CN109907125A - A kind of stability-enhanced micro-encapsulation of pricklyash peel oleoresin and preparation method thereof - Google Patents

A kind of stability-enhanced micro-encapsulation of pricklyash peel oleoresin and preparation method thereof Download PDF

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CN109907125A
CN109907125A CN201910083910.3A CN201910083910A CN109907125A CN 109907125 A CN109907125 A CN 109907125A CN 201910083910 A CN201910083910 A CN 201910083910A CN 109907125 A CN109907125 A CN 109907125A
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oleoresin
encapsulation
micro
pricklyash peel
preparation
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黄国清
肖军霞
张慧慧
郭丽萍
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Qingdao Agricultural University
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Qingdao Agricultural University
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Abstract

The present invention provides a kind of stability-enhanced micro-encapsulation of pricklyash peel oleoresin and preparation method thereof, first by protein after ultraviolet irradiation and ultrasonic treatment, it is mixed under certain condition with chitosan oligosaccharide, Arabic gum again, adjusts mixed solution pH value, be cooled to room temperature after heating;Grape wine skin slag polysaccharide is added in the above reactant, using this mixture as microcapsule wall material, high speed homogenization stirs to form O/W type emulsion after xanthoxylum oleoresin is added, and obtains micro-encapsulation of pricklyash peel oleoresin powder after spray-dried.Micro-encapsulation of pricklyash peel oleoresin powder prepared by the present invention is spherical in shape, good fluidity, smooth surface, softgel shell is fine and close, reduces the chance contacted with the external world, slows down the loss of volatile component in xanthoxylum oleoresin, the oxidation stability of sensitive component is improved, storage period can be obviously prolonged.The invention is simple and feasible, safe and efficient, is suitable for large-scale production.

Description

A kind of stability-enhanced micro-encapsulation of pricklyash peel oleoresin and preparation method thereof
Technical field
The invention belongs to the embedding techniques fields of biological field, and in particular to a kind of stability-enhanced xanthoxylum oleoresin is micro- Capsule and preparation method thereof.
Background technique
Chinese prickly ash (Zanthoxylum Bungeanum Maxim.) belongs to Rutaceae xanthoxylum, has special strong virtue Fragrance, it can be used as flavouring, also have important pharmacological action.Chinese prickly ash is deep joyous by people with its distinctive flavor of hot It meets, has become food processing industry in China some areas, the necessity in catering trade and family's diet.Currently, Chinese prickly ash is main Use form be with pepper grain or it is traditional it is powdered based on.However, effective taste composition cannot be released sufficiently in pepper grain Come, and be not uniformly dispersed in and be seasoned in food or on dish, influences sensory quality of food.In addition, zanthoxylum powder compares table Area is larger, and fragrance is volatile in storage, processing and transportational process, is also easy to absorb moisture in air moldy metamorphism.
Xanthoxylum oleoresin is extracted from Chinese prickly ash in fragrant, taste compound vegetable oil, is chartreuse or yellow oily Liquid has the distinctive fragrance of Chinese prickly ash and numb taste.Xanthoxylum oleoresin had both contained volatility Japan pepper essential oil, also contains and largely is not easy to wave Send out taste composition and pigment, resin and some non-volatile greases and polysaccharide compound.The fragrance of Chinese prickly ash is mainly Chinese prickly ash Essential oil is that a kind of volatile oil contains by the organic compounds such as terpenes and its containing oxygen derivative alcohol, aldehyde, ketone, ester etc. at being grouped as Amount is about 2%-12%, the chemical property less stable in aerobic, illumination, humidity and higher temperature.Containing there are many be in Zanthoxylum essential oil Fragrant ingredient, except as production essence raw material in addition to, contained by certain ingredients also there is physiological function, in pepper volatile oil Xanthoxylin, which has, inhibits platelet aggregation;Piperitone, 1,8- eucalyptus cerebrin, β-phellandrene, linalool etc. have confused flour beetle worm Significant toxicity action;Pepper volatile oil also has bactericidal effect to certain pathomycetes.
Microcapsules technology, be it is a kind of using natural or synthesis high molecular material having polymerization made of solid or liquid Miniature tolerant or packing material the technology of object wall shell.Microcapsules energy Protective substances exempt from it is affected by environment, have covering smell, change Active constituent is isolated in material mass, volume, state or surface property, reduces volatility and toxicity, a variety of works such as control release With.
Many scholars are using Arabic gum, maltodextrin, glycerin monostearate, corn porous starch etc. as cream at present Xanthoxylum oleoresin is prepared into O/W type lotion, is prepared for micro-encapsulation of pricklyash peel oleoresin by spray drying process by agent.These lists When one compound and its simple mixtures are as emulsifier, since the limitation of emulsifying capacity causes O/W type lotion to be easy aggregation, Micro-encapsulation of pricklyash peel oleoresin granular size after spray drying is uneven, and many tiny capsules particles are adhered to large particle surface, There is crack or hole in particle surface, and the integralities of microcapsules, compactness and mobility are bad.This causes microcapsule wall material cannot Enough effectively prevent effective component volatilization and the ability of oxidation limited xanthoxylum oleoresin and oxygen-barrier.
Summary of the invention
The object of the present invention is to provide a kind of stability-enhanced micro-encapsulation of pricklyash peel oleoresin and preparation method thereof, the present invention The micro-encapsulation of pricklyash peel oleoresin powder of preparation is spherical in shape, good fluidity, smooth surface, and capsule shell configuration is fine and close, reduces and the external world The chance of contact slows down the loss of volatile component in xanthoxylum oleoresin, improves the oxidation stability of sensitive component.
To achieve the above object, the present invention, which adopts the following technical solutions, is achieved:
The present invention provides a kind of preparation method of stability-enhanced micro-encapsulation of pricklyash peel oleoresin, it the following steps are included:
(1) protein is mixed first after ultraviolet irradiation and ultrasonic treatment, then with chitosan oligosaccharide and Arabic gum, is dissolved in Water, stirring adjust mixed solution pH, are cooled to room temperature after heating in water bath for reaction;
(2) grape wine skin slag polysaccharide is added in the above reactant, using this mixture as microcapsule wall material, Zanthoxylum essential oil tree is added Rouge, high speed homogenization stirring, forms O/W type emulsion;
(3) the O/W type emulsion is spray-dried up to micro-encapsulation of pricklyash peel oleoresin.
Further: protein is in soybean protein isolate, grape pip albumen or corn protein powder in the step (1) One or more, protein irradiates 30-60min under the ultraviolet radiator of vertical range 20W at 20cm.
Further: the grape wine skin slag polysaccharide is made by following preparation method: weighing grape wine skin slag, water is added Extraction filters;Extracting solution is concentrated in vacuo to the 1/10 of original volume, ethyl alcohol is then added and staticly settles, centrifugation obtains Thick many candies; De- albumen, washes Thick many candies with the multiple alcohol of ethyl alcohol to remove partial pigment, then carry out decolorization with macroreticular resin, is concentrated, dialysis Freeze-drying obtains the grape wine skin slag polysaccharide after desalination.
Further: the grape pip albumen is made by following preparation method: grape pip is crushed, is sieved, removing oil Rouge extracts at 85 DEG C by grape pip powder and petroleum ether according to mass volume ratio 1:8, the petroleum ether in grape pip powder is volatilized Obtain defatted grape seed powder;The defatted grape seed powder is weighed, NaOH is added by solid-liquid ratio 1:10, constant temperature mentions at 50 DEG C It takes, is centrifuged, then sediment is collected by centrifugation, vacuum freeze drying obtains institute with HCl tune pH to isoelectric point with precipitating proteins State grape pip albumen.
Further: the protein in the step (1) after ultraviolet irradiation is dissolved in distilled water, then again in 500W 30-60min is handled under ultrasonic power.
Further: the mass ratio of protein and chitosan oligosaccharide is 1:2-8:2, chitosan oligosaccharide and Arab in the step (1) The mass ratio of glue is 2:1-2:8.
It is further: the quality of solid content in the protein, chitosan oligosaccharide, Arabic gum mixed solution in the step (1) Volume by volume concentration is 0.96%-3.50%, pH 3.0-5.0.
It is further: mixed solution heating water bath 4-12h at 80-100 DEG C in the step (1).
Further: the grape wine skin slag polysaccharide being added in the step (2) accounts for the 3.3%-20.0% of general wall material amount, always Wall material mass volume ratio concentration is 1.0%-4.0%.
Further: the mass ratio of the xanthoxylum oleoresin and wall material that are added in the step (2) is 1:1-1:5, and high speed is Matter emulsification condition is 30-60 DEG C, 10000-14000r/min emulsifies 10-30min.
The present invention also provides the preparation methods, and stability-enhanced micro-encapsulation of pricklyash peel oleoresin is made.
Further: the embedding rate of xanthoxylum oleoresin is 62.1%-75.6% in the microcapsules, and xanthoxylin content is 6.3%-8.7%, average grain diameter is at 6.1-12.8 μm, and at 29-36 °, mobility is fine at angle of repose;Grease accelerated oxidation at 65 DEG C When testing 21 days, the peroxide value for the xanthoxylum oleoresin not embedded is 42.6mmol/kg, and the micro-encapsulation of pricklyash peel oleoresin mistake Oxidation number is 9.8-15.1mmol/kg.
Compared with prior art, the advantages and positive effects of the present invention are:
1, the prior art is all made of single compound and its simple mixtures as emulsifier, manufactured O/W type Zanthoxylum essential oil tree Fat liquor is easy aggregation, and the micro-encapsulation of pricklyash peel oleoresin granular size after spray drying is uneven, and many tiny capsules particles are viscous It is attached to large particle surface, causes the application range of micro-encapsulation of pricklyash peel oleoresin powder also than relatively limited.
And the present invention uses ultraviolet irradiation protein powder, is modified to the surface functional group of protein to improve its water solubility And dispersibility;The higher structure that protein is opened followed by the cavitation effect that ultrasonic wave generates, becomes the structure of protein It is more loose and expose active subunits or non-polar group and increase its water dispersible and emulsibility;Chitosan oligosaccharide is recycled both may be used With with protein, and can with Arabic gum occur Maillard reaction property, by high-temperature heating reaction form combination product, Finally using with the mixed product of grape wine skin slag polysaccharide as emulsifier, the O/W type xanthoxylum oleoresin emulsion particle diameter size of formation It is uniform, it is evenly distributed, overcomes and use single protein or polysaccharide and its simple mixtures for emulsifier preparation in the prior art Microcapsule emulsion be easy aggregation, the problems such as particle size is uneven.
2, it is existing when preparing micro-encapsulation of pricklyash peel oleoresin in order to avoid the limited emulsifying capacity of single emulsifier the problem of, It needs additionally to add artificial synthesized emulsifier just the fully emulsified of the pre-prepared liquid that can guarantee microcapsules toward contact, will affect in this way The edible safety of microcapsule product.At the same time, during preparing stable emulsion, can also generate existing wall material with The compatibility of core material is bad, and result causes the quality of product not high, and the advantage for eventually leading to microcapsules does not embody all Come.
The present invention handles protein using ultraviolet irradiation and ultrasonic synergistic, can significantly improve its with chitosan oligosaccharide, I Primary glue and the extent of reaction between any two are to form macromolecule reactant, then are formed with natural grape wine skin slag polysaccharide mixed Conjunction object is emulsifier, is adsorbed on O/W type emulsion droplet surface and forms the thick fine and close film of comparison, the xanthoxylum oleoresin of preparation Microcapsules edible safety, good biocompatibility avoid fragrance component in xanthoxylum oleoresin from volatilizing;Simultaneously by xanthoxylum oleoresin and sky Air bound is exhausted, improves the oxidation stability of micro-encapsulation of pricklyash peel oleoresin.The present invention is wrapped without adding any artificial synthetic emulsifier Rate height is buried, operating procedure is easy, assigns xanthoxylum oleoresin powder good water-soluble, dispersibility, stability.
3, it is needed to improve micro-encapsulation of pricklyash peel oleoresin particle diameter distribution uniformity using high-pressure homogeneous in existing technology Ultrasound several times, increases the process and production cost of microcapsules preparation to machine continuous homogenizing so several times or in ultrasonic device.This Invention operating procedure is easy, and only needs to control specific ultraviolet irradiation, ultrasonic treatment and emulsification condition, and it is special not need The micro-encapsulation of pricklyash peel oleoresin particle diameter distribution of reagent and equipment, production is uniform, and water dispersible is good, and flexibility (adaptability) of operation is good, can be directly It is added in conditioning food.Simple production process of the present invention is easy, safe and efficient, is easy to large-scale production.
After a specific embodiment of the invention is read in conjunction with the figure, the other features and advantages of the invention will become more clear Chu.
Detailed description of the invention
Fig. 1 is the preparation technology flow chart of micro-encapsulation of pricklyash peel oleoresin in the present invention.
Fig. 2 is micro-encapsulation of pricklyash peel oleoresin lotion prepared by embodiment 2.
Fig. 3 is micro-encapsulation of pricklyash peel oleoresin SEM figure prepared by embodiment 2.
Specific embodiment
Technical solution of the present invention is further described in detail with reference to the accompanying drawings and examples.
Grape pip albumen used in the present invention is made by following preparation method: grape pip being crushed by pulverizer, mistake 40 meshes.Using soxhlet extraction methods removing grease, the mass volume ratio example of grape pip powder and petroleum ether is 1:8 (g/mL), 6 h are extracted at 85 DEG C, the petroleum ether in grape pip powder is volatilized, and are dried rear spare.200g defatted grape seed powder is weighed, by material Liquor ratio 1:10(g/mL) 1mol/L NaOH is added, constant temperature extracts 1h at 50 DEG C, and 4000r/min is centrifuged 20min, then uses For 1mol/LHCl tune pH to isoelectric point with precipitating proteins, 4000r/min is centrifuged 20min, collects sediment, vacuum freeze drying Obtain 11.6g grape pip protein.
Grape wine skin slag polysaccharide used in the present invention is made by following preparation method: weighing 200g dry white wine skin Slag is added distilled water according to mass volume ratio 1:10 ratio and extracts 4h at 100 DEG C, filters, and filter residue repeats to extract 2 times, merges Filtrate;Extracting solution is concentrated in vacuo to 1/10 or so of original volume on a rotary evaporator, then in mass volume ratio 1:4 ratio 95% ethyl alcohol is added and staticly settles 12h at 4 DEG C, 4000r/min centrifugation 20min obtains Thick many candies;Sevag method takes off albumen 9 times, Thick many candies are washed with the multiple alcohol of 70% ethyl alcohol to remove partial pigment, then carry out decolorization with the macroreticular resin of HPD300, be concentrated, Freeze-drying obtains 5.2g grape wine skin slag polysaccharide after dialysis desalination.
Embodiment 1
As shown in Figure 1, the preparation method of micro-encapsulation of pricklyash peel oleoresin described in the present embodiment specifically includes the following steps:
1, the 20W quartz burner inside superclean bench is opened into preheating 20min, stablizes light wave in 253.7nm.By corn Albumen powder is laid in the glass culture dish that diameter is 9cm, is then placed under vertical range ultraviolet radiator at 20cm and is irradiated 30min。
2, corn protein powder 15.0g processed above is weighed, 250mL distilled water is added, magnetic stirrer 1h matches Be set to 6.0%(w/v) suspension.After handling 30min under the ultrasonic power of 500w, 4000r/min is centrifuged 10min removal not Molten object, is prepared 2.0%(w/v) corn protein powder solution.
3, then zein, chitosan oligosaccharide and Arabic gum 1:2:8 in mass ratio are mixed, dissolution is scattered in 500mL steaming Distilled water, holding total solid concentration are 0.96%(w/v), magnetic stirrer 12h is uniformly mixed it.Adjust mixed solution PH to 3.0 is cooled to room temperature after 80 DEG C of heating water bath 4h.
4,0.2g grape wine skin slag polysaccharide (the 4.0% of the total wall material of mass percent Zhan) is added in above-mentioned reaction solution again, stirs Mix uniformly mixed, total wall material concentration reaches 1.0%(w/v in mixture).Using this mixture as wall material, 5.0g Zanthoxylum essential oil tree is added Rouge, holding core wall mass ratio are 1:1, and 30 DEG C, 10000r/min emulsification 10min form O/W type emulsion.
It 5, will be described under conditions of inlet air temperature is 180 DEG C, leaving air temp is 80 DEG C, sample introduction speed is 10mL/min The spray-dried acquisition micro-encapsulation of pricklyash peel oleoresin powder of O/W type emulsion.
The micro-encapsulation of pricklyash peel oleoresin powdered oil embedding rate that the present embodiment is prepared under this condition is 62.1%, xanthoxylin Content is 6.3%, and angle of repose is 29 °, and average grain diameter is 12.8 μm.Peroxidating when grease accelerated oxidation at 65 DEG C is tested 21 days Value is 15.1mmol/kg, and the peroxide value for the xanthoxylum oleoresin not embedded is 42.6mmol/kg.
Embodiment 2
The preparation method of micro-encapsulation of pricklyash peel oleoresin described in the present embodiment specifically includes the following steps:
1, the 20W quartz burner inside superclean bench is opened into preheating 20min, stablizes light wave in 253.7nm.By grape Seed albumen is laid in the glass culture dish that diameter is 9cm, is then placed under vertical range ultraviolet radiator at 20cm and is irradiated 40min。
2, grape pip protein 15 .0g processed above is weighed, 250mL distilled water is added, magnetic stirrer 1h matches Be set to 6.0%(w/v) suspension.After handling 40min under the ultrasonic power of 500w, 4000r/min is centrifuged 10min removal not Molten object, is prepared 3.0%(w/v) grape pip protein solution.
3, grape pip albumen, chitosan oligosaccharide and Arabic gum 2:2:8 in mass ratio are mixed, dissolution is scattered in 500mL distillation Water, holding total solid concentration are 1.8%(w/v), magnetic stirrer 12h is uniformly mixed it.Adjust mixed solution pH To 3.5, room temperature is cooled to after 90 DEG C of heating water bath 8h.
4,1.0g grape wine skin slag polysaccharide (the 10.0% of the total wall material of mass percent Zhan) is added in above-mentioned reaction solution again, It is uniformly mixed, total wall material concentration reaches 2.0%(w/v in mixture).Using this mixture as wall material, 5.0g Zanthoxylum essential oil is added Resin, holding core wall mass ratio are 1:2, and 40 DEG C, 11000r/min emulsification 15min form O/W type emulsion.
It 5, will be described under conditions of inlet air temperature is 180 DEG C, leaving air temp is 80 DEG C, sample introduction speed is 10mL/min The spray-dried acquisition micro-encapsulation of pricklyash peel oleoresin powder of O/W type emulsion.
The micro-encapsulation of pricklyash peel oleoresin powdered oil embedding rate that the present embodiment is prepared under this condition is 70.9%, xanthoxylin Content is 7.2%, and angle of repose is 31 °, and average grain diameter is 10.9 μm.Peroxidating when grease accelerated oxidation at 65 DEG C is tested 21 days Value is 12.1mmol/kg, and the peroxide value for the xanthoxylum oleoresin not embedded is 42.6mmol/kg.
As shown in Fig. 2, the particle size of micro-encapsulation of pricklyash peel oleoresin lotion manufactured in the present embodiment is uniform, it is evenly distributed, It overcomes and single protein or polysaccharide and its simple mixtures is used to be easy to gather for microcapsules prepared by emulsifier in the prior art Collection, the problems such as particle size is uneven.
As shown in figure 3, micro-encapsulation of pricklyash peel oleoresin powder manufactured in the present embodiment is spherical in shape, and good fluidity, smooth surface, Softgel shell is fine and close, reduces the chance contacted with the external world, slows down Zanthoxylum essential oil oxidation rate, can be obviously prolonged storage phase.
Embodiment 3
The preparation method of micro-encapsulation of pricklyash peel oleoresin described in the present embodiment specifically includes the following steps:
1, the 20W quartz burner inside superclean bench is opened into preheating 20min, stablizes light wave in 253.7nm.By soybean Protein isolate is laid in the glass culture dish that diameter is 9cm, is then placed under vertical range ultraviolet radiator at 20cm and is irradiated 50min。
2, it weighs soybean protein isolate 15.0g processed above, is added 250mL distilled water, magnetic stirrer 1h, Be configured to 6.0%(w/v) suspension.After handling 50min under the ultrasonic power of 500w, 4000r/min is centrifuged 10min removal 4.0%(w/v is prepared in insoluble matter) soybean protein isolate solution.
3, soybean protein isolate, chitosan oligosaccharide and Arabic gum 4:2:6 in mass ratio are mixed, dissolution is scattered in 500mL steaming Distilled water, holding total solid concentration are 2.4%(w/v), magnetic stirrer 12h is uniformly mixed it.Adjust mixed solution PH to 4.0 is cooled to room temperature after 100 DEG C of heating water bath 12h.
4,3.0g grape wine skin slag polysaccharide (the 20.0% of the total wall material of mass percent Zhan) is added in above-mentioned reaction solution again, It is uniformly mixed, total wall material concentration reaches 3.0%(w/v in mixture).Using this mixture as wall material, 5.0g Zanthoxylum essential oil is added Resin, holding core wall mass ratio are 1:3, and 50 DEG C, 12000r/min emulsification 20min form O/W type emulsion.
It 5, will be described under conditions of inlet air temperature is 180 DEG C, leaving air temp is 80 DEG C, sample introduction speed is 10mL/min The spray-dried acquisition micro-encapsulation of pricklyash peel oleoresin powder of O/W type emulsion.
The micro-encapsulation of pricklyash peel oleoresin powdered oil embedding rate that the present embodiment is prepared under this condition is 75.6%, xanthoxylin Content is 8.7%, and angle of repose is 36 °, and average grain diameter is 9.7 μm.Peroxide value when grease accelerated oxidation at 65 DEG C is tested 21 days For 9.8mmol/kg, and the peroxide value for the xanthoxylum oleoresin not embedded is 42.6mmol/kg.
Embodiment 4
The preparation method of micro-encapsulation of pricklyash peel oleoresin described in the present embodiment specifically includes the following steps:
1, the 20W quartz burner inside superclean bench is opened into preheating 20min, stablizes light wave in 253.7nm.By corn Albumen powder is laid in the glass culture dish that diameter is 9cm, is then placed under vertical range ultraviolet radiator at 20cm and is irradiated 60min。
2, corn protein powder 15.0g processed above is weighed, 250mL distilled water is added, magnetic stirrer 1h matches Be set to 6.0%(w/v) suspension.After handling 30min under the ultrasonic power of 500w, 4000r/min is centrifuged 10min removal not Molten object, is prepared 2.0%(w/v) corn protein powder solution.
3, zein, chitosan oligosaccharide and Arabic gum 6:2:4 in mass ratio being mixed, dissolution is scattered in 500mL distilled water, Holding total solid concentration is 1.9%(w/v), magnetic stirrer 12h is uniformly mixed it.Adjust mixed solution pH to 4.5, room temperature is cooled to after 80 DEG C of heating water bath 6h.
4,0.5g grape wine skin slag polysaccharide (the 5.0% of the total wall material of mass percent Zhan) is added in above-mentioned reaction solution again, stirs Mix uniformly mixed, total wall material concentration reaches 2.0%(w/v in mixture).Using this mixture as wall material, 2.5g Zanthoxylum essential oil tree is added Rouge, holding core wall mass ratio are 1:4, and 60 DEG C, 13000r/min emulsification 25min form O/W type emulsion.
It 5, will be described under conditions of inlet air temperature is 180 DEG C, leaving air temp is 80 DEG C, sample introduction speed is 10mL/min The spray-dried acquisition micro-encapsulation of pricklyash peel oleoresin powder of O/W type emulsion.
The micro-encapsulation of pricklyash peel oleoresin powdered oil embedding rate that the present embodiment is prepared under this condition is 65.4%, xanthoxylin Content is 6.7%, and angle of repose is 34 °, and average grain diameter is 8.6 μm.Peroxide value when grease accelerated oxidation at 65 DEG C is tested 21 days For 14.5mmol/kg, and the peroxide value for the xanthoxylum oleoresin not embedded is 42.6mmol/kg.
Embodiment 5
The preparation method of micro-encapsulation of pricklyash peel oleoresin described in the present embodiment specifically includes the following steps:
1, the 20W quartz burner inside superclean bench is opened into preheating 20min, stablizes light wave in 253.7nm.By grape Seed albumen is laid in the glass culture dish that diameter is 9cm, is then placed under vertical range ultraviolet radiator at 20cm and is irradiated 50min。
2, grape pip protein 15 .0g processed above is weighed, 250mL distilled water is added, magnetic stirrer 1h matches Be set to 6.0%(w/v) suspension.After handling 40min under the ultrasonic power of 500w, 4000r/min is centrifuged 10min removal not Molten object, is prepared 3.0%(w/v) grape pip protein solution.
3, grape pip albumen, chitosan oligosaccharide and Arabic gum 8:2:2 in mass ratio are mixed, dissolution is scattered in 500mL distillation Water, holding total solid concentration are 2.9%(w/v), magnetic stirrer 12h is uniformly mixed it.Adjust mixed solution pH To 5.0, room temperature is cooled to after 90 DEG C of heating water bath 8h.
4,0.5g grape wine skin slag polysaccharide (the 3.3% of the total wall material of mass percent Zhan) is added in above-mentioned reaction solution again, stirs Mix uniformly mixed, total wall material concentration reaches 3.0%(w/v in mixture).Using this mixture as wall material, 3.0g Zanthoxylum essential oil tree is added Rouge, holding core wall mass ratio are 1:5, and 50 DEG C, 14000r/min emulsification 30min form O/W type emulsion.
It 5, will be described under conditions of inlet air temperature is 180 DEG C, leaving air temp is 80 DEG C, sample introduction speed is 10mL/min The spray-dried acquisition micro-encapsulation of pricklyash peel oleoresin powder of O/W type emulsion.
The micro-encapsulation of pricklyash peel oleoresin powdered oil embedding rate that the present embodiment is prepared under this condition is 68.3%, xanthoxylin Content is 6.9%, and angle of repose is 32 °, and average grain diameter is 6.1 μm.Peroxide value when grease accelerated oxidation at 65 DEG C is tested 21 days For 13.6mmol/kg, and the peroxide value for the xanthoxylum oleoresin not embedded is 42.6mmol/kg.
Embodiment 6
The preparation method of micro-encapsulation of pricklyash peel oleoresin described in the present embodiment specifically includes the following steps:
1, the 20W quartz burner inside superclean bench is opened into preheating 20min, stablizes light wave in 253.7nm.By soybean Protein isolate is laid in the glass culture dish that diameter is 9cm, is then placed under vertical range ultraviolet radiator at 20cm and is irradiated 50min。
2, it weighs soybean protein isolate 15.0g processed above, is added 250mL distilled water, magnetic stirrer 1h, Be configured to 6.0%(w/v) suspension.After handling 60min under the ultrasonic power of 500w, 4000r/min is centrifuged 10min removal 4.0%(w/v is prepared in insoluble matter) soybean protein isolate solution.
3, soybean protein isolate, chitosan oligosaccharide and Arabic gum 8:2:1 in mass ratio are mixed, dissolution is scattered in 500mL steaming Distilled water, holding total solid concentration are 3.5%(w/v), magnetic stirrer 12h is uniformly mixed it.Adjust mixed solution PH to 5.0 is cooled to room temperature after 100 DEG C of heating water bath 10h.
4,2.5g grape wine skin slag polysaccharide (the 12.5% of the total wall material of mass percent Zhan) is added in above-mentioned reaction solution again, It is uniformly mixed, total wall material concentration reaches 4.0%(w/v in mixture).Using this mixture as wall material, 6.7g Zanthoxylum essential oil is added Resin, holding core wall mass ratio are 1:3, and 40 DEG C, 12000r/min emulsification 30min form O/W type emulsion.
It 5, will be described under conditions of inlet air temperature is 180 DEG C, leaving air temp is 80 DEG C, sample introduction speed is 10mL/min The spray-dried acquisition micro-encapsulation of pricklyash peel oleoresin powder of O/W type emulsion.
The micro-encapsulation of pricklyash peel oleoresin powdered oil embedding rate that the present embodiment is prepared under this condition is 73.8%, xanthoxylin Content is 7.9%, and angle of repose is 30 °, and average grain diameter is 10.3 μm.Peroxidating when grease accelerated oxidation at 65 DEG C is tested 21 days Value is 11.4mmol/kg, and the peroxide value for the xanthoxylum oleoresin not embedded is 42.6mmol/kg.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than is limited;Although referring to aforementioned reality Applying example, invention is explained in detail, for those of ordinary skill in the art, still can be to aforementioned implementation Technical solution documented by example is modified or equivalent replacement of some of the technical features;And these are modified or replace It changes, the spirit and scope for claimed technical solution of the invention that it does not separate the essence of the corresponding technical solution.

Claims (10)

1. a kind of preparation method of stability-enhanced micro-encapsulation of pricklyash peel oleoresin, it is characterised in that it the following steps are included:
(1) protein is mixed first after ultraviolet irradiation and ultrasonic treatment, then with chitosan oligosaccharide and Arabic gum, is dissolved in Water, stirring adjust mixed solution pH, are cooled to room temperature after heating in water bath for reaction;
(2) grape wine skin slag polysaccharide is added in the above reactant, using this mixture as microcapsule wall material, Zanthoxylum essential oil tree is added Rouge, high speed homogenization stirring, forms O/W type emulsion;
(3) the O/W type emulsion is spray-dried up to micro-encapsulation of pricklyash peel oleoresin.
2. the preparation method of micro-encapsulation of pricklyash peel oleoresin according to claim 1, it is characterised in that egg in the step (1) White matter is one of soybean protein isolate, grape pip albumen or corn protein powder or a variety of, and protein is vertical range 20W's 30-60min is irradiated under ultraviolet radiator at 20cm.
3. the preparation method of micro-encapsulation of pricklyash peel oleoresin according to claim 1, it is characterised in that the grape wine skin slag Polysaccharide is made by following preparation method: weighing grape wine skin slag, flooding is added, filter;Extracting solution is concentrated in vacuo to original Then the 1/10 of volume is added ethyl alcohol and staticly settles, centrifugation obtains Thick many candies;De- albumen, with the multiple alcohol of ethyl alcohol wash Thick many candies with Partial pigment is removed, then carries out decolorization with macroreticular resin, is concentrated, vacuum freeze drying obtains the grape after desalination of dialysing Wine skin slag polysaccharide.
4. the preparation method of micro-encapsulation of pricklyash peel oleoresin according to claim 1, it is characterised in that warp in the step (1) Protein after crossing ultraviolet irradiation is dissolved in distilled water, then handles 30-60min under 500W ultrasonic power again.
5. the preparation method of micro-encapsulation of pricklyash peel oleoresin according to claim 1, it is characterised in that egg in the step (1) The mass ratio of white matter and chitosan oligosaccharide is 1:2-8:2, and the mass ratio of chitosan oligosaccharide and Arabic gum is 2:1-2:8.
6. the preparation method of micro-encapsulation of pricklyash peel oleoresin according to claim 1, it is characterised in that in the step (1) Protein, chitosan oligosaccharide, the mass volume ratio concentration of solid content is 0.96%-3.50%, pH 3.0- in Arabic gum mixed solution 5.0。
7. the preparation method of micro-encapsulation of pricklyash peel oleoresin according to claim 1, it is characterised in that add in the step (2) The grape wine skin slag polysaccharide entered accounts for the 3.3%-20.0% of general wall material amount, and general wall material amount volume by volume concentration is 1.0%-4.0%.
8. micro-encapsulation of pricklyash peel oleoresin preparation method according to claim 1, it is characterised in that be added in the step (2) Xanthoxylum oleoresin and wall material mass ratio be 1:1-1:5, high speed homogenization emulsification condition be 30-60 DEG C, 10000-14000r/ Min emulsifies 10-30min.
9. stability-enhanced micro-encapsulation of pricklyash peel oleoresin is made in the described in any item preparation methods of claim 1-8.
10. micro-encapsulation of pricklyash peel oleoresin according to claim 8, it is characterised in that xanthoxylum oleoresin in the microcapsules Embedding rate be 62.1%-75.6%, xanthoxylin content be 6.3%-8.7%, at 6.1-12.8 μm, angle of repose exists average grain diameter 29-36 °, mobility is fine;Grease accelerated oxidation at 65 DEG C micro-encapsulation of pricklyash peel oleoresin peroxide value when testing 21 days For 9.8-15.1mmol/kg.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111632564A (en) * 2020-06-11 2020-09-08 上海应用技术大学 Polyurethane peppermint oil microcapsule and preparation method thereof
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