CN111569795A - Process method for preparing black rice anthocyanin microcapsules by using microcapsule granulator - Google Patents
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Abstract
The invention discloses a process method for preparing black rice anthocyanin microcapsules by using a microcapsule granulator. The method comprises the steps of taking sodium alginate as a wall material and black rice anthocyanin as a core material, preparing the black rice anthocyanin microcapsule by ionic gelation and adopting a double-nozzle embedding method by utilizing a microcapsule embedding machine. Compared with the traditional method, the microcapsule granulator has mild preparation conditions, simple operation and short-term large-scale preparation. The black rice anthocyanin microcapsules prepared by adopting a double-nozzle embedding method have the characteristics of uniform shape, small particles, good wrapping property and the like. The black rice anthocyanin microcapsules with good functional properties can expand the application approach of black rice anthocyanin and have good guiding function on the embedded delivery of functional components.
Description
Technical Field
The invention belongs to a microencapsulation technology, and mainly relates to a process method for preparing black rice anthocyanin microcapsules by using a microcapsule granulator.
Background
The black rice anthocyanin as a natural edible pigment has the advantages of high safety, rich resources, nutrition, pharmacological action and the like compared with a synthetic pigment. Researches prove that the black rice anthocyanin is the most effective natural water-soluble free radical scavenger discovered so far, can activate retinal enzyme and enhance the vision of human eyes. And has effects of protecting blood vessel, improving memory and resisting aging.
Environmental factors such as acid, alkali, oxidant, light radiation and the like can act on the black rice anthocyanin, so that the chemical structure of the black rice anthocyanin is easily changed. The instability of the chemical structure of the black rice anthocyanin seriously influences the exertion of the physiological activity of the black rice anthocyanin and even disappears the activity. The storage and application of the black rice anthocyanin have certain limitations, and the application of the black rice anthocyanin in the fields of food and the like is severely limited.
The microcapsule is a vesicle which takes polymer as a wall shell, embeds and seals solid, liquid or gas substances. The core material can be wrapped by the material, and is isolated from the external environment, so that the original characteristics of the material are kept. In recent years, microcapsules have been widely used in the fields of medicines, foods, printing and dyeing, and the like. Therefore, the black rice anthocyanin is embedded by utilizing the microcapsule technology, the biological activity of the black rice anthocyanin is protected, and the black rice anthocyanin has great development potential.
The microcapsule granulator can decompose the controlled sodium alginate laminar flow liquid into liquid beads with uniform size through jet flow of a nozzle under high pressure by high-frequency vibration. The surface of the bead is charged like a charge when it passes through an electric field between the nozzle and the electrode. The microcapsules are formed by ion exchange reaction in the calcium chloride solution received below. Then the liquid beads are separated from each other due to the action of electrostatic force between the liquid beads, and the microcapsule is prepared.
Microencapsulation methods currently used in the food industry are: (1) spray drying method (2), spray cooling solidification method (3), oil phase separation method (4), water phase separation method (5), molecular microcapsule method (6), extrusion method (7), adsorption method and the like, but the method is limited by preparation process and equipment conditions, and the prior literature experiments mostly adopt an orifice method or an extrusion gel method to prepare microcapsules. But the major disadvantage is that the beads formed are large in diameter and are not achieved using size reduction techniques such as extrusion (electrostatic, jet cutting), spray drying, film or pressurized solvent. The black rice anthocyanin is sensitive to environmental conditions, and a method for preparing the black rice anthocyanin in large scale, such as a spray drying method, an air suspension method and the like, can damage the black rice anthocyanin. The microcapsule granulator can make liquid beads be shaped under extremely low shearing force, the granulation speed is fast and can reach 1000 granules per second at most, and the relative standard deviation of the microcapsule size at micron level is only about 5%. The microcapsule embedding machine has the characteristics of stability and high efficiency, and is suitable for popularization and industrial production of active substances. And can effectively isolate the effect of the environmental factors on the black rice anthocyanin. The processing adaptability such as photosensitivity, heat sensitivity and the like is changed, the original chemical property and biological activity are kept, and the controllable release is realized. Realizes the reduction of raw material cost and short-time mass preparation on the basis of keeping the product quality, thereby having great application potential.
Disclosure of Invention
The invention provides a process method for preparing black rice anthocyanin microcapsules by using a microcapsule granulator, which can embed black rice anthocyanin under a mild condition, keep the activity of the black rice anthocyanin and form microcapsules with uniform shapes and moderate sizes. The characteristics of stability and high efficiency are suitable for the popularization and the industrial production of the black rice anthocyanin product.
The technical problem to be solved by the invention is realized by the following technical scheme:
(1) and (3) purifying black rice anthocyanin: purifying black rice anthocyanin by using an elution adsorption method, wherein the elution adsorption method is to adsorb the black rice anthocyanin after impurity removal by using a solid phase extraction column, elute insoluble impurities by using an acidified aqueous solution, elute polyphenols by using an ethyl acetate solution, and elute the black rice anthocyanin on the adsorption column by using an acidified methanol solution. And then, removing the methanol by rotary evaporation by using a rotary evaporator to obtain pure black rice anthocyanin. Performing quantitative analysis on the purified black rice anthocyanin solution by using high performance liquid chromatography;
(2) preparation of sodium alginate solution: dissolving 1.5-2.4g of sodium alginate in 100mL of distilled water, stirring at 55-65 ℃ for 30min, and cooling to room temperature to obtain a sodium alginate solution;
(3) preparing black rice anthocyanin microcapsules: the black rice anthocyanin microcapsules are prepared by ion gelation and a double-nozzle embedding method by using a microcapsule embedding machine. Adding 2mg/mL anthocyanin solution serving as a core material into a pressure-resistant bottle matched with an instrument. Sodium alginate as wall material is added into another pressure-resistant bottle according to the volume ratio of the core to the wall being 1:2-5 (v/v). The aperture of the core material nozzle is 200 and 750 mu m, and the wall material nozzles are all selected to be nozzles with the aperture larger than 100 mu m of the core material nozzle. The distance between the spray head and the liquid level of the receiving solution is 10 cm. The pressure of the flow rate regulating valve to the conduit is regulated to ensure that the core material solution and the wall material solution are sucked into the microcapsule embedding machine according to the required volume ratio. After the core material solution and the wall material solution are simultaneously sucked by a microcapsule embedding machine, the core material solution and the wall material solution are dispersed into small droplets under the action of high-frequency oscillation and static electricity, the small droplets are dripped into 150mL of calcium chloride solution with the concentration of 1.0-2.5%, and the solution is solidified for 10min to form a film. And (3) carrying out vacuum filtration on the obtained mixed solution of the anthocyanin microcapsules and calcium chloride until solid and liquid are completely separated and no liquid drips to obtain the black rice anthocyanin microcapsules.
And (2) eluting insoluble impurities from the acidified water solution in the step (1), eluting polyphenols from an ethyl acetate solution, and eluting the black rice anthocyanin on the adsorption column from an acidified methanol solution. And then, removing the methanol by rotary evaporation by using a rotary evaporator to obtain pure black rice anthocyanin.
The best mass of the sodium alginate dissolved in the distilled water in the step (2) is 1.8g, and the best stirring temperature is 60 ℃.
The core-wall ratio of the black rice anthocyanin as the core material to the sodium alginate as the wall material in the step (3) is 1:3, the concentration of calcium chloride is 1.5% (w/v), the pore diameter of a nozzle of the core material is 450 mu m, the pore diameter of a nozzle of the wall material is 550 mu m, and the distance between the nozzle and the calcium chloride solution is 10 cm.
And (3) the microcapsule granulator has the vibration frequency of 400Hz, the voltage of 1800V, the heating temperature of 50 ℃ and the pressure of 200 mbar.
The invention provides a process method for preparing black rice anthocyanin microcapsules by using a microcapsule granulation instrument and adopting a double-nozzle embedding method, which takes sodium alginate as a wall material, black rice anthocyanin as a core material and black rice anthocyanin embedding rate as an investigation index, optimizes process parameters for preparing the black rice anthocyanin microcapsules, expands application approaches of the black rice anthocyanin, and has a good guiding effect on the sub-package embedding delivery of functional components.
Drawings
FIG. 1 is a general process route diagram of the present invention.
FIG. 2 is a graph showing the effect of core wall volume ratio on the rate of black rice anthocyanin incorporation.
FIG. 3 shows the effect of calcium chloride concentration on the rate of incorporation of anthocyanin in black rice.
FIG. 4 shows the effect of sodium alginate concentration on the rate of embedding of anthocyanin in black rice.
FIG. 5 shows the effect of the nozzle aperture on the rate of embedding of anthocyanin in black rice.
Fig. 6 and 7 are images of black rice anthocyanin microcapsules prepared by a microcapsule granulator observed by a microscope.
Detailed Description
The following detailed description of specific embodiments of the present invention is provided to illustrate and explain the present invention and to be understood not to limit the present invention.
The process method for preparing the black rice anthocyanin microcapsules by the microcapsule granulator comprises the following steps:
(1) and (3) purifying black rice anthocyanin: purifying black rice anthocyanin by using an elution adsorption method, wherein the elution adsorption method is to adsorb the black rice anthocyanin after impurity removal by using a solid phase extraction column, elute insoluble impurities by using an acidified aqueous solution, elute polyphenols by using an ethyl acetate solution, and elute the black rice anthocyanin on the adsorption column by using an acidified methanol solution. And then, removing the methanol by rotary evaporation by using a rotary evaporator to obtain pure black rice anthocyanin.
(2) Preparation of sodium alginate solution: dissolving sodium alginate in distilled water, stirring at 60 deg.C for 30min, and cooling to room temperature to obtain sodium alginate solution;
(3) preparing black rice anthocyanin microcapsules: the black rice anthocyanin microcapsules are prepared by ion gelation and a double-nozzle embedding method by using a microcapsule embedding machine. Adding the anthocyanin solution serving as a core material into a pressure-resistant bottle matched with an instrument. Sodium alginate is used as wall material and added into another pressure-resistant bottle. Selecting a proper pore diameter of the core material sprayer, and selecting a sprayer with the pore diameter larger than 100 mu m of the core material sprayer as the wall material sprayer. The distance between the spray head and the liquid level of the receiving solution is 10 cm. The vibration frequency of the microcapsule granulator is 400Hz, the voltage is 1800V, the heating temperature is 50 ℃, and the pressure is 200 mbar. The pressure of the flow rate regulating valve to the conduit is regulated to ensure that the core material solution and the wall material solution are sucked into the microcapsule embedding machine according to the required volume ratio. After the core material solution and the wall material solution are simultaneously sucked by a microcapsule embedding machine, the core material solution and the wall material solution are dispersed into small droplets under the action of high-frequency oscillation and static electricity, the small droplets are dripped into a calcium chloride solution, and the calcium chloride solution is solidified for 10min to form a film. And (3) carrying out vacuum filtration on the obtained mixed solution of the anthocyanin microcapsules and calcium chloride until solid and liquid are completely separated and no liquid drips to obtain the black rice anthocyanin microcapsules.
Example 1:
and (3) purifying black rice anthocyanin: purifying black rice anthocyanin by using an elution adsorption method, wherein the elution adsorption method is to adsorb the black rice anthocyanin after impurity removal by using a solid phase extraction column, elute insoluble impurities by using an acidified aqueous solution, elute polyphenols by using an ethyl acetate solution, and elute the black rice anthocyanin on the adsorption column by using an acidified methanol solution. And then, removing the methanol by rotary evaporation by using a rotary evaporator to obtain pure black rice anthocyanin. Performing quantitative analysis on the purified black rice anthocyanin solution by using high performance liquid chromatography; preparation of sodium alginate solution: dissolving 1.8g of sodium alginate in 100mL of distilled water, stirring at 60 ℃ for 30min, and cooling to room temperature to obtain a sodium alginate solution; preparing black rice anthocyanin microcapsules: the black rice anthocyanin microcapsules are prepared by ion gelation and a double-nozzle embedding method by using a microcapsule embedding machine. Adding 2mg/mL anthocyanin solution serving as a core material into a pressure-resistant bottle matched with an instrument. Sodium alginate as wall material is added into another pressure-resistant bottle according to the volume ratio of the core to the wall being 1: 3. The aperture of the core material sprayer is 450 microns, and the wall material sprayer is a sprayer with the aperture larger than 100 microns of the core material sprayer. The distance between the spray head and the liquid level of the receiving solution is 10 cm. The vibration frequency of the microcapsule granulator is 400Hz, the voltage is 1800V, the heating temperature is 50 ℃, and the pressure is 200 mbar. The pressure of the flow rate regulating valve to the conduit is regulated to ensure that the core material solution and the wall material solution are sucked into the microcapsule embedding machine according to the required volume ratio. After the core material solution and the wall material solution are simultaneously sucked by a microcapsule embedding machine, the core material solution and the wall material solution are dispersed into small droplets under the action of high-frequency oscillation and static electricity, the small droplets are dripped into 150mL of 1.5 percent calcium chloride solution, and the solution is solidified for 10min to form a film. And (3) carrying out vacuum filtration on the obtained mixed solution of the anthocyanin microcapsules and calcium chloride until solid and liquid are completely separated and no liquid drips to obtain the black rice anthocyanin microcapsules, wherein the embedding rate reaches 73.71%.
Example 2:
and (3) purifying black rice anthocyanin: purifying black rice anthocyanin by using an elution adsorption method, wherein the elution adsorption method is to adsorb the black rice anthocyanin after impurity removal by using a solid phase extraction column, elute insoluble impurities by using an acidified aqueous solution, elute polyphenols by using an ethyl acetate solution, and elute the black rice anthocyanin on the adsorption column by using an acidified methanol solution. And then, removing the methanol by rotary evaporation by using a rotary evaporator to obtain pure black rice anthocyanin. Performing quantitative analysis on the purified black rice anthocyanin solution by using high performance liquid chromatography; preparation of sodium alginate solution: dissolving 2.1g of sodium alginate in 100mL of distilled water, stirring at 60 ℃ for 30min, and cooling to room temperature to obtain a sodium alginate solution; preparing black rice anthocyanin microcapsules: the black rice anthocyanin microcapsules are prepared by ion gelation and a double-nozzle embedding method by using a microcapsule embedding machine. Adding 2mg/mL anthocyanin solution serving as a core material into a pressure-resistant bottle matched with an instrument. Sodium alginate as wall material is added into another pressure-resistant bottle according to the volume ratio of the core to the wall being 1: 2. The aperture of the core material sprayer is 450 microns, and the wall material sprayer is a sprayer with the aperture larger than 100 microns of the core material sprayer. The distance between the spray head and the liquid level of the receiving solution is 10 cm. The vibration frequency of the microcapsule granulator is 400Hz, the voltage is 1800V, the heating temperature is 50 ℃, and the pressure is 200 mbar. The pressure of the flow rate regulating valve to the conduit is regulated to ensure that the core material solution and the wall material solution are sucked into the microcapsule embedding machine according to the required volume ratio. After the core material solution and the wall material solution are simultaneously sucked by a microcapsule embedding machine, the core material solution and the wall material solution are dispersed into small droplets under the action of high-frequency oscillation and static electricity, the small droplets are dripped into 150mL of 1.5 percent calcium chloride solution, and the solution is solidified for 10min to form a film. And (3) carrying out vacuum filtration on the obtained mixed solution of the anthocyanin microcapsules and calcium chloride until solid and liquid are completely separated and no liquid drips to obtain the black rice anthocyanin microcapsules, wherein the embedding rate reaches 67.44%.
Example 3:
and (3) purifying black rice anthocyanin: purifying black rice anthocyanin by using an elution adsorption method, wherein the elution adsorption method is to adsorb the black rice anthocyanin after impurity removal by using a solid phase extraction column, elute insoluble impurities by using an acidified aqueous solution, elute polyphenols by using an ethyl acetate solution, and elute the black rice anthocyanin on the adsorption column by using an acidified methanol solution. And then, removing the methanol by rotary evaporation by using a rotary evaporator to obtain pure black rice anthocyanin. Performing quantitative analysis on the purified black rice anthocyanin solution by using high performance liquid chromatography; preparation of sodium alginate solution: dissolving 1.8g of sodium alginate in 100mL of distilled water, stirring at 60 ℃ for 30min, and cooling to room temperature to obtain a sodium alginate solution; preparing black rice anthocyanin microcapsules: the black rice anthocyanin microcapsules are prepared by ion gelation and a double-nozzle embedding method by using a microcapsule embedding machine. Adding 2mg/mL anthocyanin solution serving as a core material into a pressure-resistant bottle matched with an instrument. Sodium alginate as wall material is added into another pressure-resistant bottle according to the volume ratio of the core to the wall being 1: 4. The aperture of the core material sprayer is 750 mu m, and the wall material sprayer is a sprayer with the aperture larger than 100 mu m of the core material sprayer. The distance between the spray head and the liquid level of the receiving solution is 10 cm. The vibration frequency of the microcapsule granulator is 400Hz, the voltage is 1800V, the heating temperature is 50 ℃, and the pressure is 200 mbar. The pressure of the flow rate regulating valve to the conduit is regulated to ensure that the core material solution and the wall material solution are sucked into the microcapsule embedding machine according to the required volume ratio. After the core material solution and the wall material solution are simultaneously sucked by a microcapsule embedding machine, the core material solution and the wall material solution are dispersed into small droplets under the action of high-frequency oscillation and static electricity, the small droplets are dripped into 150mL of 1.5 percent calcium chloride solution, and the solution is solidified for 10min to form a film. And (3) carrying out vacuum filtration on the obtained mixed solution of the anthocyanin microcapsules and calcium chloride until solid and liquid are completely separated and no liquid drips to obtain the black rice anthocyanin microcapsules, wherein the embedding rate reaches 69.68%.
Analysis of black rice anthocyanin microcapsule product prepared by microcapsule granulator:
1. determination of encapsulation efficiency of microcapsules
And (3) determining the embedding rate of the black rice anthocyanin microcapsules: and (3) measuring the content of the black rice anthocyanin in the filtrate after suction filtration during the preparation of the black rice anthocyanin microcapsules. And calculating the embedding rate of the black rice anthocyanin microcapsules according to a formula.
In the formula:
w- (black rice anthocyanin) the embedding rate of the microcapsules,%;
A1-content of black rice anthocyanin in filtrate, g;
A2-total content of black rice anthocyanins used for the preparation of microcapsules, g.
2. Influence of core wall volume ratio on black rice anthocyanin embedding rate
Taking a black rice anthocyanin solution of 2mg/mL, and respectively preparing the black rice anthocyanin solution according to the volume ratio of the core wall (v/v): sodium alginate solutions of 1:2, 1:3, 1:4, 1:5 and 2.1% (w/v) are respectively placed in the core material pressure-resistant bottle and the wall material pressure-resistant bottle. A core material spray head with the aperture of 450 microns and a wall material spray head with the aperture of 550 microns are used, the spray heads are 10cm away from the calcium chloride solution, and the stirring speed of the calcium chloride solution is 300-400 rpm. The parameters of the microcapsule granulator are set as the vibration frequency of 400Hz, the voltage of 1800V, the heating temperature of 50 ℃ and the pressure of 200 mbar. The solution is dispersed into small drops by the suction and high-frequency oscillation of a microcapsule granulator, and the small drops are dripped into 150mL of 2.0% calcium chloride solution and solidified for 10min to form a film. The resulting mixed solution of microcapsules and calcium chloride was vacuum filtered until complete separation with no liquid dripping, and the filtrate volume was read. And (4) measuring the embedding rate. The effect of core wall volume ratio on black rice anthocyanin inclusion rate is shown in FIG. 2.
As shown in fig. 2, the anthocyanin embedding rate increases from the core-wall ratio of 1:2 to reach a maximum at the core-wall ratio of 1: 3. Subsequently, the rate of anthocyanin incorporation began to decrease. Too high a sodium alginate content results in a reduced entrapment rate, which may be associated with shrinkage of the beads during gelation. When the volume ratio of the core material is large, incomplete wrapping of the core material by the wall material can be caused, and the embedding rate can also be reduced.
3. Influence of calcium chloride concentration on black rice anthocyanin embedding rate
Taking 2mg/mL black rice anthocyanin solution, and respectively placing the sodium alginate solution in a core material pressure bottle and a wall material pressure bottle according to the volume ratio of 1:3 of the core wall to 2.1% (w/v). A microcapsule granulator is used, a core material spray head with the aperture of 450 microns and a wall material spray head with the aperture of 550 microns are selected, and the distance between the spray heads and the calcium chloride solution is 10 cm. The parameters of the microcapsule granulator are set as the vibration frequency of 400Hz, the voltage of 1800V, the heating temperature of 50 ℃ and the pressure of 200 mbar. The solution is dispersed into small droplets by the suction of a microcapsule granulator and high-frequency oscillation, and the small droplets are respectively added into 150mL of calcium chloride solution with the concentration of 1.0%, 1.5%, 2.0% and 2.5% (w/v), and solidified for 10min to form a film. The resulting mixed solution of microcapsules and calcium chloride was vacuum filtered until complete separation with no liquid dripping, and the filtrate volume was read. And (4) measuring the embedding rate. The effect of calcium chloride concentration on the rate of incorporation of black rice anthocyanin is shown in FIG. 3.
In the microcapsule forming process, calcium chloride is used as a curing agent to react with sodium alginate to form a calcium alginate gel shell to wrap anthocyanin. Therefore, calcium chloride may have an effect on the embedding effect of anthocyanin. As shown in fig. 3, the anthocyanin-embedding rate increased from 1% calcium chloride concentration to a maximum at 1.5% calcium chloride concentration. The rate of anthocyanin incorporation then begins to decrease as the calcium chloride concentration increases. The moderate increase of the concentration of the calcium chloride can lead the crosslinking of the microspheres to be denser and reduce the loss of the core material in the film forming stage. Too high a concentration of calcium chloride may cause electrostatic repulsion between ions, possibly resulting in leakage of anthocyanins from the micelles. However, the calcium ion concentration cannot be too small, otherwise the gel strength of the formed wall material is not enough.
4. Influence of sodium alginate concentration on black rice anthocyanin embedding rate
Taking 2mg/mL black rice anthocyanin solution, and respectively placing the black rice anthocyanin solution and sodium alginate solution with the concentration of 1.5%, 1.8%, 2.1% and 2.4% (w/v) in the core material pressure bottle and the wall material pressure bottle according to the volume ratio of 1:3 of the core wall. A microcapsule granulator is used, a core material spray head with the aperture of 450 microns and a wall material spray head with the aperture of 550 microns are selected, and the distance between the spray heads and the calcium chloride solution is 10 cm. The parameters of the microcapsule granulator are set as the vibration frequency of 400Hz, the voltage of 1800V, the heating temperature of 50 ℃ and the pressure of 200 mbar. The solution is dispersed into small drops by the suction of a microcapsule granulator and high-frequency oscillation, and the small drops are dripped into 150mL of 2.0% calcium chloride solution and solidified for 10min to form a film. The resulting mixed solution of microcapsules and calcium chloride was vacuum filtered until complete separation with no liquid dripping, and the filtrate volume was read. And (4) measuring the embedding rate. The effect of sodium alginate concentration on the rate of black rice anthocyanin incorporation is shown in FIG. 4.
The sodium alginate as wall material can determine the polymerization strength, spherical shape, balling speed and the like of the spherical shell of the microcapsule. As can be seen from fig. 4, the anthocyanin entrapment rate increased with increasing sodium alginate concentration, reached a maximum at 2.1%, and then decreased. When the concentration of sodium alginate is lower, the embedding effect is poor, and the embedding rate is lower, which is probably because the microcapsule prepared by the method is low in spherical shell strength and poor in embedding effect because enough carboxyl is not available to generate gel and cannot fully react with calcium ions. Along with the increase of the concentration of the sodium alginate, the formed microcapsule shell has the advantages of water holding capacity rising, enhanced polymerization degree and full reaction with calcium ions. The space network in the rubber shell is more compact, and the gel strength is increased.
5. Influence of nozzle aperture on black rice anthocyanin embedding rate
Taking 2mg/mL black rice anthocyanin solution, and respectively placing the sodium alginate solution in a core material pressure bottle and a wall material pressure bottle according to the volume ratio of 1:3 of the core wall to 2.1% (w/v). Core material sprayers with the aperture of 200 microns, 300 microns, 450 microns and 750 microns are respectively used, the aperture of the wall material sprayer is larger than 100 microns of the core material sprayer, and the distance between the sprayer and the calcium chloride solution is 10 cm. The parameters of the microcapsule granulator are set as the vibration frequency of 400Hz, the voltage of 1800V, the heating temperature of 50 ℃ and the pressure of 200 mbar. The solution is dispersed into small drops by the suction of a microcapsule granulator and high-frequency oscillation, and the small drops are dripped into prepared 150mL calcium chloride solution with certain concentration and solidified for 10min to form a film. The resulting mixed solution of microcapsules and calcium chloride was vacuum filtered until complete separation with no liquid dripping, and the filtrate volume was read. And (4) measuring the embedding rate. The influence of the nozzle aperture on the embedding rate of the black rice anthocyanin is shown in figure 5.
It can be seen from fig. 5 that the early anthocyanin encapsulation efficiency increases as the showerhead aperture increases, reaches a maximum when the showerhead aperture reaches 450 μm, and then decreases. It can be seen that the nozzle hole diameter has an influence on the embedding rate. Too small a nozzle hole diameter results in an increase in extrusion pressure. According to darcy's law, an increase in the trans-pore pressure generally results in an increase in the flux of the dispersed phase, affecting the content of encapsulated anthocyanins. The too large aperture of the nozzle can increase the forming time of the liquid bead. These all result in a decrease in the rate of embedding of anthocyanins.
6. Structure observation of black rice anthocyanin microcapsules
The black rice anthocyanin microcapsules prepared by the microcapsule granulator are observed by a microscope, and the test results are shown in fig. 6 and 7. The black rice anthocyanin microcapsules are spherical, have good dispersibility, smooth and complete particle surfaces and no cracks or pores, show higher microcapsule encapsulation efficiency, and have good protection effect on core materials by wall materials.
Claims (5)
1. A process method for preparing black rice anthocyanin microcapsules by using a microcapsule granulator is characterized by comprising the following steps:
(1) and (3) purifying black rice anthocyanin: purifying black rice anthocyanin by using an elution adsorption method, wherein the elution adsorption method is to adsorb the black rice anthocyanin after impurity removal by using a solid phase extraction column, elute insoluble impurities by using an acidified aqueous solution, elute polyphenols by using an ethyl acetate solution, and elute the black rice anthocyanin on the adsorption column by using an acidified methanol solution. And then, removing the methanol by rotary evaporation by using a rotary evaporator to obtain pure black rice anthocyanin. Performing quantitative analysis on the purified black rice anthocyanin solution by using high performance liquid chromatography;
(2) preparation of sodium alginate solution: dissolving 1.5-2.4g of sodium alginate in 100mL of distilled water, stirring at 55-65 ℃ for 30min, and cooling to room temperature to obtain a sodium alginate solution;
(3) preparing black rice anthocyanin microcapsules: the black rice anthocyanin microcapsules are prepared by ion gelation and a double-nozzle embedding method by using a microcapsule embedding machine. Adding 2mg/mL anthocyanin solution serving as a core material into a pressure-resistant bottle matched with an instrument. Sodium alginate is added into another pressure-resistant bottle as a wall material according to the volume ratio of the core to the wall of 1: 2-5. The aperture of the core material nozzle is 200 and 750 mu m, and the wall material nozzles are all selected to be nozzles with the aperture larger than 100 mu m of the core material nozzle. The distance between the spray head and the liquid level of the receiving solution is 10 cm. The pressure of the flow rate regulating valve to the conduit is regulated to ensure that the core material solution and the wall material solution are sucked into the microcapsule embedding machine according to the required volume ratio. After the core material solution and the wall material solution are simultaneously sucked by a microcapsule embedding machine, the core material solution and the wall material solution are dispersed into small droplets under the action of high-frequency oscillation and static electricity, the small droplets are dripped into 150mL of 1.0-2.5% calcium chloride solution, and the solution is solidified for 10min to form a film. And (3) carrying out vacuum filtration on the obtained mixed solution of the anthocyanin microcapsules and calcium chloride until solid and liquid are completely separated and no liquid drips to obtain the black rice anthocyanin microcapsules.
2. The process for preparing black rice anthocyanin microcapsules by using a microcapsule granulator according to claim 1, wherein the acidified aqueous solution in the step (1) elutes insoluble impurities, the ethyl acetate solution elutes polyphenols, the acidified methanol solution elutes black rice anthocyanin on the adsorption column, and then the methanol is removed by rotary evaporation by using a rotary evaporator to obtain pure black rice anthocyanin.
3. The process method for preparing black rice anthocyanin microcapsules by using a microcapsule granulator according to claim 1, wherein the optimal mass of the sodium alginate dissolved in the distilled water in the step (2) is 1.8g, and the optimal stirring temperature is 60 ℃.
4. The process method for preparing the black rice anthocyanin microcapsules by using the microcapsule granulator according to claim 1, wherein the core-wall ratio of the core material black rice anthocyanin to the wall material sodium alginate in the step (3) is 1:3, the concentration of calcium chloride is 1.5% (w/v), the pore diameter of a core material nozzle is 450 μm, the pore diameter of a wall material nozzle is 550 μm, and the nozzle is 10cm away from the calcium chloride solution.
5. The process for preparing black rice anthocyanin microcapsules by using a microcapsule granulator according to claim 1, wherein the microcapsule granulator in the step (3) has the vibration frequency of 400Hz, the voltage of 1800V, the heating temperature of 50 ℃ and the pressure of 200 mbar.
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