outside being embedded are coated
Wall material is the modern industry new and high technology to grow up in recent years, can be widely applied to weaving, fragrance, cosmetics, print
The fields such as dye, food.Its principle is exactly the microencapsulation being embedded in solid, liquid or gas material in terms of micron or nanometer
In, and the expected release for the material that is embedded is controlled under certain conditions.At present microencapsulation technology food, medicine, fragrance,
The industries such as dyestuff are used widely, it is known that the wall material of microcapsules is the key that microencapsulation technology, good wall material one
Aspect, which can be played on the good protection of core material, and homeostasis is not easy is influenced by external environment and decomposes denaturation, keeps its biology living
Property reaches larger reserving degree or raising, on the other hand can also make to embed by the control of delivery mode, time, speed and amount
Object biological function is preferably played.The raw material for making microcapsule wall material all the time has single protein, sodium alginate, shell
Glycan, gelatin, porous-starch etc. also have compounding for protein and polysaccharide.For oiliness core material, usually wrapped with aqua
Wrap up in the microcapsules to form oil-in-water structure, as wall material selection when, have the following problems: (1) wall material of single protide due to
The reason stability that hydrophily is weaker and shell thickness is relatively thin is poor, and extraneous poor environment can destroy embedded object;(2) due to embedding
Effect is poor, to influence the bioactivity of core material, reduces human absorptivity;(3) due to being formed between single protein macromolecule
Shell the reason of there are larger gaps, shell structurre is relatively thin, cannot achieve small enteric release, and sustained release effect truly is not achieved
Fruit.(4) selection of shell structurre only considers harmless to human body or animal, does not consider the health-care effect of deep layer further.
Summary of the invention
The purpose of the present invention is to solve above-mentioned technical problem, a kind of simple process is provided, core-shell structure is stablized, sustained release
Effect is good, absorbs beneficial to human consumption, has both health-care effect, the good albumen of embedding rate, conversion ratio, effective percentage, bioactivity
Albumen-inulin microcapsules preparation method.
Technical solution comprising the following specific steps
(1) ovalbumin is soluble in water, ovalbumin dispersion liquid is obtained after carrying out magnetic agitation;
(2) inulin is added into the ovalbumin dispersion liquid, is ultrasonically treated after magnetic agitation, obtained albumen egg
White-inulin solution;
(3) oiliness core material is added in the ovalbumin-inulin solution, obtains mixed solution;
(4) mixed solution is placed in shearing under high speed shear instrument and obtains colostrum, then high pressure microjet homogeneous is more
Secondary, finally spray drying obtains microcapsule granule.
In the step (1), egg protein concentration is 1.0-1.4%w/w in ovalbumin dispersion liquid.
In the step (2), inulin concentration is 1.0-1.4%w/w in the ovalbumin-inulin solution.
In the step (2), magnetic agitation frequency is 30-40rpm/min, ultrasonic intensity 180-200W/cm2, surpass
The sound time is 1-2 hours.
In the step (3), the additive amount additive amount of the medium oil core material of mixed solution is 5-10%w/w.
In the step (4), the revolving speed of the high speed shear instrument is 20000-25000rpm/min, shear time 1-
3min, control high pressure microjet homogeneous pressure is 11-13kPa.
In the step (4), spray drying condition are as follows: inlet air temperature is 170-190 DEG C, and leaving air temp is 85-90 DEG C, into
Stream speed is 500-600ml/h.
For the problems in background technique, inventor has made intensive studies the wall material of existing core-shell structure, by ovum
Albumin is compounded with inulin, and inulin is a kind of functional oligofructose and a kind of soluble dietary fiber, and having improves enteron aisle
Function, body from lacking of proper care and geriatric disease is helpful to preventing,, can be under the cavitation effect of ultrasound due to not charged
Physical bond occurs for protein, therefore, is ultrasonically treated after inulin is added in ovalbumin dispersion liquid, can be formed good
Emulsifier, be added oiliness core material when, ovalbumin be adsorbed on oiliness core surfaces formed core-shell structure emulsion droplet when, due to chrysanthemum
Powder molecular weight is small, can enter the gap between protein molecular, under the cavitation of ultrasound, and itself has certain coagulate
Colloidality, so will form fine and close firm shell, to construct stable core-shell structure.This stable core-shell structure is on the one hand
The success rate and stability to embedded object encapsulating can be improved, also further protect the bioactivity of embedded object;On the other hand, table
The smooth no recess in face, shell is thick and solid, and this wall material overwhelming majority reaches slow release effect in small enteric release.
Egg protein concentration is preferably 1.0-1.4%w/w1.2%w/w in the ovalbumin dispersion liquid, the albumen egg
Inulin concentration is 1.0-1.4%w/w in white-inulin solution., the conversion ratio and bioactivity of embedded object can be excessively reduced, and
Increase cost, it is very few to reduce embedding rate, increase the loss of oiliness core material.
Step (2) first carries out magnetic agitation, so that ovalbumin and inulin sufficiently dissolve, then carries out being ultrasonically treated again molten
Mixed solution after solution can make albumen and inulin combine closely under the cavitation of ultrasound in this way, increase its hydrophilic group
With the number of hydrophobic group, therefore its emulsion emulsifiers is improved, the preferably described magnetic agitation frequency is 30-40rpm/min, ultrasound
Intensity of wave is 180-200W/cm2, ultrasonic time is 1.5-2 hours.
The additive amount of the medium oil core material of step (3) mixed solution is preferably 10%w/w, compared to wall material, oiliness core
The additive amount of material is preferably controlled in 10%w/w, the emulsibility and stability of lotion can be excessively reduced, to reduce microcapsule wall material
Quality, the very few loss that will increase wall material raw material increases cost from another point of view.
Colostrum is obtained in step (4) mixed solution elder generation high speed shear, then high pressure microjet homogeneous is multiple, micro- using high pressure
Jet stream confrontation colostrum carry out second emulsifying, come into full contact with emulsifier with oiliness core material, thus reach improve emulsibility and surely
Qualitative purpose.
The oiliness core material, which refers to for liposoluble substance (core material) to be dissolved in oil-based solvent, to be made, the liposoluble substance
(core material) can enumerate curcumin, vitamin D, tocopherol, phytosterol etc., and medium chain triglyceride can be used in the oil-based solvent
The preparation method of three esters, rapeseed oil, peanut oil, corn oil etc., oiliness core material can be with reference to existing state of the art.
The method of the present invention is simple, easy to operate, easily controllable, compound as wall material using ovalbumin and inulin, has and takes
Same synergistic effect can form stable core-shell structure, and had good sustained release effect absorbs beneficial to human consumption, has both health-care effect, embed
Rate, conversion ratio, effective percentage, bioactivity are good.
Detailed description of the invention
Fig. 1 is the encapsulation rate of embedded object in the microcapsules of different inulin additive amounts;
Fig. 2 is embedded object utilization rate in the microcapsules of different inulin additive amounts;
Fig. 3 is the SURFACTANT ADSORPTION amount of the microcapsule wall material of different inulin additive amounts;
Fig. 4 is the absorption that the microcapsules of different inulin additive amounts simulate unsaturated fatty acid in digestion in vitro;
Fig. 5 is the microstructure of the microcapsule wall material of different inulin additive amounts, and wherein Fig. 5 a is the micro- glue of single ovalbumin
The microstructure of cyst wall material;Fig. 5 a is the microstructure that inulin additive amount is 1.0%w/w microcapsule wall material;Fig. 5 c adds for inulin
Dosage is the microstructure of 1.2%w/w microcapsule wall material;Fig. 5 d is that inulin additive amount is the microcosmic of 1.4%w/w microcapsule wall material
Structure.
Specific embodiment
The preparation of oiliness core material:
The preparation of microcapsules core material: 15% (w/v) glutathione aqueous solution is prepared, the triglycerides of phase homogenous quantities is added to
In, 3% (w/w) soybean lecithin is added as emulsifier, the high speed dispersion 4min under 12000r/min is made W/O lotion, obtains
Oiliness core material to glutathione microcapsules core material as following embodiments.
Embodiment 1 is a kind of using ovalbumin and inulin as the novel microcapsule wall material preparation method of wall material, and specific steps are such as
Under:
(1) ovalbumin is soluble in water, ovalbumin dispersion liquid is obtained after carrying out magnetic agitation, makes the ratio of ovalbumin
Example is 1.0%w/w;
(2) inulin is added to the ovalbumin dispersion liquid, the additive amount of inulin is 1.0%w/w, and magnetic agitation frequency is
30rpm/min, ultrasonic intensity 180W/cm2, ultrasonic time is 1 hour.;
(4) oiliness core material is added in the ovalbumin-inulin solution, additional amount 5%w/w, it is molten obtains mixing
Liquid;
(5) ovalbumin-inulin and oiliness core material mixed solution shearing 1min under high speed shear instrument is placed in obtain
To colostrum, revolving speed 20000rpm/min, then in the case where circulating in pressure and being 11kPa, high pressure microjet homogeneous is three times.
It (6) is 170 DEG C in inlet air temperature by the ovalbumin-inulin and triglycerides mixed emulsion, leaving air temp
It is 85 DEG C, under conditions of control feed flow rate is 500ml/h, spray drying obtains microcapsule granule.
Microcapsule wall material is up to 90.32% to the embedding rate of oiliness core material, and surfactant adsorption amount reaches
2.86mg/m2, and the embedded object conversion ratio under this wall material reaches 62.71%, effective percentage reaches 72.39%, bioactivity and reach
45.39%;Burst size is 21.43% in simulate the gastric juice, and burst size is 89.90% in simulated intestinal fluid, and extreme portions are in small intestine
In be digested absorption, small part discharges under one's belt, avoids embedded object from losing activity in severe gastric environment, more protects
Embedded object is digested.
Embodiment 2 is a kind of using ovalbumin and inulin as the novel microcapsule wall material preparation method of wall material, and specific steps are such as
Under:
(1) ovalbumin is soluble in water, ovalbumin dispersion liquid is obtained after carrying out magnetic agitation, makes the ratio of ovalbumin
Example is 1.2%w/w;
(2) inulin is added to the ovalbumin dispersion liquid, the additive amount of inulin is 1.2%w/w, and magnetic agitation frequency is
40rpm/min, ultrasonic intensity 200W/cm2, ultrasonic time is 2 hours.;
(4) oiliness core material is added in the ovalbumin-inulin solution, additional amount 10%w/w, it is molten obtains mixing
Liquid;
(5) ovalbumin-inulin and oiliness core material mixed solution are placed under high speed shear instrument and shear 1.5min
Obtain colostrum, revolving speed 25000rpm/min, then high pressure microjet homogeneous is three times in the case where circulating in pressure and being 12kPa.
It (6) is 190 DEG C in inlet air temperature by the ovalbumin-inulin and triglycerides mixed emulsion, leaving air temp
It is 85 DEG C, under conditions of control feed flow rate is 600ml/h, spray drying obtains microcapsule granule.
Microcapsule wall material is up to 94.16% to the embedding rate of oiliness core material, and surfactant adsorption amount reaches
3.97mg/m2, and the embedded object conversion ratio under this wall material reaches 71.76%, effective percentage reaches 82.31%, bioactivity and reach
59.07%;Burst size is 18.32% in simulate the gastric juice, and burst size is 95.53% in simulated intestinal fluid, and the overwhelming majority is in small intestine
In be digested absorption, few part discharges under one's belt, avoids embedded object from losing activity in severe gastric environment, more protects
Embedded object has been protected to be digested.
Embodiment 3 is a kind of using ovalbumin and inulin as the novel microcapsule wall material preparation method of wall material, and specific steps are such as
Under:
(1) ovalbumin is soluble in water, ovalbumin dispersion liquid is obtained after carrying out magnetic agitation, makes the ratio of ovalbumin
Example is 1.4%w/w;
(2) inulin is added to the ovalbumin dispersion liquid, the additive amount of inulin is 1.4%w/w, and magnetic agitation frequency is
35rpm/min, ultrasonic intensity 190W/cm2, ultrasonic time is 1.5 hours.;
(4) oiliness core material is added in the ovalbumin-inulin solution, additional amount 10%w/w, it is molten obtains mixing
Liquid;
(5) ovalbumin-inulin and oiliness core material mixed solution shearing 3min under high speed shear instrument is placed in obtain
To colostrum, revolving speed 23000rpm/min, then in the case where circulating in pressure and being 13kPa, high pressure microjet homogeneous is three times.
It (6) is 180 DEG C in inlet air temperature by the ovalbumin-inulin and triglycerides mixed emulsion, leaving air temp
It is 90 DEG C, under conditions of control feed flow rate is 600ml/h, spray drying obtains microcapsule granule.
Microcapsule wall material is up to 87.96% to the embedding rate of oiliness core material, and surfactant adsorption amount reaches
3.47mg/m2, and the embedded object conversion ratio under this wall material reaches 69.51%, effective percentage reaches 77.21%, bioactivity and reach
53.67%;Burst size is 24.72% in simulate the gastric juice, and burst size is 92.11% in simulated intestinal fluid, and extreme portions are in small intestine
In be digested absorption, small part discharges under one's belt, avoids embedded object from losing activity in severe gastric environment, more protects
Embedded object is digested.
Comparative example 1
In addition to not adding ovalbumin, remaining is the same as embodiment 2.
Microcapsule wall material is up to 34.12% to the embedding rate of oiliness core material, and surfactant adsorption amount reaches
0.29mg/m2, and the embedded object conversion ratio under this wall material reaches 41.23%, effective percentage reaches 32.32%, bioactivity and reach
13.32%;Burst size is 51.32% in simulate the gastric juice, and burst size is 72.53% in simulated intestinal fluid, and the overwhelming majority is in gastric juice
Middle release, causes embedded object to inactivate, and unfavorable human consumption absorbs.
Comparative example 2
In addition to not adding inulin, remaining is the same as embodiment 2.
Microcapsule wall material is up to 73.12% to the embedding rate of oiliness core material, and surfactant adsorption amount reaches
1.16mg/m2, and the embedded object conversion ratio under this wall material reaches 51.23%, effective percentage reaches 62.32%, bioactivity and reach
31.92%;Burst size is 41.32% in simulate the gastric juice, and burst size is 68.53% in simulated intestinal fluid, and significant portion is in gastric juice
Middle release, causes embedded object to inactivate, and unfavorable human consumption absorbs.
Fig. 1 is the encapsulation rate of embedded object in the microcapsules of different inulin additive amounts, as can be seen from Figure adding when inulin
Dosage is 1.2%w/w, this wall material has highest embedding rate, is made full use of to embedded object;Fig. 2 is different inulin additive amounts
Microcapsules in embedded object utilization rate, as can be seen from Figure when the additive amount of inulin be 1.2%w/w, the conversion ratio of this wall material,
Efficient and bioactivity highest guarantees that embedded object is absorbed by the body with best activity;Fig. 3 is micro- glue of different inulin additive amounts
The SURFACTANT ADSORPTION amount of cyst wall material, as can be seen from Figure when the additive amount of inulin is 1.2%w/w, this wall material has most
Big surface excess consolidates shell core thick and solid, and embedded object is largely protected not caused to inactivate by external condition influence;Fig. 4
It is that the microcapsules of different inulin additive amounts simulate the absorption of unsaturated fatty acid in digestion in vitro, works as chrysanthemum as can be seen from Figure
The additive amount of powder is 1.2%w/w, and the embedded object overwhelming majority of this wall material is digested absorption in small intestine, and few part is under one's belt
Release, avoids embedded object from losing activity in severe gastric environment, more embedded object is protected to be digested;Figure
5 be the microstructure of the microcapsule wall material of different inulin additive amounts, and wherein Fig. 5 a is the micro- of single ovalbumin microcapsule wall material
See structure;Fig. 5 b is the microstructure that inulin additive amount is 1.0%w/w microcapsule wall material;Fig. 5 c is that inulin additive amount is 1.2%
The microstructure of w/w microcapsule wall material;Fig. 5 d is the microstructure that inulin additive amount is 1.4%w/w microcapsule wall material, by figure
It can be seen that when inulin additive amount be 1.2%w/w, surface is smooth, and shell is firm thick and solid, full grains without recess, and with than
It is compared compared with example 1, ovalbumin-inulin composite micro-capsule wall material has larger in embedding rate, conversion ratio, effective percentage, bioactivity
It improves, and comparative example 1 discharges under one's belt in the overwhelming majority, is unfavorable for absorption of human body.And compared with comparative example 2, ovalbumin-
Inulin composite micro-capsule wall material all improves a lot in conversion ratio, effective percentage, bioactivity, slightly improves on encapsulation rate, and
Comparative example 2 discharges under one's belt in major part, is unfavorable for absorption of human body.Therefore the micro capsule technology letter of preparation of the embodiment of the present invention
Single, core-shell structure is stablized, and had good sustained release effect absorbs beneficial to human consumption, has both health-care effect, embedding rate, conversion ratio, effectively
Rate, bioactivity are good.