CN105053745A - Preparation method for curcumin microcapsule with egg white powder as wall material - Google Patents
Preparation method for curcumin microcapsule with egg white powder as wall material Download PDFInfo
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Abstract
The present invention belongs to the preparation field of microcapsules, and particularly relates to a preparation method for a curcumin microcapsule with egg white powder as a wall material. The curcumin microcapsule is prepared by using the curcumin as a core material and the egg white powder and gelatin (mass ratio, egg white powder/gelatin = 1:1) as the wall material, stirring, mixing, embedding (temperature, 50 DGE C; time, 100 minutes), homogenizing the core material and the wall material (mass ratio, the core material/the wall material = 1:20) with the addition of emulsifiers (mass ratio, core material/emulsifier = 1:2) to obtain emulsified liquid, and finally spray drying the emulsified liquid. By optimizing the mass ratio of the core material and the wall material, the mass ratio of the emulsifiers and the core material, the mass ratio of the egg white powder and the gelatin and other factors, the embedding rate of the curcumin microcapsule is greatly improved, and the embedding rate reaches 86.72%.
Description
Technical field
The invention belongs to the preparation field of microcapsules, being specifically related to a kind of take egg-white powder as the method that curcumin microcapsule prepared by wall material.
Background technology
Microcapsules technology has been succeeded application in many fields such as food, chemical industry, medicine, biotechnology, makes many properties of product be improved and improve.Its application in the food industry mainly concentrates on the embedding of the raw-food materials such as grease, essence and flavoring agent, essential oil, pigment, vitamin and anticorrisive agent or additive, with starvation, light, reach and extend the raw-food material shelf-life, change food state, improve the objects such as mixed performance.
Egg is the food that nutritive value is very high, and containing good protein, amino acid, lecithin, fat, cholesterol, the vitamins and other nutritious components of needed by human body, digestibility is high, and especially the absorptivity of protein can up to 98%.Protein is mainly from egg, and egg-white powder is the excellent product of being refined by pure egg, and have desugar, take off raw meat, purity is high, dissolve the features such as rapid, egg-white powder also has good functional characteristic, as high gelation, emulsibility, water-retaining property etc.Meanwhile, egg-white powder is everlasting in dyeing as sticking agent.
Curcumin is having of extracting from turmeric rhizome
βthe uranidin of-diketone structure, it is bright in colour, safety non-toxic, and has certain pharmacological function concurrently.Curcumin mainly comprises the slightly discrepant three kinds of compounds of molecular structure, all containing multiple double bond, phenolic hydroxyl group and carbonyl etc. in their molecule, so chemical reactivity is stronger.This is the main cause that the stability of curcumin is easily subject to the impact of multiple chemical factors, and light, heat can impel its oxidation Decomposition, lose colour developing power.In addition, curcumin is water-soluble hardly, easily forms precipitation in an acidic solution, which hampers its large-scale application in acidic beverages.Therefore, managing to strengthen its stability and increasing its solubility in water is the key point whether curcumin can be used widely.Adopt microcapsules technology to be embedded in the material of food ingredient composition, not only can improve its stability, and dissolubility also makes moderate progress.Through microencapsulation curcumin can broadly for cake, candy, beverage, ice cream, have in the food such as color wine.
The present invention take curcumin as core, egg-white powder and gelatin are that microcapsules prepared by wall material, have studied core wall ratio, emulsifying agent and core mass ratio, egg-white powder and gelatin proportioning to the impact of curcumin microcapsule embedding rate, set up the Mathematical Modeling between embedding rate and each factor, and apply response phase method each factor is optimized, be convenient to the control of technical process and meet the demand of food additives to stability.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, providing a kind of take egg-white powder as the method that curcumin microcapsule prepared by wall material.By being optimized factors such as core wall ratio, emulsifying agent, core mass ratio, egg-white powder and gelatin proportionings, greatly improve the embedding rate of curcumin microcapsule, embedding rate reaches 86.72%.
For achieving the above object, the present invention adopts following technical scheme:
Be the method that curcumin microcapsule prepared by wall material with egg-white powder, take curcumin as core, egg-white powder and gelatin are wall material, add emulsifying agent, stir, mixing, embedding, homogeneous obtains emulsion, and last spraying dry obtains curcumin microcapsule; Wherein,
The mass ratio of core and wall material is 1:20;
The quality proportioning of egg-white powder and gelatin is 1:1;
Emulsifying agent and core mass ratio 2:1;
Embedding temperature 50 C;
Embedding time 100min.
the computational methods of embedding rate are:
1, the making of calibration curve
Take 0.01g curcumin, dissolve with ethanol, proceed in 100mL volumetric flask, use ethanol constant volume, obtain 0.1mg/mL stock solution, pipette 0.7 respectively, 0.8,0.9,1.0,1.1, the above-mentioned stock solution of 1.2mL is in 10mL volumetric flask, add ethanol and be diluted to scale, with ethanol for blank sample, measure absorbance at 426nm place;
Regression equation is: y=0.1557x-0.0108, R
2=0.9917
2, curcumin microcapsule metallization processes, as shown in Figure 9.
3, the mensuration of microcapsule product embedding rate
0.01g curcumin adds monoglyceride after mixing with wall material, magnetic agitation 10min, homogeneous 5min, centrifugal (10000r/min, 10min), get supernatant VmL, recording supernatant absorbance is A, substitute into calibration curve and calculate supernatant c (μ g/mL), be calculated as follows: embedding rate=c × V × 10
-6/ 0.01 × 100%.
beneficial effect of the present invention is:
1) the present invention adopts microcapsules technology to be embedded in by curcumin in the material be made up of egg white and gelatin, not only can improve its stability, and dissolubility also makes moderate progress; Through microencapsulation curcumin can broadly for cake, candy, beverage, ice cream, have in the food such as color wine;
2) the present invention is by being optimized factors such as core wall ratio, emulsifying agent, core mass ratio, egg-white powder and gelatin proportionings, and determine optimal proportion, greatly improve the embedding rate of curcumin microcapsule, embedding rate reaches 86.72%.
Accompanying drawing explanation
Fig. 1 egg-white powder and gelatin proportioning are on the impact of curcumin embedding rate;
Fig. 2 emulsifying agent and core mass ratio are on the impact of curcumin embedding rate;
The impact of Fig. 3 core wall comparison curcumin embedding rate;
Fig. 4 embeds the impact of temperature on curcumin embedding rate;
Fig. 5 embeds the impact of time on curcumin embedding rate;
Fig. 6 Y=f(A, B) response surface figure (1) and contour plots analysis figure (2);
Fig. 7 Y=f(A, C) response surface figure (1) and contour plots analysis figure (2);
Fig. 8 Y=f(B, C) response surface (1) and contour plots analysis figure (2);
Fig. 9 curcumin microcapsule metallization processes figure.
Detailed description of the invention
The present invention's the following example further illustrates the present invention, but protection scope of the present invention is not limited to the following example.
embodiment 1
A kind of take egg-white powder as the method that curcumin microcapsule prepared by wall material, take 100g egg-white powder to mix with 100g gelatin, dissolve as wall material, add curcumin 10g, emulsifying agent monoglyceride 20g, be uniformly mixed, embed, homogeneous obtains emulsion, and last spraying dry obtains curcumin microcapsule; Wherein, temperature 50 C is embedded; Embedding time 100min.
With this understanding, embedding rate reaches 86.72%.
The present invention is directed to each condition to be optimized, to choose optimal conditions, reach best embedding rate.
1, egg-white powder and gelatin proportioning are on the impact of curcumin embedding rate
At core wall than being 1:25, emulsifying agent and core mass ratio 2:1, embedding temperature 50 C, under the condition of embedding time 100min, get egg-white powder: gelatin is respectively 1:9,2:8,3:7,4:6,5:5,6:4,7:3,8:2,9:1, the embedding rate respectively after assaying reaction.Experimental result is shown in Fig. 1.
Gelatin and egg-white powder composite, the stability of emulsion can be improved, improve embedding rate.Fig. 1 shows, the proportioning of different content egg-white powder and gelatin, on microcapsules efficiency to affect difference larger.When egg-white powder: during gelatin=1:1, microcapsules efficiency is best.Along with the continuation of egg-white powder increases, embedding rate declines gradually; And gelatine content is too high, when spraying dry, wall sticking phenomenon is comparatively remarkable, and microcapsule product loss is just more.
2, emulsifying agent and core mass ratio are on the impact of curcumin embedding rate
At core wall than for 1:25, egg-white powder: gelatin 1:1, embedding temperature 50 C, under the condition of embedding time 100min, gets emulsifying agent with core mass ratio is respectively 2:1,1:1,1:2,1:3,1:4, the embedding rate after difference assaying reaction.Result of the test is shown in Fig. 2.
Shown by Fig. 2, emulsifier is comparatively large on the impact of embedding rate, and a small amount of emulsifying agent adds the viscosity that just obviously can reduce emulsion; The viscosity of emulsion can be made again to significantly improve as excessive, unfavorable to stablizing of emulsion, thus impact embedding effect.The smell of product can be affected in addition.When emulsifying agent and core mass ratio are 2:1, the embedding rate of curcumin is the highest.
3, the impact of core wall comparison curcumin embedding rate
At egg-white powder: gelatin 1:1, emulsifying agent and core mass ratio 2:1, embedding temperature 50 C, under the condition of embedding time 100min, gets core wall ratio and is respectively 1:15,1:20,1:25,1:30,1:35, the embedding rate respectively after assaying reaction.Result of the test is shown in Fig. 3.
As shown in Figure 3, when wall material content is lower, less by the curcumin of inclusion, along with the increase of wall material addition, curcumin content presents the trend of a first increases and then decreases, and when core wall ratio reaches 1:25, curcumin content reaches peak value.This is because curcumin formed with wall material is 1:1 type inclusion compound, the amount of wall material inclusion core is limited, time within maximum inclusion amount, along with the increase of wall material amount, curcumin content increases, after wall material molecule inner chamber is full of by curcumin molecule, then increase wall material, curcumin content reduces gradually.
4, temperature is embedded on the impact of curcumin embedding rate
At core wall than being 1:25, egg-white powder: gelatin is 1:1, emulsifying agent and core mass ratio 2:1, under the condition of embedding time 100min, getting embedding temperature and being respectively 20,30,40,50,60 DEG C, the embedding rate respectively after assaying reaction.Result of the test is shown in Fig. 4.
As can be seen from Figure 4, when temperature is lower, embedding rate increases gradually along with the liter of temperature, and when embedding temperature at about 50 DEG C, the embedding rate of curcumin reaches the highest, and temperature continues to raise, and embedding rate declines on the contrary.This is because curcumin will slough water hull disease before the hydrophobic cavity entering wall material discharge Bound moisture, this is an endothermic process, and namely raised temperature is conducive to the combination of Subjective and Objective molecule; Afterwards, wall material is by hydrogen bond, and Van der Waals force and hydrophobic effect realize the embedding to curcumin, and this is an exothermic process, raised temperature, and curcumin will be released again, cause embedding rate to decline.Therefore, it is best for embedding temperature with 50 DEG C.
5, the time that embeds is on the impact of curcumin embedding rate
At core wall than for 1:25, egg-white powder: gelatin is 1:1, emulsifying agent and core mass ratio 2:1, under the condition of embedding temperature 50 C, getting the embedding time is respectively 40,60,80,100,120 DEG C, distinguishes the embedding rate after assaying reaction.Result of the test is shown in Fig. 5.
Can find out the increase along with the embedding time from Fig. 5, the embedding rate of curcumin is in increase; After the time reaches 100min, the embedding rate of curcumin slightly declines.
6, response surface optimization curcumin microcapsule embedding rate
6.1Box-Behnken experimental design and experimental result
On single factor experiment basis, according to Box-Behnken experimental design principle, with core wall ratio, emulsifying agent and core mass ratio, egg-white powder and gelatin proportioning for independent variable, take embedding rate as response, the totally 17 groups of response surface analysises experiment of design Three factors-levels, studies each independent variable and reciprocation thereof to the impact of curcumin microcapsule embedding rate.Use DesignExpert8.0.6.1 software, experiment centered by experiment 4,5,12,13,16, in order to estimate experimental error, other are factorial experiment.Design factor and level in table 1, experimental design and the results are shown in Table 2.
Table 1 response phase method experimental factor and level code table
Table 2Box-Behnken experimental design and result
6.2 response surface optimization experimental results
Utilize Design-Expert8.0.6.1 program to carry out ANOVA analysis to the data obtained, analysis result is in table 3.
The variance analysis of table 3 regression model
Note: * * represents that extremely significantly (p<0.01) * represents significantly (0.01<p<0.05)
The regression equation that three factors obtain through over-fitting is: Y=86.70+0.00125 × A+0.00375 × B+0.0025 × C+0.012 × A × B-0.015 × A × C+0.01 × B × C-1.16 × A
2-0.87 × B
2-1.28 × C
2.
As shown in Table 3, model
p<0.0001, coefficient correlation
r 2=0.9980, adjusted coefficient of determination
r adj 2=0.9990, lose and intend item
p=0.7671>0.05 is not remarkable, and this model highly significant is described, test method is reliable, and the analysis using this equation influence factor that is virtually reality like reality level is feasible.From table 3, Pr>F item can be known, quadratic term A
2, B
2, C
2have embedding rate and affect extremely significantly, the impact of other factors is not remarkable, and this shows the change more complicated of response, and each experimental factor is not simple linear relationship on the impact of response, but in secondary relation, and there is reciprocation between Three factors.
6.3 response surface analysises and optimization
On the basis of variance analysis, utilize Design-Expert8.0.6.1 Software on Drawing significant interaction factors A B, the reciprocation surface chart of AC, BC and contour map, Fig. 6,7,8 gives 3D and the circle of equal altitudes of three interactive response surfaces of factor of influence intuitively.
As can be seen from peak and the isopleth of response surface, in selected scope, there is extreme value, is namely the central point of isopleth minimum ellipse, is also the peak on response surface design simultaneously.When obtaining maximum response (Y) by Design-Expert8.0.6.1 analysis, the optimum process condition of its maximum embedding rate is: core wall is than being 1:20, and emulsifying agent and core mass ratio are 2:1, egg-white powder and gelatin proportioning 1:1, and theoretical maximum embedding rate is 86.75%.
7, replication experiment
Gained Optimizing Process Parameters is used to carry out egg-white powder and gelatin embedding curcumin demonstration test, with egg-white powder and gelatin proportioning 1:1, emulsifying agent and core mass ratio 2:1, core wall is best than 1:20, carry out 3 repeated experiments, obtaining embedding rate mean value is 86.72%.The optimization of response phase method to egg-white powder and gelatin embedding curcumin process conditions is feasible, and the process conditions obtained have actual application value.
The foregoing is only preferred embodiment of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (1)
1. be the method that curcumin microcapsule prepared by wall material with egg-white powder, it is characterized in that: take curcumin as core, egg-white powder and gelatin are wall material, add emulsifying agent, stir, mix, embed, homogeneous obtains emulsion, and last spraying dry obtains curcumin microcapsule; Wherein,
The mass ratio of core and wall material is 1:20;
The quality proportioning of egg-white powder and gelatin is 1:1;
Emulsifying agent and core mass ratio 2:1;
Embedding temperature 50 C;
Embedding time 100min.
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| CN111481524A (en) * | 2020-03-31 | 2020-08-04 | 右江民族医学院 | Curcumin microencapsulation method |
| CN113367307A (en) * | 2021-06-23 | 2021-09-10 | 天津春发生物科技集团有限公司 | Long-acting microcapsule essence and preparation method thereof |
| CN114984873A (en) * | 2022-06-10 | 2022-09-02 | 云南中烟工业有限责任公司 | Preparation method of response surface method optimized aroma-enhancing component microcapsule |
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| CN113367307A (en) * | 2021-06-23 | 2021-09-10 | 天津春发生物科技集团有限公司 | Long-acting microcapsule essence and preparation method thereof |
| CN114984873A (en) * | 2022-06-10 | 2022-09-02 | 云南中烟工业有限责任公司 | Preparation method of response surface method optimized aroma-enhancing component microcapsule |
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