CN112063195A - Passion fruit peel anthocyanin microcapsule and secondary embedding preparation method thereof - Google Patents
Passion fruit peel anthocyanin microcapsule and secondary embedding preparation method thereof Download PDFInfo
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- CN112063195A CN112063195A CN202010730026.7A CN202010730026A CN112063195A CN 112063195 A CN112063195 A CN 112063195A CN 202010730026 A CN202010730026 A CN 202010730026A CN 112063195 A CN112063195 A CN 112063195A
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0097—Dye preparations of special physical nature; Tablets, films, extrusion, microcapsules, sheets, pads, bags with dyes
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/40—Colouring or decolouring of foods
- A23L5/42—Addition of dyes or pigments, e.g. in combination with optical brighteners
- A23L5/43—Addition of dyes or pigments, e.g. in combination with optical brighteners using naturally occurring organic dyes or pigments, their artificial duplicates or their derivatives
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
- A23P10/00—Shaping or working of foodstuffs characterised by the products
- A23P10/30—Encapsulation of particles, e.g. foodstuff additives
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
Abstract
The invention discloses a passion flower pericarp anthocyanin microcapsule and a secondary embedding preparation method thereof, and the method comprises the following steps: taking passion fruit peel anthocyanin as a core material, taking gelatin and Arabic gum as wall materials, and preparing a single-layer microcapsule wet capsule by a complex coacervation method; taking nano SiO2Adding into distilled water of 60 deg.C, stirring for 30min, ultrasonic treating for 2 hr to obtain dispersion, adding acacia into the dispersion, mixing and stirring for 30min to obtain nanometer SiO2Modified arabic gum solution; mixing nano SiO2The modified Arabic gum solution is fully mixed with the single-layer microcapsule wet capsuleMixing, stirring at room temperature of 200r/min for 30min, and spray drying to obtain passion flower pericarp anthocyanin microcapsule. The invention adopts a secondary embedding method and uses nano SiO2The modified Arabic gum is used as the second layer wall material, so that the capsule wall structure is more compact, and the defects that the single-layer microcapsule has insufficient capsule wall toughness and strength, poor microcapsule stability, large influence of environmental factors such as temperature, humidity and pH and the like are overcome.
Description
Technical Field
The invention relates to the technical field of microcapsule preparation, in particular to a passion flower pericarp anthocyanin microcapsule and a secondary embedding preparation method thereof.
Background
Anthocyanins are compounds formed by combining anthocyanidins and sugars, and are widely present in the cell sap of flowers, fruits, stems, leaves and root organs of plants. Anthocyanin is a natural pigment, is safe and nontoxic, has a plurality of health care functions for human body, and is applied to industries of food, health care products, cosmetics, medicines and the like. However, the basic structure of anthocyanin is diphenyl benzopyran cation, and the structure lacks an electron, so that the anthocyanin has extremely strong antioxidant activity, but because of the existence of hydroxyl and epoxy ions on the molecular structure of anthocyanin, the anthocyanin has poor structural stability and is easily influenced by factors such as temperature, relative humidity, illumination, pH, enzyme, metal ions and the like, so that the application range of anthocyanin is greatly limited.
The main measures for improving the stability of anthocyanin are adding a stabilizer, modifying an anthocyanin structure and microencapsulation. The microcapsule effect of the anthocyanin is more outstanding, and the microcapsule can effectively improve the heat resistance, light resistance and metal ion resistance of the anthocyanin and avoid the influences of temperature, humidity, pH and the like. The microcapsule technology is that an inner material (core material) is coated by an outer protective shell material (wall material) to form a core-shell structure; or dispersing the core material in a protective material matrix for protecting the core material from adverse conditions (e.g., heat, light, oxygen, and the presence of metal ions, etc.); or release the core material to the outside at a controlled rate, thereby facilitating application in various fields.
However, the anthocyanin microencapsulation technology is currently studied to prepare single-layer microcapsules, for example, regarding passion flower pericarp anthocyanin, the most adopted method is to prepare single-layer passion flower pericarp anthocyanin microcapsules by taking gelatin and arabic gum as wall materials. The single-layer microcapsule has certain defects, such as insufficient toughness and strength of the capsule wall, poor stability of the microcapsule, and the like, and is still influenced by environmental factors such as temperature, humidity, pH and the like.
The existing research shows that the double-layer microcapsule system formed by the secondary embedding technology is stable, the wall thickness of the microcapsule is thick, and the environmental pressure can be well resisted. In addition, in recent years, it has become a hot spot to modify polymer materials with nanoparticles to prepare microcapsules with excellent performance, wherein nano-SiO is2The material has surface energy, good dispersibility and barrier property, and is a high-quality material for improving the compactness and thermal stability of the wall material.
Disclosure of Invention
In order to solve the problems, the invention provides a passion flower pericarp anthocyanin microcapsule and a secondary embedding preparation method thereof2The modified Arabic gum is used as a second layer wall material, and a secondary embedding method is adopted to prepare the double-layer microcapsule.
The invention realizes the purpose through the following technical scheme:
a secondary embedding preparation method of passion fruit peel anthocyanin microcapsules comprises the following steps: comprises the steps of
Taking passion flower pericarp anthocyanin as a core material and gelatin and Arabic gum as wall materials, and preparing a single-layer microcapsule wet capsule by a complex coacervation method;
step two, taking nano SiO2Adding into distilled water of 55-65 deg.C, stirring for 25-35min, ultrasonic treating for 1.5-2.5h to obtain stable dispersion, adding acacia into the dispersion, mixing and stirring for 25-35min to obtain nanometer SiO2Modified arabic gum solution;
step three, mixing the nano SiO2Fully mixing the modified Arabic gum solution with the single-layer microcapsule wet capsule, stirring at room temperature of 240r/min for 25-35min, and spray drying to obtain the first-layer wall material of the Arabic gum and the nanometer SiO2The modified Arabic gum is the passion flower pericarp anthocyanin microcapsule with the second layer of wall material.
The further improvement is that 0.15g of nano SiO is added into every 100mL of distilled water2Adding 6g of Arabic gum to the mixture, and preparing nano SiO2The modified gum arabic solution was then mixed with 100mL single-layer microcapsule wet capsules.
In a further improvement, in the third step, the spray drying conditions are as follows: the air inlet temperature is 180 ℃, the air outlet temperature is 90 ℃, and the feeding speed is 7.5 mL/min.
The further improvement is that the specific operation of the step one is as follows:
(1) preparation of gelatin and Arabic gum raw material liquid
Taking gelatin and Arabic gum as wall materials, controlling the wall material ratio of gelatin to Arabic gum to be 5:6, adding the wall materials into distilled water, controlling the wall material concentration to be 1.5%, and stirring in a water bath at 40 ℃ at a rotating speed of 200r/min to fully dissolve the gelatin and the Arabic gum to obtain a raw material solution;
(2) formation of microcapsules
Adding passion flower pericarp anthocyanin as core material into raw material liquid, controlling the core-wall ratio to be 1:5.5, stirring while adding, adjusting pH of the solution to 3.49 with 10% glacial acetic acid after complete dissolution, and performing complex coacervation reaction at 40 ℃ for 30 min;
(3) curing of microcapsules
After the complex coacervation reaction, cooling the obtained microcapsule solution to room temperature, continuing stirring for 1h, then cooling the microcapsule solution to 15 ℃, adding glutamine transaminase according to the addition amount of 30g/100g of gelatin, continuously stirring for 3h, completing solidification, and filtering to obtain the single-layer microcapsule wet capsule.
A passion flower pericarp anthocyanin microcapsule is prepared by the preparation method.
The invention has the beneficial effects that:
(1) the passion flower pericarp anthocyanin double-layer microcapsule is prepared by adopting a secondary embedding method, and the defects that the capsule wall of the single-layer microcapsule is insufficient in toughness and strength, the microcapsule is poor in stability, and the influence of environmental factors such as temperature, humidity and pH is large are overcome, so that the passion flower pericarp anthocyanin double-layer microcapsule can better resist environmental pressure.
(2) The second layer of the wall material adopts nano SiO2The modified Arabic gum is used as a wall material, and the nano SiO is fully utilized2Surface energy possessed, goodDispersibility and barrier property, nano SiO2The hydroxyl group and the hydroxyl group on the Arabic gum molecule form a hydrogen bond, so that the capsule wall structure is more compact and is not easy to break, and compared with the common double-layer microcapsule, the embedding rate, the droplet particle size, the moisture content, the SEM, the thermal stability (DSC), the storage stability and the like of the microcapsule are improved in different ranges.
Drawings
FIG. 1 is a schematic illustration of a method according to an embodiment of the present invention;
FIG. 2 is a schematic illustration of the effect of core wall ratio on the encapsulation efficiency of microcapsules;
FIG. 3 is a schematic diagram showing the influence of the wall material ratio on the embedding rate of microcapsules;
FIG. 4 is a graph showing the effect of wall material concentration on the encapsulation efficiency of microcapsules;
FIG. 5 is a schematic diagram showing the effect of pH of complex coacervation on the encapsulation efficiency of microcapsules;
FIG. 6 is a schematic diagram showing the effect of reaction temperature on the embedding rate of microcapsules;
FIG. 7 is a schematic diagram showing the effect of reaction time on the encapsulation efficiency of microcapsules;
FIG. 8 is a schematic diagram showing the effect of enzyme addition on the encapsulation efficiency of microcapsules;
FIG. 9 is a schematic illustration of the embedding rates of three microcapsules;
fig. 10 is an optical microscope schematic of three microcapsules, wherein samples (a), (b), and (c): single-layer microcapsule, gum arabic-double-layer microcapsule and gum arabic/SiO2-a double layer microcapsule;
FIG. 11 is a schematic view of the droplet size of three microcapsules;
FIG. 12 is a schematic representation of the moisture content of three microcapsules;
fig. 13 is a SEM illustration of three microcapsules, wherein samples (a), (b), and (c): single-layer microcapsule, gum arabic-double-layer microcapsule and gum arabic/SiO2-a double layer microcapsule;
figure 14 is a schematic thermal stability diagram of three microcapsules.
Detailed Description
The present application will now be described in further detail with reference to the drawings, it should be noted that the following detailed description is given for illustrative purposes only and is not to be construed as limiting the scope of the present application, as those skilled in the art will be able to make numerous insubstantial modifications and adaptations to the present application based on the above disclosure.
Examples
Materials and instruments:
raw materials: acacia is purchased from national drug group chemical reagents, ltd; nano SiO2Purchased from Zhoushan Mingri Co., Ltd. The instrument comprises the following steps: a desiccator (specification 307mm × 330mm, Kunming disc Longhuasen laboratory facility department), a magnetic stirring water bath (HH-S4 type, Changzhou Lange instruments manufacturing Co., Ltd.), an ultrasonic cell disruptor (JRA-650 type, Wuxi Jie Ruian instruments Co., Ltd.), a pH meter (PHS-25 type, Shanghai apparatus electronic science instruments Co., Ltd.), a spray drier (B-290 type, Switzerland Buchi laboratory technology Co., Ltd.), a 1/10000 electronic analytical balance (BSA224S type, Beijing Saedodoris instruments System Co., Ltd.), an ultraviolet spectrophotometer (760CRT type, Shanghai apparatus electronic science instruments Co., Ltd.), a constant temperature and humidity incubator (SPX-150B type, Tianjin Tester instruments Co., Ltd.), a scanning electron microscope (SC-4800 type, Hitachi technology Co., Japan), a differential calorimetric scanner (DSC204F1 type, german limp instruments manufacturing ltd).
As shown in figure 1, a secondary embedding preparation method of passion flower pericarp anthocyanin microcapsules comprises the following steps: comprises the steps of
Taking passion flower pericarp anthocyanin as a core material and gelatin and Arabic gum as wall materials, and preparing a single-layer microcapsule wet capsule by a complex coacervation method, wherein the specific operations are as follows:
(1) preparation of gelatin and Arabic gum raw material liquid
Taking gelatin and Arabic gum as wall materials, controlling the wall material ratio of gelatin to Arabic gum to be 5:6, adding the wall materials into distilled water, controlling the wall material concentration to be 1.5%, and stirring in a water bath at 40 ℃ at a rotating speed of 200r/min to fully dissolve the gelatin and the Arabic gum to obtain a raw material solution;
(2) formation of microcapsules
Adding passion flower pericarp anthocyanin as core material into raw material liquid, controlling the core-wall ratio to be 1:5.5, stirring while adding, adjusting pH of the solution to 3.49 with 10% glacial acetic acid after complete dissolution, and performing complex coacervation reaction at 40 ℃ for 30 min;
(3) curing of microcapsules
After the complex coacervation reaction, cooling the obtained microcapsule solution to room temperature, continuing stirring for 1h, then cooling the microcapsule solution to 15 ℃, adding glutamine transaminase according to the addition amount of 30g/100g of gelatin, continuously stirring for 3h, completing solidification, and filtering to obtain the single-layer microcapsule wet capsule.
Step two, taking 0.15g of nano SiO2Adding into 100mL of distilled water of 55-65 deg.C, stirring for 30min, ultrasonic treating for 2h to obtain stable dispersion, adding 6g of acacia into the dispersion, mixing and stirring for 30min to obtain nanometer SiO2Modified arabic gum solution;
step three, mixing the nano SiO2Fully mixing the modified Arabic gum solution with a 100mL single-layer microcapsule wet capsule, stirring at room temperature of 200r/min for 30min, and spray drying (air inlet temperature of 180 ℃, air outlet temperature of 90 ℃, feeding speed of 7.5mL/min, and nitrogen blowing speed of 20mL/min) to obtain a first layer wall material prepared from the gelatin and the Arabic gum and a first layer wall material prepared from nano SiO2Passiflora edulis pericarp anthocyanin microcapsule (Arabic gum/SiO) with modified Arabic gum as second layer wall material2Double-layer microcapsules).
1 research and verification of the process parameters of step one of the embodiment of the invention
1.1 Single factor test
1.1.1 Effect of core wall ratio on microencapsulation embedding Rate
Other conditions for preparing the microcapsule are unchanged, and the influence of different core wall ratios on the embedding rate of the microcapsule is researched. As shown in fig. 2, the wall material specific gravity increases, and the microencapsulation rate tends to increase first and then decrease. The core-wall ratio is 1: at time 5, the encapsulation efficiency of the microcapsule reaches the maximum, and is 96.00 percent. The reason is that the core material can not be completely wrapped due to too few wall materials; the wall material is too much, and an empty capsule without the core material is formed, so that the wall material is wasted. Therefore, the core-wall ratio is selected from 1:5 is more preferable.
1.1.2 influence of wall Material ratio on the embedding Rate of microcapsules
As shown in fig. 3, the embedding rate of microcapsules tended to increase and then decrease as the specific gravity of gum arabic increased. Gelatin: gum arabic ═ 1: at 1, the embedding rate increased to a maximum of 94.25%. Protein and polysaccharide are in interaction of positive and negative charges in complex coacervation, gelatin is positively charged when the pH of the solution is less than the isoelectric point of the solution, amino ions are ionized, Arabic gum is generally negatively charged, when the wall materials are in a proper proportion, the positive and negative charges of the solution are equal, the formed complex coacervate is the most, and the good embedding effect on anthocyanin is achieved; the proportion of wall materials is not proper, the formation of complex aggregates is too little, the generated microcapsules are insufficient, and the embedding rate is reduced.
1.1.3 Effect of wall Material concentration on microencapsulation embedding Rate
The wall material concentration is an important factor influencing the complex coacervation process, and the formation of the microcapsule is not favored by over-high or under-low wall material concentration. As shown in fig. 4, when the fixed core wall ratio is 1: 4, the wall material ratio is 1: 1, when the pH value of complex coacervation is 3.5, the reaction temperature is 40 ℃, the reaction time is 30min, and the addition amount of TG enzyme is 30g/100g of gelatin, different wall material concentrations influence microencapsulation. When the wall material concentration is increased, the embedding rate is increased, and the peak value is 94.18% at 1.5%. When the wall material concentration exceeds 1.5%, the embedding rate tends to decrease, because the wall material concentration is too high, the ion concentration in the system is increased, and the interaction between polymers is weakened. Meanwhile, the increase of the wall material concentration enables the microcapsules to be easily adhered, and the embedding rate is reduced.
1.1.4 Effect of Complex coacervation pH on microencapsulation encapsulation efficiency
Gelatin is an amphoteric protein, and when the pH of a solution is lower than the isoelectric point of the gelatin, the gelatin is positively charged, and when the pH of the solution is higher than the isoelectric point of the gelatin, the gelatin is negatively charged. Gum arabic molecules are generally negatively charged in solution, and by adjusting the pH, gelatin is positively charged, and the two charges are oppositely charged and undergo a complex coacervation reaction.
The effect of pH of complex coacervation on the encapsulation efficiency of microcapsules is shown in fig. 5, where a maximum value of 94.23% was present at pH 3.5. Because the quantity of positive and negative charges provided by the wall material is equal, the cross-linking effect is optimal, and the most complex aggregates are generated. When the pH value is more than or less than 3.5, the complex aggregates are reduced, the core material is not completely wrapped, and the embedding rate is reduced.
1.1.5 Effect of reaction temperature on the encapsulation efficiency of microcapsules
The reaction temperature often plays an important role in chemical reactions, as shown in fig. 6, which illustrates the effect of the reaction temperature on the encapsulation efficiency of microcapsules. As can be seen, the complex condensation temperature is 20-40 ℃, and the embedding rate is increased. The temperature rise has positive effect on the complex coacervation reaction, the temperature is lower, the gelatin is in a gel state, and the complex coacervation reaction is not easy to occur; the temperature is increased, the viscosity of the gelatin is reduced to a certain extent, the fluidity is enhanced, and the reaction is sufficient; but the temperature is higher than 40 ℃, under the continuous stirring, the thermal motion of gelatin and Arabic gum molecules is accelerated, the gelatin and Arabic gum molecules are not easy to gather near the core material, and meanwhile, the core material is damaged by high temperature. Therefore, the reaction temperature is most preferably 40 ℃.
1.1.6 Effect of reaction time on microencapsulation encapsulation efficiency
As shown in fig. 7, proper extension of the reaction time facilitates microcapsule formation. The reaction time is 15-30 min, the embedding rate is increased, the highest point is reached in 30min, and then the highest point is decreased. The reason is that the reaction time is short and the complex coacervation is not completed; the microcapsule is conglutinated and gathered after the time is too long, the capsule wall is slightly broken, and the embedding rate is reduced. Therefore, 30min was selected for the subsequent study in this example.
1.1.7 Effect of TG enzyme addition on microcapsule embedding Rate
The microcapsule structure formed in the complex coacervation stage is unstable and is easily influenced by the pH and temperature of the solution, a curing process is needed at the moment, a curing agent enables protein molecules to be cross-linked, and the structure is stabilized. Other preparation conditions were fixed, and the influence of the addition amount of TG enzyme on the embedding rate of microcapsules was examined.
As shown in figure 8, the addition amount of TG enzyme is 15-30 g/100g of gelatin, the enzyme is fully combined with the action site of protein to generate covalent crosslinking, the microcapsule structure is stable, the addition amount is 30g/100g of gelatin, and the embedding rate reaches the highest; the addition amount is continuously increased, and the embedding rate is reduced, which can be explained as that the protein is excessively crosslinked due to the excessively high enzyme amount, the microcapsules are adhered, and the embedding rate is reduced.
1.2 Plackett-Burman test design results analysis
Plackett-Burman testThe results of the design are analyzed in Table 1, and the levels of the test factors and effects are shown in Table 2. And performing T test on each factor by using Minitab 18 software, and selecting the factor with higher confidence as a significant factor for further analysis. As can be seen from Table 2, the main factor affecting the embedding rate is x1(core-wall ratio), x2(wall material ratio) and x4(Complex coacervation pH). Therefore, the core-wall ratio, the wall-material ratio and the complex aggregation pH were selected as subjects for further investigation.
TABLE 1 Plackett-Burman test design and results
TABLE 2 Plackett-Burman test factor levels and Effect
1.3 analysis of the steepest climbing test result
The significance of the steepest climbing test of the subject lies in that the main factors are found out, the main factors are enabled to change towards the maximum direction of the response value at the same time, the maximum response interval is approached, the peak value is found out, and an effective response surface equation model is established to better reflect the real situation. Table 2 identifies the direction of the climb, with positive core-to-wall ratio, wall-to-wall ratio and complex coacervation pH T, from low to high. The test results are shown in table 3, and the embedding rate of test 3 is the highest, so that the ratio of A to 1:5, B is 1: and 1, C is the central point of the subsequent response surface test, and is 3.5.
TABLE 3 design and results of steepest climb test
1.4 response surface result optimization analysis
1.4.1 model building and significance analysis
Based on the single-factor and Plackett-Burman test Design results, other conditions are fixed, the core-wall ratio (A), the wall material ratio (B) and the complex agglomeration pH (C) are taken as factors, the microcapsule embedding rate is taken as a response value, 17 groups of tests are obtained by Box-Behnken Design of Design-Expert V8.6.0.1 software, and the Design scheme and the results are shown in Table 4:
table 4 response surface design and results
And (3) performing regression fitting by using software Design-Expert V8.6.0.1 to obtain a regression equation with the embedding rate as a response value:
Y＝95.78-2.64A-4.23B-2.35C+0.12AB+0.27AC+0.88BC-4.60A2-6.05B2-3.68C2。
to verify the validity of the equation, it was further subjected to analysis of variance, the results of which are shown in table 5. Significance test P<0.0001<0.01, indicating that the model is statistically significant, wherein the significance of the first order terms A (core-wall ratio), B (wall-wall ratio) and C (complex aggregation pH) is extremely significant (P)<0.0001), has significant influence on the microcapsule preparation process; draft term 0.1817>0.05, the mismatching item is not obvious, which shows that the regression equation has good fitting to the experiment, and the factors have strong interaction; determining the coefficient R20.9858, the experimental error is very small, which shows that the fitting degree of the model is good, and the method can be used for analyzing and predicting the process of preparing passion fruit peel anthocyanin microcapsules by a complex coacervation method.
TABLE 5 regression model analysis of variance results
a indicates extreme significance, i.e. P < 0.01;
b indicates significance, i.e. P <0.05.
The process for preparing the passion flower pericarp anthocyanin microcapsules by a single-factor test, Plackett-Burman test design and response surface analysis test optimization complex coacervation method takes a core-wall ratio, a wall material ratio and a complex coacervation pH as variables and an embedding rate as a response value. The model P is less than 0.01, and the model is significant; the mishap P is more than 0.05, and the mishap item is not significant. The regression equation is shown to fit the experiment well. Therefore, the optimal process adopted in the first step of the embodiment 1 is as follows: the core-wall ratio is 1:5.5, the wall material ratio is 5:6, the wall material concentration is 1.5%, the complex coacervation pH is 3.49, the reaction temperature is 40 ℃, the reaction time is 30min, the addition amount of TG enzyme is 30g/100g of gelatin, the embedding rate under the condition is 96.12%, and the effect is optimal in all process parameters.
2 Performance testing of the double-layer microcapsules prepared in the examples of the present invention
2.1 comparative test: the comparative tests were set up as follows:
comparative example 1
A passion flower pericarp anthocyanin single-layer microcapsule is a single-layer microcapsule (single-layer microcapsule) prepared by a complex coacervation method, and comprises the following specific steps:
(1) preparation of gelatin and Arabic gum raw material liquid
Taking gelatin and Arabic gum as wall materials, controlling the wall material ratio of gelatin to Arabic gum to be 5:6, adding the wall materials into distilled water, controlling the wall material concentration to be 1.5%, and stirring in a water bath at 40 ℃ at a rotating speed of 200r/min to fully dissolve the gelatin and the Arabic gum to obtain a raw material solution;
(2) formation of microcapsules
Adding passion flower pericarp anthocyanin as core material into raw material liquid, controlling the core-wall ratio to be 1:5.5, stirring while adding, adjusting pH of the solution to 3.49 with 10% glacial acetic acid after complete dissolution, and performing complex coacervation reaction at 40 ℃ for 30 min;
(3) curing of microcapsules
After the complex coacervation reaction, cooling the obtained microcapsule solution to room temperature, continuing stirring for 1h, then cooling the microcapsule solution to 15 ℃, adding glutamine transaminase according to the addition amount of 30g/100g of gelatin, and continuously stirring for 3h to finish the solidification;
(4) drying of microcapsules
Drying by adopting a spray drying method, wherein the parameters are as follows: the air inlet temperature is 180 ℃, the air outlet temperature is 90 ℃, and the feeding speed is 7.5mL/min, thus obtaining the single-layer microcapsule.
Comparative example 2
A passion flower pericarp anthocyanin double-layer microcapsule is a double-layer microcapsule, and the method comprises the steps of fully mixing 100mL of gum arabic aqueous solution with the mass concentration of 6% with 100mL of single-layer microcapsule wet capsule on the basis of the first step of the embodiment, stirring at the room temperature of 200r/min for 30min, and performing spray drying (the air inlet temperature is 180 ℃, the air outlet temperature is 90 ℃, and the feeding speed is 7.5mL/min) to obtain the double-layer microcapsule (gum arabic-double-layer microcapsule) with the gum arabic as a second-layer wall material.
2.2 Performance testing of products
The same performance tests were performed on the above examples and comparative examples 1-2 as follows:
2.2.1 encapsulation efficiency
The embedding rate is one of important parameters for evaluating the quality of microcapsules, and as shown in FIG. 9, is a single layer microcapsule (comparative example 1), a gum arabic-double layer microcapsule (comparative example 2), and gum arabic/SiO2Comparison of the encapsulation efficiency of the double-layer microcapsules (examples). The embedding rates of the three microcapsules are respectively 96.12%, 97.24% and 97.85%, and therefore, the secondary embedding method can improve the embedding rate of the microcapsules. Arabic gum/SiO2The highest embedding rate of the double-layer microcapsules is due to the nano-SiO2The hydroxyl group and the hydroxyl group on the Arabic gum molecule form a hydrogen bond, so that the microcapsule wall structure is more compact and is not easy to break, and the core material is not easy to flow out.
2.2.2 droplet size
The morphology of the three microcapsules was observed by an optical microscope, and as shown in FIG. 10, (a), (b) and (c) represent a single-layer microcapsule, a gum arabic-double-layer microcapsule and gum arabic/SiO2Double layerPhotographs of the wet capsules of the microcapsules. As can be seen, the wall material forms a gel film to tightly coat the passion flower pericarp anthocyanin, and the microcapsules are spherical. (c) The average particle size of the medium liquid drop is larger than that of the other two microcapsules. This phenomenon is also demonstrated by the average particle size of the droplets measured using software S-EYE 1.4.7.645, shown in figure 11, the microcapsule particle size order being: arabic gum/SiO2Double-layer microcapsules>Arabic gum-double-layer microcapsule>A single layer of microcapsules.
This can be explained by the fact that the microcapsules of larger particle size in the single layer of microcapsules are easily broken during stirring; the gum arabic-double-layer microcapsule wall becomes thicker, so that the microcapsule is more stable; arabic gum/SiO2The droplet size of the double-layer microcapsule is larger, besides the increase of the microcapsule wall thickness, the droplet size is also increased by the nano SiO2The addition of (2) increases the capsule wall strength, and even the microcapsules with large particle size are not easy to break in collision. The subject is to provide a nano SiO2In the mechanical property research of the modified Arabic gum film, nano SiO2The conclusion that the film strength can be improved can also explain the result.
2.2.3 moisture content
The moisture content is an important factor for evaluating the shelf life of the food powder, the moisture content is low, the food powder is not easy to deteriorate, and the shelf life is prolonged. As shown in FIG. 12, single layer microcapsules, gum arabic-double layer microcapsules and gum arabic/SiO were compared2The moisture content of the double-layer microcapsules, gum arabic-double-layer microcapsules was 4.65%, higher than the minimum requirement of powder in food applications (4.00%). Arabic gum/SiO2The water content of the double-layer microcapsule is lowest and is less than 3%, so that the storage is facilitated. The difference is influenced by the water binding capacity of the material, and the nano SiO is added2Nano SiO2The hydroxyl group of (2) forms a hydrogen bond with the hydrophilic group of the arabic gum, and the contact of water molecules with the hydrophilic group of the material can be reduced. This and the object are to nano SiO2The research conclusion of the water vapor permeability of the modified Arabic gum film is consistent, and the nano SiO is properly added2The ability of the material to bind water may be reduced.
2.2.4 appearance Structure
The microcapsule powder prepared by spray drying is ideally in the form of smooth spheres, but in practice, most of the surface of the microcapsule shows wrinkles, depressions and crumbling due to the influence of the wall material and process conditions during the preparation process, because water evaporates rapidly during the drying process, and the wall material tends to be uneven and shrink.
As shown in fig. 13, (a) the surface of the single-layer microcapsule is concave and has more wrinkles; (b) the gum arabic-double-layer microcapsule reduces damage in the spray drying process due to the protection effect of the gum arabic layer; (c) arabic gum/SiO2Although the surface of the double-layer microcapsule is also wrinkled, the double-layer microcapsule is smoother than other two microcapsules, has no obvious crack, and the core material is better wrapped in the wall material, which indicates that nano SiO is added into the microcapsule wall material2The microcapsules can keep an integral structure in the spray drying process.
2.2.5 thermal stability
As shown in FIG. 14, the DSC curves of the three microcapsules are shown, and the single-layer microcapsule, gum arabic-double-layer microcapsule and gum arabic/SiO2The degradation of the double-layer microcapsules is endothermic, with melting temperatures of 82.51 ℃, 127.84 ℃ and 156.12 ℃ respectively. It can be seen that the secondary embedding method improves the thermal stability of the microcapsules.
2.2.6 storage stability
Stability of free passion fruit pericarp anthocyanin and spray dried microcapsule powder samples under light, temperature (4 ℃, 20 ℃, 40 ℃ and 60 ℃) and relative humidity (11%, 33%, 53% and 75%). Reaction rate constant (k), coefficient (R)2) And half-life (t)1/2) The measured values are shown in Table 6.
TABLE 6 reaction rate constant (k), coefficient (R) of microcapsules in different storage environments2) And half-life (t)1/2)
a different capital letter in the upper right of the rate constant (k) indicates that k in the same column is significantly different (P < 0.05);
the different lower case letters in the upper right of the rate constant (k) indicate significant differences in k values (P <0.05) for the same row.
Aiming at the illumination stability, the double-layer microcapsule has stronger protection effect on anthocyanin than the single-layer microcapsule; simultaneously, nano SiO is added2Of Arabic gum/SiO2The half-life of the double-layer microcapsule is 14.18 percent higher than that of the Arabic gum-double-layer microcapsule (Table 6), which indicates that the nano SiO is2The light resistance of the microcapsule can be improved by adding the microcapsule wall material into the microcapsule.
Aiming at the temperature stability, under the condition of lower temperature (4 ℃ and 20 ℃), the free anthocyanin and the microcapsule sample are stable and have no obvious difference (P)>0.05); the temperature rises to 40 ℃, the stability of free anthocyanin begins to be greatly reduced, and t1/2Reduced to 87.45 days, and microencapsulated anthocyanin (single-layer microcapsule, gum arabic-double-layer microcapsule and gum arabic/SiO)2Double-layer microcapsules) effectively protect the core material; at 60 ℃ which is the worst storage condition, the four samples were observed to fade in color and to appear brownish yellow during the experiment, due to the partial conversion of the predominantly red yellow melting salt cation of anthocyanin into colorless methanopseudobase and yellowish chalcone structure.
For humidity stability, the samples have higher stability under dry ambient conditions (11% and 33%); the relative humidity reaches 75%, the wall material is a water-soluble material, so that the permeability and the mechanical property of the wall material can be changed to different degrees after moisture absorption, and the core material is exposed in a high relative humidity environment, the structure changes towards an unstable direction, and the degradation is accelerated; arabic gum/SiO2Double-layer microcapsules at 75% relative humidity t1/2Increased by 25.51% compared with free anthocyanin, and nanometer SiO2Can reduce the water vapor permeation rate of the film, and the nano SiO is added2And the moisture resistance of the microcapsule is also increased in the microcapsule wall material.
The secondary embedding method improves the stability of the microcapsule by increasing the wall thicknessSiO rice2Successful crosslinking with gum arabic improves the photostability and thermal stability of the microcapsules, and can maintain longer t under high humidity conditions1/2。
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (5)
1. A secondary embedding preparation method of passion fruit peel anthocyanin microcapsules comprises the following steps: the method is characterized in that: comprises the steps of
Taking passion flower pericarp anthocyanin as a core material and gelatin and Arabic gum as wall materials, and preparing a single-layer microcapsule wet capsule by a complex coacervation method;
step two, taking nano SiO2Adding into distilled water of 55-65 deg.C, stirring for 25-35min, ultrasonic treating for 1.5-2.5h to obtain stable dispersion, adding acacia into the dispersion, mixing and stirring for 25-35min to obtain nanometer SiO2Modified arabic gum solution;
step three, mixing the nano SiO2Fully mixing the modified Arabic gum solution with the single-layer microcapsule wet capsule, stirring at room temperature of 240r/min for 25-35min, and spray drying to obtain the first-layer wall material of the Arabic gum and the nanometer SiO2The modified Arabic gum is the passion flower pericarp anthocyanin microcapsule with the second layer of wall material.
2. The secondary embedding preparation method of passion flower pericarp anthocyanin microcapsules of claim 1: the method is characterized in that: 0.15g of nano SiO is added into every 100mL of distilled water2Adding 6g of Arabic gum to the mixture, and preparing nano SiO2The modified gum arabic solution was then mixed with 100mL single-layer microcapsule wet capsules.
3. The secondary embedding preparation method of passion flower pericarp anthocyanin microcapsules of claim 1: the method is characterized in that: in the third step, the spray drying conditions are as follows: the air inlet temperature is 180 ℃, the air outlet temperature is 90 ℃, and the feeding speed is 7.5 mL/min.
4. The secondary embedding preparation method of passion flower pericarp anthocyanin microcapsules of claim 1: the method is characterized in that: the specific operation of the first step is as follows:
(1) preparation of gelatin and Arabic gum raw material liquid
Taking gelatin and Arabic gum as wall materials, controlling the wall material ratio of gelatin to Arabic gum to be 5:6, adding the wall materials into distilled water, controlling the wall material concentration to be 1.5%, and stirring in a water bath at 40 ℃ at a rotating speed of 200r/min to fully dissolve the gelatin and the Arabic gum to obtain a raw material solution;
(2) formation of microcapsules
Adding passion flower pericarp anthocyanin as core material into raw material liquid, controlling the core-wall ratio to be 1:5.5, stirring while adding, adjusting pH of the solution to 3.49 with 10% glacial acetic acid after complete dissolution, and performing complex coacervation reaction at 40 ℃ for 30 min;
(3) curing of microcapsules
After the complex coacervation reaction, cooling the obtained microcapsule solution to room temperature, continuing stirring for 1h, then cooling the microcapsule solution to 15 ℃, adding glutamine transaminase according to the addition amount of 30g/100g of gelatin, continuously stirring for 3h, completing solidification, and filtering to obtain the single-layer microcapsule wet capsule.
5. A passion flower pericarp anthocyanin microcapsule is characterized in that: which is obtained by the production method according to any one of claims 1 to 4.
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