CN102742810A - Garlic oil microcapsule with shell made of soybean protein isolate and chitosan and preparation method and application thereof - Google Patents

Garlic oil microcapsule with shell made of soybean protein isolate and chitosan and preparation method and application thereof Download PDF

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CN102742810A
CN102742810A CN2012102498898A CN201210249889A CN102742810A CN 102742810 A CN102742810 A CN 102742810A CN 2012102498898 A CN2012102498898 A CN 2012102498898A CN 201210249889 A CN201210249889 A CN 201210249889A CN 102742810 A CN102742810 A CN 102742810A
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protein isolate
soybean protein
garlic oil
shitosan
wall material
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CN102742810B (en
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肖军霞
黄国清
孙燕婷
王世清
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Qingdao Agricultural University
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Abstract

The invention provides a garlic oil microcapsule with a shell made of soybean protein isolate and chitosan and a preparation method and application thereof. The preparation method includes making the soybean protein isolate, the chitosan and garlic oil into uniform emulsion; adjusting pH of the emulsion to 6.5, mixing to obtain microcapsule suspension, adjusting pH again to 6.0, adding glutamine transaminase, mixing to solidify the microcapsule, washing to collect wet microcapsule, and vacuum-freezing and drying to obtain the solid microcapsule, wherein mass ratio of the soybean protein isolate and the chitosan is 4:1 and mass ratio of a core and the shell is 1:1-1:4. The garlic oil microcapsule is obtained by electrostatic mutual attraction for the chitosan and the soybean protein isolate and embedding of the garlic oil, and accordingly pungent smell of the garlic oil can be covered, loss of diallyl sulfides in the garlic oil can also be avoided in food processing, and stability of the garlic oil is improved. Application of the garlic oil to the food industry is broadened.

Description

A kind of is the garlic oil microcapsules of wall material with soybean protein isolate and shitosan
Technical field
The invention belongs to the microcapsules technology field, being specifically related to a kind of is the garlic oil microcapsules of wall material with soybean protein isolate and shitosan.
Background technology
Garlic is a kind of spice that is loved by the people, and has been widely applied in the middle of the food such as flavoring, meat products.The main flavor components of garlic is a sulfur-containing compound, and these compositions are to thermally labile, in process, very easily decomposes and makes garlic lose its acid originally.Garlic oil is the active ingredient that from garlic, extracts, and except that the acid with garlic, also has anti-inflammation, improves immunity of organisms, Prevention of Cardiovascular systemic disease, cancer-resisting and the anti-ageing effect of waiting for a long time.Because the solubility of garlic oil in water is very low; And has special pungent acid; Contained main component allyl sulfide ether compound is unstable in the garlic oil in addition; Highly volatile and be subject to the influence of pH, light, heat and oxygen and go bad in processing and transporting procedures, these have all greatly limited it in Application in Food Industry.
The garlic flavor food of selling in the market is mashed garlic or garlic oil directly to be added in the raw material process, and loses desired local flavor and mouthfeel but the sulfur-containing compound in the garlic can change in storage and process or decompose.If can be pulverulence through the microencapsulation technical transform with garlic oil, not only its penetrating odor can be covered, and the storage-stable of garlic oil can be significantly improved, this is significant in the Application in Food Industry scope for enlarging garlic oil.
Microcapsules technology has been widely used in the embedding of vitamin, grease, pigment and spice etc.; These products have been added in the numerous food such as milk powder, chewing gum, instant beverage, can change states of matter, protection sensitive composition, the release of control local flavor, shelter bad flavor and delay food spoilage etc.Research about garlic oil capsule preparation technology has CN101804145A (a kind of garlic oil enteric pellet capsule and preparation method thereof), CN1107341A (compound garlic oil capsule and production method thereof), CN1448129A (allicin and garlic oil cyclodextrine derivative clathrate and preparation method thereof) etc.; But be to be applied to field of medicaments mostly; And just the garlic oil of liquid state is coated; Protect the active ingredient of garlic oil to a certain extent and isolated pungent smell; Also have certain toxicity but coat raw material, be inappropriate for food industry and adopt.Therefore, utilizing the edibility raw material to take the embedding garlic oil is the emphasis of studying at present.
Complex coacervation is a kind of important Microencapsulation Method, and it utilizes two kinds of purposes that reach the embedding core with the electrostatic interaction between the polyelectrolyte of different electric charges.The microcapsules cyst membrane that multiple cohesion forms is fine and close, and can obtain different sustained release performances through controlled condition, so complex coacervation is compared with other microcapsules technology and had remarkable advantages.Complex coacervation has been used to the embedding of essence, fish oil, vitamin and anticorrisive agent etc.
Shitosan is a kind of polysaccharide of positively charged because it self has good adsorptivity, film forming and biocompatibility, and nontoxic, harmless, be easy to biodegradation, be widely used in the microencapsulation of medicine, food, cosmetics etc.Soybean protein isolate then is a kind of wide material sources, cheap phytoprotein, has good emulsifying property, water-retaining property, foaminess and gelation, is widely used in the varieties of food items as a kind of raw material.
At present relevant for adopting blending method to prepare the research report of the compound edible film of soybean protein isolate-shitosan; This type of edible film is mainly used in meat products processing and aspects such as fresh-keeping, preserving fruit and vegetable utilizing and packaging for foodstuff, and functional characteristics such as its tensile strength of more single soy protein isolate film and chitosan film, elongation at break are obviously raising all.Soybean protein isolate is electronegative more than isoelectric point (pH4.5-4.8), thereby realizes microencapsulation around can overlaying on core with positively charged shitosan generation electrostatic interaction coherent packet under the acid condition.Also do not find to adopt soybean protein isolate and shitosan to prepare the research report of garlic oil microcapsules through complex coacervation as the wall material at present.
Summary of the invention
To the problems referred to above that run in the garlic oil capsule preparation in the prior art, the invention provides a kind of is the garlic oil microcapsules of wall material with soybean protein isolate and shitosan.The present invention adopts soybean protein isolate and shitosan as microencapsulation wall material, and garlic oil prepares the garlic oil microcapsules as core through complex coacervation, with the penetrating odor of covering garlic oil and the stability that improves garlic oil.Said garlic oil microcapsules can be used as flavoring to be added in meat products, instant food and the conditioning food etc., in process, has good stable property, can remedy the deficiency of direct interpolation mashed garlic or garlic oil technology.
For realizing the foregoing invention purpose, the present invention adopts following technical proposals to be achieved:
A kind of is the method that the wall material prepares the garlic oil microcapsules with soybean protein isolate and shitosan, and it may further comprise the steps:
(1) the preparation soybean protein isolate aqueous solution is solvent preparing chitosan solution with the acetum;
(2) garlic oil is joined in the soybean protein isolate solution; Mix with chitosan solution then; With soybean protein isolate and shitosan is the wall material, is core with the garlic oil, and the mass ratio that keeps soybean protein isolate and shitosan is that the total solid concentration of 4:1, soybean protein isolate and shitosan is that the mass ratio of 0.5%-2.5% (w/v), core and wall material is 1:1-1:4; 35-55 ℃ of following high speed homogenization forms the emulsion of homogeneous; Regulate pH value to 6.5 and stirring at low speed, the multiple condensed phase that multiple aggregation generation takes place for soybean protein isolate and shitosan is wrapped in the garlic oil surface, forms microcapsule suspensions;
(3) the pH value to 6.0 of adjusting microcapsule suspensions; Amount with 18.75U/ gram soybean protein isolate adds glutamine transaminage, and stirring at low speed is solidified 1h, standing demix; Filter, wash the back and collect wet capsule, obtain solid-state garlic oil microcapsules through vacuum freeze drying.
Further improvement to technique scheme: said step is suspended in soybean protein isolate in the distilled water in (1); Under 50 ℃, 500W ultrasonic power, handle 5min; The centrifugal 10min of 5000r/min removes insoluble matter, adopts distilled water that the supernatant constant volume is obtained the soybean protein isolate aqueous solution; Adopt the acetum preparing chitosan solution of 1% (w/v).
Further improvement to technique scheme: the emulsification condition in the said step (2) refers to emulsification 5min under 4000-8000r/min.
Further improvement to technique scheme: adopt NaOH solution to regulate emulsion pH value to 6.5 in the said step (2), adopt HCl solution to regulate the pH value to 6.0 of microcapsule suspensions in the said step (3).
Further improvement to technique scheme: the stirring at low speed in the said step (2) during microencapsulation refers to stirring 10min under 100-200r/min.
Further improvement to technique scheme: the ratio enzyme of glutamine transaminage is lived and is the 125U/g enzyme preparation in the said step (3).
Further improvement to technique scheme: said step (3) stirs under 45 ℃, 60r/min condition solidifies microcapsules.
It is the garlic oil microcapsules that the wall material prepares that the present invention also provides with soybean protein isolate and shitosan.
It is that the garlic oil microcapsules that the wall material prepares are preparing the garlic flavor Application in Food that the present invention also provides with soybean protein isolate and shitosan.
Compared with prior art, advantage of the present invention and good effect are:
The present invention adopts soybean protein isolate and shitosan as condensing microencapsulation wall material again.The present invention utilizes the ultrasonic Treatment soybean protein isolate, is used for improving the dissolubility and the emulsifying activity of soybean protein isolate.Soybean protein isolate is electronegative more than isoelectric point (pH4.5-4.8).Shitosan is positively charged under acid condition, and has excellent biological compatibility and degradability.The two all be nontoxic, natural, have functional nutriment; Combine the embedding garlic oil through the static adelphotaxy; Multiple cohesion garlic oil microcapsules have been obtained; Both can cover the penetrating odor of garlic oil, can avoid the loss of allyl sulfide ether compound in food processing process in the garlic oil again, thereby can improve the stability of garlic oil; Expand garlic oil in Application in Food Industry, improve people's life.
The glutamine transaminage that the present invention adopts is cured the garlic oil microcapsules; This enzyme can be well and protein generation bridge linking effect; Replace poisonous glutaraldehyde to solidify microcapsules, thereby improved the edibility of microcapsule product, and can prolong the shelf life of product.The present invention has prepared a kind of edible garlic oil microcapsules that condense again, and alternative mashed garlic and garlic oil are used to produce various garlicky food as flavoring.
The present invention also to the garlic oil microcapsules application in sausage study; Sausage to add mashed garlic and garlic oil respectively contrasts, and it is better than the flavour of food products that adds mashed garlic, garlic oil that the subjective appreciation result confirms to add the food of garlic oil microcapsules.
After the advantages specific embodiment of the present invention, other characteristics of the present invention and advantage will become clearer.
Description of drawings
Fig. 1 is the form sketch map of garlic oil used among the present invention.
The form sketch map of the garlic oil microcapsules that Fig. 2 makes for the present invention.
Fig. 3 prepares the process chart of garlic oil microcapsules for soybean protein isolate of the present invention-shitosan complex coacervation.
Fig. 4 is the total ion current figure that GC/MS of the present invention analyzes garlic oil.
Fig. 5 is the total ion current figure that GC/MS of the present invention analyzes the garlic oil microcapsules.
The specific embodiment
Below in conjunction with the accompanying drawing and the specific embodiment technical scheme of the present invention is done further detailed explanation.
Embodiment 1
The technological process of production of garlic oil microcapsule preparation method according to the invention is seen Fig. 1, the wall material that soybean protein isolate and shitosan attract each other and form these microcapsules through static, and garlic oil is as core.
At first prepare the soybean protein isolate aqueous solution: the 4g soybean protein isolate is suspended in the 100mL distilled water; Under 50 ℃, 500W ultrasonic power, handle 5min; The centrifugal 10min of 5000r/min; Remove insoluble matter, employing distilled water to 100mL, promptly obtains the soybean protein isolate solution of 2.67% (w/v) with the supernatant constant volume.
Acetum with 1% (w/v) is the chitosan solution of solvent preparation 2% (w/v) again.
With distilled water 2.67% soybean protein isolate solution is diluted to desired concn before using, the chitosan solution of 2% (w/v) is diluted to desired concn with the acetum of 1% (w/v).In the present embodiment 2.67% soybean protein isolate solution is diluted to 0.8% (w/v), the chitosan solution of 2% (w/v) is diluted to 0.2% (w/v) with the acetum of 1% (w/v).
The garlic oil that 0.2g is commercially available joins in the soybean protein isolate solution of said 0.8% (w/v) of 40mL, and the chitosan solution with 40mL said 0.2% (w/v) mixes then, under 45 ℃, stirs the emulsion that 5min forms homogeneous with 6000r/min; Drip the NaOH solution adjust pH to 6.5 of 10% (w/v) subsequently, under 45 ℃, mix liquid 10min and form microcapsule suspensions with 100r/min; Keep 45 ℃ of temperature; Adopt the HCl solution of 10% (w/v) to regulate microcapsule suspensions pH value to 6.0 then, add glutamine transaminage 6U, stirring at low speed (about 60r/min) 1h; Microcapsules are solidified; Standing demix filters, washes and collect wet capsule, obtains solid-state garlic oil microcapsules through vacuum freeze drying.The efficient of garlic oil microcapsules and productive rate are respectively 45.57% and 32.58% under these process conditions.The efficient and the productive rate of garlic oil microcapsules are calculated as follows:
Figure BDA00001905315600061
Figure BDA00001905315600062
Embodiment 2
In the present embodiment 2.67% soybean protein isolate solution is diluted to 2.4% (w/v), the chitosan solution of 2% (w/v) is diluted to 0.6% (w/v) with the acetum of 1% (w/v).
Respectively that 1.2g, 0.6g and 0.3g is commercially available garlic oil joins in the soybean protein isolate solution of 3 parts of said 2.4% (w/v) of 40mL; Mix with the chitosan solution of 3 parts of 40mL said 0.6% (w/v) respectively then, under 45 ℃, mix the emulsion that liquid 5min forms homogeneous with 6000r/min; Drip the NaOH solution adjust pH to 6.5 of 10% (w/v) subsequently, under 45 ℃, stir 10min and form microcapsule suspensions with 100r/min; Keep 45 ℃ of temperature; Adopt the HCl solution of 10% (w/v) to regulate microcapsule suspensions pH value to 6.0 then, add glutamine transaminage 18U, stirring at low speed (about 60r/min) 1h; Microcapsules are solidified; Standing demix filters, washes and collect wet capsule, obtains solid-state microcapsules through vacuum freeze drying.Microcapsules efficient and productive rate are respectively 58.11% and 61.50%, 69.20% and 64.77%, 49.75% and 59.72% under these process conditions.
Embodiment 3
In the present embodiment 2.67% soybean protein isolate solution is diluted to 2.4% (w/v), the chitosan solution of 2% (w/v) is diluted to 0.6% (w/v) with the acetum of 1% (w/v).
The garlic oil that 0.6g is commercially available joins in the soybean protein isolate solution of said 2.4% (w/v) of 40mL; Chitosan solution with 40mL said 0.6% (w/v) mixes then; Prepare 2 parts of this mixed liquors altogether; Under 35 ℃, mix the emulsion that liquid 5min forms homogeneous with 4000 with 8000r/min respectively, other treatment conditions are with embodiment 2.Microcapsules efficient and productive rate are respectively 53.32% and 58.83%, 54.66% and 58.38% under these process conditions.
Embodiment 4
In the present embodiment 2.67% soybean protein isolate solution is diluted to 2.4% (w/v), the chitosan solution of 2% (w/v) is diluted to 0.6% (w/v) with the acetum of 1% (w/v).
The garlic oil that 0.6g is commercially available joins in the soybean protein isolate solution of said 2.4% (w/v) of 40mL; Chitosan solution with 40mL said 0.6% (w/v) mixes then; Prepare 2 parts of this mixed liquors altogether; Under 35 ℃, 55 ℃, mix the emulsion that liquid 5min forms homogeneous with 6000r/min respectively, other treatment conditions are with embodiment 2.Microcapsules efficient and productive rate are respectively 59.06% and 52.92%, 53.50% and 53.38% under these process conditions.
Embodiment 5
The garlic oil that 1g is commercially available joins in the soybean protein isolate solution of said 2.67% (w/v) of 60mL, and the chitosan solution with 20mL said 2% (w/v) mixes then, under 45 ℃, mixes the emulsion that liquid 5min forms homogeneous with 6000r/min; Drip 10% NaOH (w/v) solution adjust pH to 6.5 subsequently, under 45 ℃, stir 10min and form microcapsule suspensions with 100r/min; Keep 45 ℃ of temperature; Adopt 10% HCl (w/v) solution adjusting microcapsule suspensions pH value to 6.0, add glutamine transaminage 30U, stirring at low speed (about 60r/min) 1h; Microcapsules are solidified; Standing demix filters, washes and collect wet capsule, obtains solid-state microcapsules through vacuum freeze drying.Microcapsules efficient and productive rate are respectively 56.45% and 50.66% under these process conditions.
Garlic oil and the garlic oil microcapsules that adopt preparation method of the present invention to make are analyzed through GC/MS, and its main component changes like table 1, Fig. 4 and shown in Figure 5.The result find after the embedding the garlic main body of oil more not the embedding garlic oil only lost the methacrylic disulfide, kept main active ingredient such as diallyl list thioether in the garlic oil, diallyl disulphide, methyl-2-acrylic trithioether, diallyl trithioether and diallyl four thioethers.
The GC/MS analysis result of table 1 garlic oil and garlic oil microcapsules main component
Figure BDA00001905315600081
Embodiment 6: the garlic oil microcapsules are as the application of flavoring in sausage making
The garlic oil microcapsules are carried out the sausage action oriented research, as contrast, adopt mathematics method that the subjective appreciation result is analyzed with the sausage that adds mashed garlic and garlic oil respectively, concrete steps are following:
With the various batch mixes in the table 2 and stir, adopt manual bowel lavage, the wet intestines of having irritated after the ligation are put into the warm water rinsing several times, the oil slick salting liquor of flush away casing surface attachment etc. dirty thing.Sausage daylight after the washing shines 2~3d down, is put into draughty place hanging 15d maturation then.Steam 10~15min after the meat intestines maturation; With reference to SB/T 102782002 subjective appreciation indexs, adopt mathematics method that the subjective appreciation result is analyzed, the result shows that the sausage that has added the garlic oil microcapsules has typical garlic taste; And garlic perfume (or spice) is soft; Garlic acid is arranged during inlet, and explosive force is strong, and its local flavor and mouthfeel obviously are superior to adding the sausage of mashed garlic and garlic oil.This shows that garlic oil microcapsules among the present invention can be used as flavoring and add in the sausage, replaces mashed garlic or garlic oil to be used to produce garlicky sausage.
Table 2 is made the batching (unit: gram) of garlicky sausage
Figure BDA00001905315600091
Said garlic oil microcapsules both can have been covered the penetrating odor of former garlic oil, can avoid the volatilization of garlic oil active ingredient again, can be used as flavoring and were applied to meat product, instant food and conditioning food etc., particularly were applied in the sausage of garlicky goods.
Above embodiment is only in order to explaining technical scheme of the present invention, but not limits it; Although the present invention has been carried out detailed explanation with reference to previous embodiment, for the person of ordinary skill of the art, still can make amendment to the technical scheme that previous embodiment is put down in writing, perhaps part technical characterictic wherein is equal to replacement; And these modifications or replacement do not make the essence of relevant art scheme break away from the spirit and the scope of the present invention's technical scheme required for protection.

Claims (9)

1. one kind is the method that the wall material prepares the garlic oil microcapsules with soybean protein isolate and shitosan, it is characterized in that it may further comprise the steps:
(1) the preparation soybean protein isolate aqueous solution is solvent preparing chitosan solution with the acetum;
(2) garlic oil is joined in the soybean protein isolate solution; Mix with chitosan solution then; With soybean protein isolate and shitosan is the wall material, is core with the garlic oil, and the mass ratio that keeps soybean protein isolate and shitosan is that the total solid concentration of 4:1, soybean protein isolate and shitosan is that the mass ratio of 0.5%-2.5% (w/v), core and wall material is 1:1-1:4; 35-55 ℃ of following high speed homogenization forms the emulsion of homogeneous; Regulate pH value to 6.5 and stirring at low speed, the multiple condensed phase that multiple aggregation generation takes place for soybean protein isolate and shitosan is wrapped in the garlic oil surface, forms microcapsule suspensions;
(3) the pH value to 6.0 of adjusting microcapsule suspensions; Amount with 18.75U/ gram soybean protein isolate adds glutamine transaminage, and stirring at low speed is solidified 1h, standing demix; Filter, wash the back and collect wet capsule, obtain solid-state garlic oil microcapsules through vacuum freeze drying.
2. according to claim 1 a kind of be the method that the wall material prepares the garlic oil microcapsules with soybean protein isolate and shitosan; It is characterized in that in the said step (1) soybean protein isolate being suspended in the distilled water; Under 50 ℃, 500W ultrasonic power, handle 5min; The centrifugal 10min of 5000r/min removes insoluble matter, with distilled water the supernatant constant volume is obtained the soybean protein isolate aqueous solution; Adopt the acetum preparing chitosan solution of 1% (w/v).
3. according to claim 2 a kind of be the method that the wall material prepares the garlic oil microcapsules with soybean protein isolate and shitosan, it is characterized in that the emulsification condition that forms emulsion in the said step (2) refers to emulsification 5min under 4000-8000r/min.
4. according to claim 1 a kind of be the method that the wall material prepares the garlic oil microcapsules with soybean protein isolate and shitosan; It is characterized in that adopting in the said step (2) NaOH solution to regulate emulsion pH value to 6.5, adopt HCl solution to regulate the pH value to 6.0 of microcapsule suspensions in the said step (3).
5. according to claim 1 a kind of be the method that the wall material prepares the garlic oil microcapsules with soybean protein isolate and shitosan, the stirring at low speed when it is characterized in that microencapsulation in the said step (2) refers to stirring 10min under 100-200r/min.
6. according to claim 1 a kind of be the method that the wall material prepares the garlic oil microcapsules with soybean protein isolate and shitosan, the ratio enzyme that it is characterized in that glutamine transaminage in the said step (3) is lived and is the 125U/g enzyme preparation.
7. according to claim 1 a kind of be the method that the wall material prepares the garlic oil microcapsules with soybean protein isolate and shitosan, it is characterized in that said step (3) stirs under 45 ℃, 60 r/min conditions solidifies microcapsules.
According to claim 1-7 each described a kind of be the garlic oil microcapsules that the wall material prepares with soybean protein isolate and shitosan.
9. according to claim 8 is that the garlic oil microcapsules that the wall material prepares are preparing the garlic flavor Application in Food with soybean protein isolate and shitosan.
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