CN108690206A - A kind of citral pickering emulsion and preparation method thereof that nano-cellulose is stablized - Google Patents
A kind of citral pickering emulsion and preparation method thereof that nano-cellulose is stablized Download PDFInfo
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- CN108690206A CN108690206A CN201810437437.XA CN201810437437A CN108690206A CN 108690206 A CN108690206 A CN 108690206A CN 201810437437 A CN201810437437 A CN 201810437437A CN 108690206 A CN108690206 A CN 108690206A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/09—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
- C08J3/091—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids characterised by the chemical constitution of the organic liquid
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- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
- C08B15/02—Oxycellulose; Hydrocellulose; Cellulosehydrate, e.g. microcrystalline cellulose
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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Abstract
It is that after ammonium persulfate oxidation modification, nano-cellulose suspension is obtained by washing using microcrystalline cellulose as raw material the present invention provides a kind of preparation method for the citral pickering emulsion stablized using nano-cellulose;This suspension is freeze-dried, nano-cellulose powder is obtained;Nano-cellulose powder is scattered in the citric acid-sodium citrate acidic buffer solution that pH is 3, forms nano-cellulose suspension, citral pickering emulsion is obtained by high speed homogenization then to addition citral and medium chain triglyceride in above-mentioned suspension.Citral pickering emulsion prepared by the present invention has the characteristics that nano-cellulose dosage is few, preparation process is simple and application cost is low, can effectively improve the stability of citral under acid condition, delay its degradation.
Description
Technical field
The invention belongs to field of food chemical industry, are related to a kind of citral pickering emulsion, specifically a kind of Nanowire
The citral pickering emulsion and preparation method thereof that dimension element is stablized.
Background technology
Citral is a kind of fat-soluble, volatile open chain monoterpene, is primarily present in litsea citrate oil and lemon-grass oil
In, it is a kind of natural perfume material with broad prospect of application, and synthesize one of the important source material of fine perfumery, distinctive lemon
Lemon fragrance can bring pleasant fresh feel to people, and therefore, citral is commonly used for the seasoning of the food such as beverage, cake, flavouring,
It can also be used for modulation citrus oils, lemon oil and lemon extract.Meanwhile citral is also a kind of antiseptic and natural anticorrosion of wide spectrum
Agent.
But there are carbonyls and double bond in lemon aldehyde structure, and it is anti-that the chemistry such as condensation, addition, oxidation and cyclisation easily occurs
It answers.Especially under acidic environment, its degradation reaction speed can be accelerated, many odorous compounds beastly are generated, cause
The loss of Fresh Lemon breath.And most of orange class fruit drink is acidity, this property of citral seriously constrains it
In the application of beverage and fragrance industry.
In food processing technology, the carrier systems based on lotion are widely used, can by lotion delivery system
Functional nutrient ingredient in package, protection and release food improves product to make it be not easy to be aoxidized during preservation
Flavor quality and nutritional quality extend its shelf life.Oil-in-water emulsion, nanoemulsions and multilayer emulsion are mostly used to lemon at present
Aldehyde is embedded.But phenomena such as these lotions are dynamic stabilization system, and long term storage is easy to happen aggregation and layering.
Pickering emulsion refers to by the New Emulsion of solid particle stabilized emulsion system, and stable mechanism is that solid particle exists
Oil-water interfaces formed Irreversible Adsorption, to formed space steric effect hinder drop between coalescence, meanwhile, solid particle it
Between mutually the tangle network structure of formation increase emulsion intercalation method to a certain extent.Stablize with Small molecular surfactant
Lotion compare, which there is resistant to aggregation, deflocculation, anti-Ovshinsky to be melted into the advantages such as ripe and stability is good.In recent years, some are eaten
Solid particle of grade such as polysaccharide, protein etc. has been demonstrated to be used for stablizing pickering emulsion.These solid particles due to
The good characteristics such as its recyclability, sustainability, biodegradability and biocompatibility can be used as conveying bioactivity
The carrier of substance, it may also be used for cladding unstable compound.Using nano-cellulose as Solid particle emulsifying agents, by high speed
Matter prepares citral pickering emulsion, and nano-cellulose is arranged closely in oil-water interfaces, improves the stability of citral, should
Method has many advantages, such as that preparation process is simply and at low cost, and stability of emulsion is strong, and citral under acid condition can be effectively relieved
Degradation rate.At present using nano-cellulose as Solid particle emulsifying agents, the correlative study of citral pickering emulsion is prepared still
It does not report.
Invention content
For above-mentioned technical problem in the prior art, the present invention provides the citral skins that a kind of nano-cellulose is stablized
Crin lotion and preparation method thereof, the citral pickering emulsion and preparation method thereof that this nano-cellulose is stablized are wanted
Solve that citral in the prior art is degradable in acid condition, the technical problem of stability difference.
The present invention provides a kind of preparation methods for the citral pickering emulsion that nano-cellulose is stablized, including following step
Suddenly:
1)One the step of preparing ammonium persulfate aqueous solution;
It dissolves ammonium persulfate into deionized water, stirring forms ammonium persulfate aqueous solution, in the over cure until fully dissolving
In sour aqueous ammonium, a concentration of 0.5 ~ 2mol/L of the ammonium persulfate;
2)One the step of preparing nano-cellulose suspension;
It weighs microcrystalline cellulose and is added to step 1)In obtained ammonium persulfate aqueous solution, in rotating speed 1000r/min magnetic agitations
Under, it is put into 60 DEG C of water-bath constant temperature and stirs 4 ~ 16h, fully after reaction, stopping agitating and heating obtaining nano-cellulose suspension;
The material ratio of microcrystalline cellulose and ammonium persulfate aqueous solution is 1 ~ 2.5 gram:1L;
3)One the step of preparing nano-cellulose powder;
By step 2)Obtained nano-cellulose suspension is centrifuged at 10000rpm, removes the complete ammonium persulfate of unreacted, from
The heart at least twice, until suspension pH be 7;Precooling 4h, then exists under the conditions of suspension after having centrifuged is placed in -70 DEG C
Condenser temperature is -70 DEG C, vacuum degree is freeze-dried for 24 hours under the conditions of being 5Pa, obtains nano-cellulose powder;
4)One the step of preparing citral pickering emulsion;
By step 3)Obtained nano-cellulose powder is dissolved in the citric acid-sodium citrate buffer solution that pH is 3, is sufficiently stirred
Afterwards, obtain nano-cellulose suspension, in the nano-cellulose suspension, the nano-cellulose a concentration of 4 ~
Lemon is added dropwise by mass-volume concentration in nano-cellulose suspension under 10000 ~ 19000rpm high speed homogenizations in 10g/L
The mass volume ratio of lemon aldehyde and medium chain triglyceride, the citral and nano-cellulose suspension is 0.5 ~ 2g:100ml,
The medium chain triglyceride citral and be 0.5 ~ 2g with the mass volume ratio of nano-cellulose suspension:100ml, high speed is
The matter time is 2 ~ 5min, obtains citral pickering emulsion.
A kind of citral pickering emulsion of the present invention is using nano-cellulose as Solid particle emulsifying agents, and citral is in
Chain triglyceride is oil phase, after the lotion is stored 14 days at 40 DEG C, in lotion the retention rate of citral up to 40.48 ~
55.31%。
The present invention after ammonium persulfate oxidation modification, is received by washing using commercially available microcrystalline cellulose as raw material
Rice cellulose suspension;This suspension is freeze-dried, nano-cellulose powder is obtained;Nano-cellulose powder is scattered in pH
In 3 citric acid-sodium citrate acidic buffer solution, to form nano-cellulose suspension, add then in above-mentioned suspension
Enter citral and medium chain triglyceride, by high speed homogenization, obtains citral pickering emulsion.
Cellulose is that nature contains abundant renewable resource, cheap and easy to get, environmentally safe, have low-density,
The properties such as Environmental Sustainability, adjustability and low cost, and there is reproducible advantage.Microcrystalline cellulose is the one of cellulose
Kind important derivatives, are obtained through acidolysis or mechanical treatment by native cellulose, have large specific surface area, high-hydroscopicity and pole
The good characteristics such as good mobility, can be used as emulsifier and anti-agglomerating agent.But microcrystalline cellulose have it is stronger it is intermolecular and
Intramolecular active force, causes it to be insoluble in water, this property greatly limits its emulsifiability.It is modified through ammonium persulfate
Nano-cellulose has the advantageous properties such as higher surface-active, higher length-width ratio and high intensity, is to stablize pickering emulsion
Ideal emulsified material.
The present invention is compared with prior art, and technological progress is significant.Citral pickering emulsion prepared by the present invention,
Grain size is small and particle diameter distribution is uniform, and nano-cellulose is arranged closely in oil-water interfaces, and Irreversible Adsorption shape occurs in oil-water interfaces
At stable lotion, it is effectively prevent emulsion polymerization and Ostwald ripening, after lotion is stored 14 days at 40 DEG C, citral in lotion
Retention rate is up to 40.48 ~ 55.31%, and under same condition of storage, citral retention rate is only 0.95% in blank control group.
Citral pickering emulsion prepared by the present invention is few with nano-cellulose dosage, preparation process is simple and the spies such as application cost is low
Point can effectively improve the stability of citral under acid condition, delay its degradation.
Description of the drawings
Fig. 1 is the citral pickering emulsion outside drawing prepared by the embodiment of the present invention 1.
Specific implementation mode
The invention will now be described in further detail by way of examples and with reference to the accompanying drawings, but is not intended to limit the present invention.
Embodiment 1
(1)The preparation of ammonium persulfate aqueous solution
Ammonium persulfate is dissolved in 1L deionized waters, stirring forms ammonium persulfate aqueous solution, described until fully dissolving
In ammonium persulfate aqueous solution, a concentration of 2mol/L of the ammonium persulfate;
(2)The preparation of nano-cellulose suspension
1.5 grams of commercially available microcrystalline celluloses are added to step(1)In obtained 1L ammonium persulfate aqueous solutions, in rotating speed 1000r/
Under min magnetic agitations, it is put into 60 DEG C of water-bath constant temperature stirring 4h and stops agitating and heating fully after reaction, obtain nano-cellulose
Suspension;
(3)The preparation of nano-cellulose powder
By step(2)Obtained nano-cellulose suspension is centrifuged at 10000rpm, removes the complete ammonium persulfate of unreacted, from
Calculation, until the pH of suspension is 7;Precooling 4h under the conditions of suspension after having centrifuged is placed in -70 DEG C, then in cold-trap
Temperature is -70 DEG C, vacuum degree is freeze-dried for 24 hours under the conditions of being 5Pa, obtains nano-cellulose powder;
(4)The preparation of citral pickering emulsion
By 0.6g steps(3)Obtained nano-cellulose powder is dissolved in the citric acid-sodium citrate buffer solution that 100mLpH is 3,
After being sufficiently stirred, nano-cellulose suspension is obtained.In the nano-cellulose suspension, the nano-cellulose concentration
For 6g/L.Under 10000rpm high speed homogenizations, it is sweet that chain in 1g citrals and 0.5g is added dropwise in nano-cellulose suspension
Oily three esters, high speed homogenization time are 4min, obtain citral pickering emulsion.
By the citral pickering emulsion of above-mentioned gained 40oC is placed 14 days, passes through gas chromatograph(6890GC is beautiful
Agilent Science and Technology Ltd.s of state)Its citral retention rate is measured, is 55.31%.
Embodiment 2
(1)The preparation of ammonium persulfate aqueous solution
Ammonium persulfate is dissolved in 1L deionized waters, stirring forms ammonium persulfate aqueous solution, described until fully dissolving
In ammonium persulfate aqueous solution, a concentration of 0.5mol/L of the ammonium persulfate;
(2)The preparation of nano-cellulose suspension
2 grams of commercially available microcrystalline celluloses are added to step(1)In obtained 1L ammonium persulfate aqueous solutions, in rotating speed 1000r/min
Under magnetic agitation, it is put into 60 DEG C of water-bath constant temperature stirring 16h and stops agitating and heating fully after reaction, it is outstanding to obtain nano-cellulose
Supernatant liquid;
(3)The preparation of nano-cellulose powder
By step(2)Obtained nano-cellulose suspension is centrifuged at 10000rpm, removes the complete ammonium persulfate of unreacted, from
Calculation, until the pH of suspension is 7;Precooling 4h under the conditions of suspension after having centrifuged is placed in -70 DEG C, then in cold-trap
Temperature is -70 DEG C, vacuum degree is freeze-dried for 24 hours under the conditions of being 5Pa, obtains nano-cellulose powder;
(4)The preparation of citral pickering emulsion
By 1g steps(3)Obtained nano-cellulose powder is dissolved in the citric acid-sodium citrate buffer solution that 100mLpH is 3, is filled
After dividing stirring, nano-cellulose suspension is obtained.In the nano-cellulose suspension, the nano-cellulose is a concentration of
10g/L.Under 16000rpm high speed homogenizations, 1.5g citrals and 2g medium chain triglycerides are added dropwise in nano-cellulose suspension
Three esters, high speed homogenization time are 3min, obtain citral pickering emulsion.
By the citral pickering emulsion of above-mentioned gained 40oC is placed 14 days, passes through gas chromatograph(6890GC is beautiful
Agilent Science and Technology Ltd.s of state)Its citral retention rate is measured, is 40.48%.
Embodiment 3
(1)The preparation of ammonium persulfate aqueous solution
Ammonium persulfate is dissolved in 1L deionized waters, stirring forms ammonium persulfate aqueous solution, described until fully dissolving
In ammonium persulfate aqueous solution, a concentration of 1mol/L of the ammonium persulfate;
(2)The preparation of nano-cellulose suspension
2.5 grams of commercially available microcrystalline celluloses are added to step(1)In obtained 1L ammonium persulfate aqueous solutions, in rotating speed 1000r/
Under min magnetic agitations, it is put into 60 DEG C of water-bath constant temperature stirring 8h and stops agitating and heating fully after reaction, obtain nano-cellulose
Suspension;
(3)The preparation of nano-cellulose powder
By step(2)Obtained nano-cellulose suspension is centrifuged at 10000rpm, removes the complete ammonium persulfate of unreacted, from
Calculation, until the pH of suspension is 7;Precooling 4h under the conditions of suspension after having centrifuged is placed in -70 DEG C, then in cold-trap
Temperature is -70 DEG C, vacuum degree is freeze-dried for 24 hours under the conditions of being 5Pa, obtains nano-cellulose powder;
(4)The preparation of citral pickering emulsion
By 0.4g steps(3)Obtained nano-cellulose powder is dissolved in the citric acid-sodium citrate buffer solution that 100mLpH is 3,
After being sufficiently stirred, nano-cellulose suspension is obtained.In the nano-cellulose suspension, the nano-cellulose concentration
For 4g/L.Under 13000rpm high speed homogenizations, chain in 0.5g citrals and 1.5g is added dropwise in nano-cellulose suspension
Triglycerides, high speed homogenization time are 2min, obtain citral pickering emulsion.
By the citral pickering emulsion of above-mentioned gained 40oC is placed 14 days, passes through gas chromatograph(6890GC is beautiful
Agilent Science and Technology Ltd.s of state)Its citral retention rate is measured, is 48.19%.
Embodiment 4
(1)The preparation of ammonium persulfate aqueous solution
Ammonium persulfate is dissolved in 1L deionized waters, stirring forms ammonium persulfate aqueous solution, described until fully dissolving
In ammonium persulfate aqueous solution, a concentration of 1.5mol/L of the ammonium persulfate;
(2)The preparation of nano-cellulose suspension
1 gram of commercially available microcrystalline cellulose is added to step(1)In obtained 1L ammonium persulfate aqueous solutions, in rotating speed 1000r/min
Under magnetic agitation, it is put into 60 DEG C of water-bath constant temperature stirring 12h and stops agitating and heating fully after reaction, it is outstanding to obtain nano-cellulose
Supernatant liquid;
(3)The preparation of nano-cellulose powder
By step(2)Obtained nano-cellulose suspension is centrifuged at 10000rpm, removes the complete ammonium persulfate of unreacted, from
Calculation, until the pH of suspension is 7;Precooling 4h under the conditions of suspension after having centrifuged is placed in -70 DEG C, then in cold-trap
Temperature is -70 DEG C, vacuum degree is freeze-dried for 24 hours under the conditions of being 5Pa, obtains nano-cellulose powder;
(4)The preparation of citral pickering emulsion
By 0.8g steps(3)Obtained nano-cellulose powder is dissolved in the citric acid-sodium citrate buffer solution that 100mLpH is 3,
After being sufficiently stirred, nano-cellulose suspension is obtained.In the nano-cellulose suspension, the nano-cellulose concentration
For 8g/L.Under 19000rpm high speed homogenizations, 2g citrals and 1g medium chain triglycerides are added dropwise in nano-cellulose suspension
Three esters, high speed homogenization time are 5min, obtain citral pickering emulsion.
By the citral pickering emulsion of above-mentioned gained 40oC is placed 14 days, passes through gas chromatograph(6890GC is beautiful
Agilent Science and Technology Ltd.s of state)Its citral retention rate is measured, is 53.10%.
Comparative example 1
1g citrals and 0.5g medium chain triglycerides are added in the citric acid-sodium citrate buffer solution that 100mLpH is 3,
10000rpm speed down cuts disperse 4min to get citral aqueous solution(Blank control).
By the blank control of above-mentioned gained 40oC is placed 14 days, passes through gas chromatograph(6890GC, U.S. Agilent
Science and Technology Ltd.)Its citral retention rate is measured, is 0.95%.
The present embodiment is to be compared citral pickering emulsion with blank control, more effectively illustrate the present invention
Effect.The lotion of the present invention is 40oAfter C is stored 14 days, citral retention rate is 40.48 ~ 55.31%% in lotion, same
Condition of storage under, in blank control citral retention rate be 0.95%.Illustrate that nanofiber crude granule substantially increases citral
Stability in acid condition.
Above said content is only the basic explanation under present inventive concept, and is appointed made by technical solution according to the present invention
What equivalent transformation, is within the scope of protection of the invention.
Claims (1)
1. a kind of preparation method for the citral pickering emulsion that nano-cellulose is stablized, it is characterised in that include the following steps:
1)One the step of preparing ammonium persulfate aqueous solution;
It dissolves ammonium persulfate into deionized water, stirring forms ammonium persulfate aqueous solution, in the over cure until fully dissolving
In sour aqueous ammonium, a concentration of 0.5 ~ 2mol/L of the ammonium persulfate;
2)One the step of preparing nano-cellulose suspension;
It weighs microcrystalline cellulose and is added to step 1)In obtained ammonium persulfate aqueous solution, in rotating speed 1000r/min magnetic agitations
Under, it is put into 60 DEG C of water-bath constant temperature and stirs 4 ~ 16h, fully after reaction, stopping agitating and heating obtaining nano-cellulose suspension;
The material ratio of microcrystalline cellulose and ammonium persulfate aqueous solution is 1 ~ 2.5 gram:1L;
3)One the step of preparing nano-cellulose powder;
By step 2)Obtained nano-cellulose suspension is centrifuged at 10000rpm, removes the complete ammonium persulfate of unreacted, from
The heart at least twice, until suspension pH be 7;Precooling 4h, then exists under the conditions of suspension after having centrifuged is placed in -70 DEG C
Condenser temperature is -70 DEG C, vacuum degree is freeze-dried for 24 hours under the conditions of being 5Pa, obtains nano-cellulose powder;
4)One the step of preparing citral pickering emulsion;
By step 3)Obtained nano-cellulose powder is dissolved in the citric acid-sodium citrate buffer solution that pH is 3, is sufficiently stirred
Afterwards, obtain nano-cellulose suspension, in the nano-cellulose suspension, the nano-cellulose a concentration of 4 ~
Lemon is added dropwise by mass-volume concentration in nano-cellulose suspension under 10000 ~ 19000rpm high speed homogenizations in 10g/L
The mass volume ratio of lemon aldehyde and medium chain triglyceride, the citral and nano-cellulose suspension is 0.5 ~ 2g:100ml,
The medium chain triglyceride citral and be 0.5 ~ 2g with the mass volume ratio of nano-cellulose suspension:100ml, high speed is
The matter time is 2 ~ 5min, obtains citral pickering emulsion.
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Cited By (2)
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CN113004559A (en) * | 2021-03-08 | 2021-06-22 | 四川大学 | Active gelatin-based edible film and preparation and application methods thereof |
CN113368049A (en) * | 2021-06-17 | 2021-09-10 | 江南大学 | Pickering emulsion based on fat crystal nanoparticle stability and preparation method thereof |
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Cited By (3)
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