Preparation method and application of blueberry anthocyanin microcapsules
Blueberry anthocyanin microcapsules were prepared using composite wall materials and freeze-drying technology, which solved the problem of poor anthocyanin stability and achieved high stability and high encapsulation rate, making them suitable for the food industry.
Patent Information
- Application Number
- CN202310535268.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-05-11
- Publication Date
- 2026-01-20
- Estimated Expiration
- 2043-05-11
AI Technical Summary
Anthocyanins are unstable and easily affected by environmental factors such as temperature, pH, light, metal ions, and oxygen, resulting in low utilization rates.
Blueberry anthocyanins were encapsulated using a composite wall material and freeze-drying technology to prepare blueberry anthocyanin microcapsules. The microcapsule solution consisted of a mixture of maltodextrin, glycerol glycolipids and a thickener. After forming the microcapsule solution, it was then freeze-dried under vacuum.
It improves the stability and antioxidant properties of anthocyanins, enhances the encapsulation rate, and provides better preservation and delivery effects.
Smart Images
Figure CN116571178B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the field of microcapsules, in particular to a preparation method and application of blueberry anthocyanin microcapsules. BACKGROUND
[0002] Anthocyanins are the largest class of natural water-soluble pigments in plants, usually in the form of glycosides, called anthocyanins. Anthocyanins are abundant in nature, have a variety of health benefits, such as anti-inflammatory, anti-diabetic, anti-cancer, high compatibility with biological systems, etc., and are non-toxic, so anthocyanins are considered to be the most suitable natural antioxidants for application in the food industry. However, anthocyanins are a class of unstable compounds, which are easily affected by factors such as pH, light, temperature, enzymes, oxygen and metal ions. Therefore, certain measures need to be taken to protect anthocyanins from adverse external conditions. SUMMARY
[0003] In view of the problems of poor stability, low utilization rate and easy influence of environmental factors such as temperature, pH, light, metal ions and oxygen of anthocyanins in the prior art, the present application provides a microcapsule comprehensive development and application method which can protect anthocyanins from adverse external conditions.
[0004] The method for encapsulating blueberry anthocyanins by using a composite wall material through freeze-drying technology is adopted in the present application, and the prepared blueberry anthocyanin microcapsules have good stability and antioxidant properties.
[0005] The purpose of the present application is achieved by adopting the following technical solutions:
[0006] The first purpose of the present application is to provide a preparation method of blueberry anthocyanin microcapsules, comprising the following steps:
[0007] (1) A certain proportion of maltodextrin, glycolipid and thickening agent are weighed and mixed in deionized water, heated and dissolved, and then stirred uniformly at a certain speed to form a composite wall material solution;
[0008] (2) After the composite wall material solution is cooled, the anthocyanin solution is added to the composite wall material solution, heated and mixed, and then cooled to form a microcapsule solution;
[0009] (3) The water and other solvents are evaporated and removed by using vacuum freeze-drying technology, and anthocyanin microcapsule powder is obtained.
[0010] Preferably, in step (1), the glycolipid includes monogalactosyldiacylglycerol (MGDG) or digalactosyldiacylglycerol (DGDG).
[0011] Preferably, in step (1), the thickening agent includes at least one of gelatin, soybean protein isolate, modified starch, xanthan gum and gum arabic.
[0012] More preferably, the modified starch comprises any one of corn modified starch, potato modified starch, cassava modified starch, rice modified starch, and wheat modified starch.
[0013] Preferably, in step (1), the mass ratio of the malt dextrin, the glyceroglycolipid, the thickening agent, and the deionized water is 5-8:2-4:1-3:100-120.
[0014] Preferably, in step (1), the DE value of the malt dextrin is 15-22.
[0015] Preferably, in step (1), the heating and dissolving is performed in a water bath, and the heating temperature is 60-90℃.
[0016] More preferably, in step (1), the heating and dissolving is performed in a water bath, and the heating temperature is 80℃.
[0017] Preferably, in step (1), the stirring is performed at a rotation speed of 350-650 rpm for 30-60 min.
[0018] Preferably, in step (2), the content of the anthocyanin in the anthocyanin solution is not less than 0.05 mg / mL.
[0019] Preferably, in step (2), the volume ratio of the added anthocyanin solution to the complex wall material solution is 8:1.
[0020] Preferably, in step (2), the content of the anthocyanin in the microcapsule solution is not less than 0.1 μg / mL.
[0021] Preferably, in step (2), the cooling method of the wall material solution is natural cooling to room temperature.
[0022] Preferably, in step (2), the temperature of the prepared microcapsule solution is controlled at 40-80℃ by water bath heating.
[0023] More preferably, in step (2), the temperature of the prepared microcapsule solution is controlled at 60℃ by water bath heating.
[0024] Preferably, in step (3), the vacuum freeze-drying is performed in a vacuum freeze-drying machine at -55 to -50℃.
[0025] Preferably, in step (3), the embedding rate of the anthocyanin in the prepared anthocyanin microcapsule powder reaches 89.21%-97.35%.
[0026] The second object of the present application is to provide a blueberry anthocyanin microcapsule prepared by the above preparation method.
[0027] A third object of the present application is to provide an application of the blueberry anthocyanin microcapsule, and the obtained blueberry anthocyanin microcapsule is used in the preparation of products in the field of food industry.
[0028] Preferably, the product in the field of food industry comprises food additives such as antioxidants, pigments and the like.
[0029] The present application has the following beneficial effects:
[0030] 1. The present application uses blueberry anthocyanin as the core material, and uses malt dextrin, glycolipid and thickening agent as the composite wall material, and a blueberry anthocyanin microcapsule is prepared, which has very good embedding rate and stability. The present application uses the composite wall material to prepare the microcapsule by freeze-drying technology, which provides a research basis for better development and utilization of blueberry anthocyanin, and can derive anthocyanin microcapsules with various properties through the technology.
[0031] 2. Malt dextrin has good emulsifying effect and thickening effect, and can enhance the dispersibility and solubility of the product, but the film-forming property of malt dextrin is not very good, especially some malt dextrin with a slightly high DE value, which cannot well retain the embedding material after drying. Glycolipid is an important component of cell membrane, which is a glycolipid compound combined by diglyceride and galactose by glycosidic bond. The glycosidic bond in glycolipid has strong self-assembly and variability, which is beneficial to emulsification and aggregation of high molecular sugar compounds, and thus can enhance the film-forming property of the malt dextrin with a slightly high DE value, thereby promoting the stability of the embedding wall material.
[0032] 3. The present application uses malt dextrin and glycolipid as the main components of the wall material, and then adds thickening agent to form a composite wall material. The three wall material components are all food-grade materials, and can provide effective functional effects for specific applications as a composite packaging material.
[0033] 4. The several thickening agents used in the present application all have the properties of no odor, no taste and insoluble in cold water, can absorb multiple amounts of cold water to swell and soften, can be dissolved in hot water, and can form a gel after cooling.
[0034] 5. Glycolipid is an important component of cell membrane, and also has various biological activities such as antioxidant, antiviral, antibacterial, antitumor and anti-inflammatory. The use of glycolipid as the component of the wall material can increase more functionality of the anthocyanin microcapsule.
[0035] 6、The present application is the use of freeze-drying technology to develop anthocyanin microcapsules, freeze-drying is considered to be a suitable method for drying heat-sensitive materials, which refers to the process of extracting water from frozen materials without melting water in a high-vacuum atmosphere using the principle of ice sublimation. Since this process is carried out in a vacuum and at a lower temperature, adverse reactions are greatly reduced. BRIEF DESCRIPTION OF DRAWINGS
[0036] The present application is further illustrated by the accompanying drawings, but the embodiments in the drawings do not constitute any limitation on the present application, and other drawings can also be obtained by those of ordinary skill in the art without creative labor on the basis of the following drawings.
[0037] Figure 1 is the FTIR graph of anthocyanin (ANS) and the microcapsules obtained in Examples 1-5; wherein a is Example 1, b is Example 2, c is Example 3, d is Example 4, e is Example 5;
[0038] Figure 2 is the SEM graph of anthocyanin (ANS) and the microcapsules obtained in Examples 1-5; wherein a represents Example 1, b represents Example 2, c represents Example 3, wherein d represents Example 4, wherein e represents Example 5, wherein f represents anthocyanin powder (ANS) that has not been prepared into microcapsules;
[0039] Figure 3 is the XRD graph of anthocyanin (ANS) and the microcapsules obtained in Examples 1-5; wherein a represents Example 1, b represents Example 2, c represents Example 3, wherein d represents Example 4, wherein e represents Example 5, wherein f represents anthocyanin powder (ANS) that has not been prepared into microcapsules. DETAILED DESCRIPTION
[0040] In order to more clearly illustrate the present application, the technical features, objectives and beneficial effects of the present application are more clearly understood, the technical solutions of the present application are described in detail as follows, but it cannot be understood as limiting the scope of the present application.
[0041] Microencapsulation is a physical and chemical method, and also a technology that can enhance or protect the characteristics of core materials. Generally speaking, there are two main reasons for the good effect of the encapsulation of bioactive substances. First, microencapsulation provides an environment that can protect the loss or degradation of the activity of the compound. These conditions usually involve high temperature, light, the presence of metal ions, moisture, unfavorable pH conditions and oxygen, etc.; second, microencapsulation can promote the controlled release of the target adsorption area. Microencapsulation also solves the problems of handling and masking bad flavors during transportation, diluting bioactive compounds and two or more related problems.
[0042] Microencapsulation is to protect the core material from the outside environment by building a physical and chemical barrier between anthocyanins and external environmental factors, to achieve the preservation and delivery of anthocyanins in harsh in-vivo digestion environment. Such capsules with size from microns to nanometers are increasingly attracting people's attention, and have wide applications in pharmaceutical, cosmetic, food and agricultural industries. Spray drying and freeze drying are often used to encapsulate functional materials, however, anthocyanins are heat sensitive, and the spray drying process is prone to produce particles with high surface-to-volume ratio, which causes heat exposure and leads to the degradation of anthocyanins and the reduction of antioxidant activity of microcapsules. In addition, the loss of product on the wall of the drying chamber will cause a lot of waste of material. The non-uniform particle size distribution, large particles and various morphological characteristics of the powder limit their food applications. On the contrary, freeze drying is mainly developed for the encapsulation of such sensitive compounds. It is mainly related to its process, in which mass transfer is not completed by evaporation. The frozen feed emulsion is sublimed, thereby producing a powder. Therefore, using blueberry anthocyanins as the core material and adopting composite wall material by freeze drying technology to prepare microcapsules can provide a research basis for the development and utilization of blueberry anthocyanins, and also can provide technical support and theoretical reference for the application of anthocyanins in food industry.
[0043] The raw materials, reagents or devices used in the following examples, unless otherwise specified, can be obtained from conventional commercial channels or can be obtained by existing known methods.
[0044] The DE value of malt dextrin used in the examples is 20.
[0045] The present application is further described in conjunction with the following examples.
[0046] Example 1
[0047] (1) Malt dextrin, MGDG and gelatin were added into deionized water respectively, and the mass ratio of malt dextrin, MGDG, gelatin and deionized water was 7:3:2:110. After being dissolved in water bath at 80℃, the composite wall material solution was formed by stirring at a speed of 500r / min for 40min;
[0048] (2) After the wall material solution was cooled at room temperature, the anthocyanin solution with a concentration of 0.05mg / mL was mixed with the wall material solution according to the volume ratio of 8:1. After being heated and mixed uniformly at 60℃ for 40min, the microcapsule solution was formed by natural cooling to room temperature;
[0049] (3) The water and other solvents were evaporated by vacuum freeze drying technology at-50℃ and vacuum degree of 0bar, and the anthocyanin microcapsule powder ANS / MD / MGDG was obtained. The anthocyanin embedding rate was 97.35% measured by pH differential method.
[0050] Example 2
[0051] (1) Maltodextrin, MGDG and soybean protein isolate were added into deionized water respectively, the mass ratio of maltodextrin, MGDG, soybean protein isolate and deionized water was 6:3:2:100, after dissolving in water bath at 90℃, stirring at 550r / min for 30min, the composite wall material solution was formed;
[0052] (2) After the wall material solution was cooled at room temperature, the anthocyanin solution with a concentration of 0.05mg / mL was mixed with the wall material solution according to the volume ratio of 8:1, after heating and mixing uniformly at 40℃ for 40min, it was naturally cooled to room temperature, forming the microcapsule solution;
[0053] (3) The water and other solvents were evaporated by vacuum freeze-drying technology at-50℃ and 0bar vacuum degree, anthocyanin microcapsule powder was obtained, the anthocyanin embedding rate was 94.26% measured by pH differential method.
[0054] Example 3
[0055] (1) Maltodextrin, DGDG and corn modified starch were added into deionized water respectively, the mass ratio of maltodextrin, DGDG, corn modified starch and deionized water was 5:4:3:120, after dissolving in water bath at 70℃, stirring at 650r / min for 50min, the composite wall material solution was formed;
[0056] (2) After the wall material solution was cooled at room temperature, the anthocyanin solution with a concentration of 0.05mg / mL was mixed with the wall material solution according to the volume ratio of 8:1, after heating and mixing uniformly at 60℃ for 40min, it was naturally cooled to room temperature, forming the microcapsule solution;
[0057] (3) The water and other solvents were evaporated by vacuum freeze-drying technology at-50℃ and 0bar vacuum degree, anthocyanin microcapsule powder was obtained, the anthocyanin embedding rate was 96.23% measured by pH differential method.
[0058] Example 4
[0059] (1) Maltodextrin, DGDG and xanthan gum were added into deionized water respectively, the mass ratio of maltodextrin, DGDG, xanthan gum and deionized water was 6:4:2:100, after dissolving in water bath at 80℃, stirring at 600r / min for 60min, the composite wall material solution was formed;
[0060] (2) After the wall material solution was cooled at room temperature, the anthocyanin solution with a concentration of 0.05mg / mL was mixed with the wall material solution according to the volume ratio of 8:1, after heating and mixing uniformly at 60℃ for 40min, it was naturally cooled to room temperature, forming the microcapsule solution;
[0061] (3) The water and other solvents were evaporated by vacuum freeze-drying technology at -50°C and 0 bar vacuum, to obtain anthocyanin microcapsule powder. The anthocyanin embedding rate was 93.35% as measured by pH differential method.
[0062] Example 5
[0063] (1) Maltodextrin, MGDG and gum arabic were added into deionized water respectively, and the mass ratio of maltodextrin, MGDG, gum arabic and deionized water was 8:2:1:100-120. After being dissolved in water bath at 60°C, the complex wall material solution was stirred at a speed of 350 r / min for 30 min;
[0064] (2) After the wall material solution was cooled at room temperature, the anthocyanin solution with a concentration of 0.05 mg / mL was mixed with the wall material solution at a volume ratio of 8:1. After being heated and mixed uniformly at 60°C for 40 min, the microcapsule solution was naturally cooled to room temperature;
[0065] (3) The water and other solvents were evaporated by vacuum freeze-drying technology at -50°C and 0 bar vacuum, to obtain anthocyanin microcapsule powder. The anthocyanin embedding rate was 93.35% as measured by pH differential method.
[0066] Comparative Example
[0067] (1) Maltodextrin and gelatin were added into deionized water respectively, and the mass ratio of maltodextrin, gelatin and deionized water was 10:2:110. After being dissolved in water bath at 80°C, the complex wall material solution was stirred at a speed of 500 r / min for 40 min;
[0068] (2) After the wall material solution was cooled at room temperature, the anthocyanin solution with a concentration of 0.05 mg / mL was mixed with the wall material solution at a volume ratio of 8:1. After being heated and mixed uniformly at 60°C for 40 min, the microcapsule solution was naturally cooled to room temperature;
[0069] (3) The water and other solvents were evaporated by vacuum freeze-drying technology at -50°C and 0 bar vacuum, to obtain anthocyanin microcapsule powder. The anthocyanin embedding rate was 93.35% as measured by pH differential method.
[0070] Experimental Example
[0071] 1. Detection method of embedding rate:
[0072] In specific embodiments of the present application, the content of anthocyanins in the microcapsules and anthocyanin solution is determined by pH differential method. The absorbance of the solution sample is quantitatively determined at wavelengths of 520 nm and 700 nm on an ultraviolet spectrophotometer (model TU-1900), and the content of anthocyanins is calculated by the following formula.
[0073]
[0074] In the formula, A pH1.0 and A pH4.5 are the maximum absorbance of the sample diluted with buffer at pH 1.0 and pH 4.5, respectively;
[0075] MW is the molecular weight (449.2 g / mol);
[0076] DF is the dilution factor;
[0077] ε is the extinction coefficient (26,900 mol / (L·cm -1 )) ;
[0078] L is the optical path length (1 cm);
[0079] V is the final volume (mL);
[0080] m is the mass (g).
[0081] The microcapsule embedding rate is calculated according to the following formula:
[0082]
[0083] In the formula, M1 refers to the content of total anthocyanins in the microcapsules (mg);
[0084] M2 refers to the content of anthocyanins on the surface of the microcapsules (mg).
[0085] 2. Storage stability detection:
[0086] Since light and temperature generally have a greater impact on anthocyanins, the present application detects the storage stability of anthocyanin microcapsules under temperature and light, respectively. The light intensity of the fluorescent lamp is 1000 lux, and the natural light is indoor natural light with a light intensity ranging from 200 to 600 lux. The specific detection results are shown in Table 1 below:
[0087] Table 1 Anthocyanin retention rate after different temperature or light treatment
[0088]
[0089] As can be seen from Table 1, after treatment under different temperature or light conditions, the blueberry anthocyanin microcapsules prepared by the present application using maltodextrin, glycolipid and thickening agent as the composite wall material have higher retention rate than the blueberry anthocyanin microcapsules prepared in the comparative examples using traditional maltodextrin and thickening agent as the composite wall material, which indicates that the blueberry anthocyanin microcapsules prepared in the present application have better stability, and thus it can also be seen that the addition of glycolipid as the additive of the wall material has a good enhancing effect on the stability of the wall material.
[0090] Finally, it should be noted that the above examples are only used to illustrate the technical solutions of the present application, and are not intended to limit the scope of protection of the present application. Although the present application has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solutions of the present application can be modified or replaced by equivalents without departing from the essence and scope of the technical solutions of the present application.
Claims
1. A method for preparing blueberry anthocyanin microcapsules, characterized in that, Includes the following steps: (1) Weigh out maltodextrin, glycerol glycolipid and thickener according to the proportion and mix them in deionized water. After heating and dissolving, stir evenly at a certain speed to form a composite wall material solution. (2) After the composite wall material solution cools down, add the anthocyanin solution to the composite wall material solution, heat and mix well, and after cooling, form a microcapsule solution; (3) Using vacuum freeze-drying technology, water and other solvents are evaporated and removed to obtain anthocyanin microcapsule powder; In step (1), the mass ratio of the maltodextrin, the glycerol glycolipid, the thickener and the deionized water is 5-8:2-4:1-3:100-120; In step (1), the glycerol glycolipid includes monogalactosylglycerol diglyceride MGDG or digalactosylglycerol diglyceride DGDG; In step (1), the thickener includes at least one of gelatin, soy protein isolate, modified starch, xanthan gum, and gum arabic.
2. The method for preparing blueberry anthocyanin microcapsules according to claim 1, characterized in that, The modified starch includes any one of corn modified starch, potato modified starch, cassava modified starch, rice modified starch, and wheat modified starch.
3. The method for preparing blueberry anthocyanin microcapsules according to claim 1, characterized in that, In step (1), the heating and dissolving is carried out in a water bath at a temperature of 60-90°C; the stirring is carried out at a speed of 350-650 rpm for 30-60 minutes.
4. The method for preparing blueberry anthocyanin microcapsules according to claim 1, characterized in that, In step (2), the anthocyanin content in the anthocyanin solution is not less than 0.05 mg / mL; the volume ratio of the anthocyanin solution to the composite wall material solution is 8:
1.
5. The method for preparing blueberry anthocyanin microcapsules according to claim 1, characterized in that, In step (3), the vacuum freeze drying is carried out in a vacuum freeze dryer at -55~-50℃.
6. A blueberry anthocyanin microcapsule, characterized in that, It was prepared using the preparation method described in claim 1.
7. An application of the blueberry anthocyanin microcapsules as described in claim 6, characterized in that, The blueberry anthocyanin microcapsules are used in the preparation of products in the food industry.