Oral fast-dissolving high-porous sucrose granules and preparation method thereof

Abstract

The present invention provides an oral instant high-porosity sucrose granule and a preparation method thereof, wherein the preparation method is as follows: sucrose, α-lactose and water are mixed to form a solution; ultra-high pressure treatment is performed; a spray is generated by an atomizer, and the droplets generated by the spray are sprayed into a container containing liquid nitrogen; ultrasonic-assisted quick freezing is performed: finally vacuum freeze drying is performed to obtain highly porous sucrose granules. The present invention is based on ultrasonic quick freezing spray drying technology, innovatively applied to sucrose molecules, supplemented by ultra-high pressure technology and additionally adding α-lactose, synergistically increasing the glass transition temperature of sucrose granules, reducing the degree of sucrose crystallization and greatly increasing its porosity. Such highly porous sucrose granules can be quickly dissolved in the oral cavity, reducing the intake of sucrose without reducing the sweetness of the oral cavity, thereby achieving the purpose of reducing sugar and controlling sugar.

Description

Technical Field

[0001] The invention belongs to the technical field of food processing, and in particular relates to a method for preparing oral instant-dissolving high-porous sucrose particles. Background Art

[0002] Excessive sugar intake will burden human health and increase the risk of dental caries, obesity, coronary heart disease, hypertension, gout, diabetes, dementia and other diseases. Reducing sugar intake has become an inevitable trend. The current mainstream direction of reducing sugar intake in my country is to regulate from a macro level, such as using functional sugar alcohols and sweeteners to replace sucrose and starch sugar. However, sweeteners have different properties and flavors. Even if they are compounded, there is still no one or more that can truly replace sucrose.

[0003] Traditional sugar exists in the form of crystals. The outer layer dissolves in the mouth, and the remaining solid crystals inside will be completely digested and absorbed by the human body, generating heat. Studies have shown that it only takes 1.5 to 4.0 seconds for dissolved sugar molecules to stimulate the taste buds to produce sweetness, so the slower dissolution rate of ordinary sugar crystals in the mouth is the main reason why consumers feel the sweetness slowly. If the sugar crystal has a uniform spherical and highly porous structure, then its larger specific surface area than ordinary sugar crystals can enable it to quickly absorb water in the mouth and have better solubility. In addition, its larger porosity makes its quality far lower than that of ordinary sugar crystals, but it does not affect the sweetness produced by the taste buds. Therefore, consumers can reduce their sugar intake while maintaining the same taste, achieving the purpose of reducing and controlling sugar to a certain extent.

[0004] As a new drying technology, ultrasonic quick freezing spray drying combines the advantages of spray drying and freeze drying. The resulting products have the advantages of high porosity, relatively complete preservation of nutrients, higher biological activity, and better product quality. Food ultra-high pressure technology is a non-thermal processing technology and a physical processing process. It has the characteristics of safety, high efficiency, instant compression, and uniform action. It can achieve the purpose of sterilization, enzyme inactivation, increasing the glass transition temperature, material modification, and the generation of new tissue structures, and improving food quality. Summary of the invention

[0005] Technical problem to be solved: The purpose of the present invention is to provide an orally rapidly dissolving high-porous sucrose granule and a preparation method thereof. The orally rapidly dissolving high-porous sucrose granule is prepared by ultra-high pressure and ultrasonic quick freezing spray drying technology and can be rapidly dissolved in the oral cavity. Due to the high porosity, the intake of sucrose can be reduced without affecting the sweetness produced by the taste buds.

[0006] Technical solution: A highly porous sucrose granule that can be dissolved orally, wherein the water content of the granule is 0.7% to 3.0%, the particle size is 10 to 37 μm, the porosity is ≥ 90%, and the complete dissolution time in saliva is 2 to 3 seconds. A method for preparing a highly porous sucrose granule that can be dissolved orally comprises the following steps:

[0007] (1) sucrose, α-lactose (10-20 wt.% of the sucrose mass) and water are mixed, and stirred at 35-40° C. and 750-850 rpm for 25-35 min to fully dissolve the mixture, thereby preparing a sucrose solution with a concentration of 15 wt.%;

[0008] (2) subjecting the sucrose solution to ultrahigh pressure treatment: using a vacuum sealer to seal the sucrose solution in a polyethylene bag, placing the bag in a pressure chamber and immersing the bag in pressure-transmitting medium water, and subjecting the bag to ultrahigh pressure treatment for 10 to 20 minutes;

[0009] (3) pressure spraying the sucrose solution treated with ultrahigh pressure: the sucrose solution is transported to the atomizer nozzle through a constant flow pump, so that the sucrose solution is atomized into tiny droplets, and the average particle size of the tiny droplets is controlled to be between 400 and 800 nm, and the droplets generated by the spray are sprayed into a container containing liquid nitrogen to obtain ice crystal particles with smaller particle size;

[0010] (4) Ultrasonic-assisted quick freezing: A container containing small ice crystals and liquid nitrogen is placed in an ultrasonic-assisted quick freezing device for freeze drying to obtain highly porous sucrose particles.

[0011] Furthermore, in step (2), the ultrahigh pressure is 300-500 MPa, the pressure increasing method is linear pressure increasing, the speed is 100 MPa / min, and the pressure reducing method is instantaneous pressure reducing.

[0012] Furthermore, in step (3), the pump speed of the peristaltic pump in the constant flow pump is 25%; the spraying equipment is a nano-scale ionization spray dryer, and the tiny droplets are precisely controlled and generated by an atomizer with piezoelectric technology. The height of the nozzle from the liquid nitrogen surface is 5 to 10 cm, the feed rate is 5 to 7 mL / min, the gas flow rate is 120 to 130 L / min, the pressure is 45 to 55 hPa, and the spray frequency is 110 kHz.

[0013] Furthermore, in step (4), the conditions for ultrasonic-assisted quick freezing are: the ultrasonic frequency is 40 to 50 kHz, the freezing medium includes anhydrous ethanol, glycerol and ethylene glycol, and the power required for each liter of impregnation liquid is 50 to 60 W.

[0014] Furthermore, in step (4), the ultrasound is performed intermittently, the duration of a single ultrasound is 5 to 10 seconds, and the interval between two adjacent ultrasounds is 20 to 25 seconds.

[0015] Furthermore, in step (4), the freeze-drying conditions are: the freeze-drying temperature is -80°C, the pre-cooling time is 24 hours, and the drying time is 48 hours.

[0016] Beneficial effects:

[0017] 1. The oral fast-dissolving high-porous sucrose granules prepared by the present invention are porous spherical small particles. Compared with ordinary sugar crystals, they have a larger specific surface area, a smaller bulk density, and a higher porosity. They can quickly absorb water and dissolve in the oral cavity, and have the advantage of reducing sucrose intake while maintaining the same sweetness and taste.

[0018] 2. The preparation method of the oral fast-dissolving high-porous sucrose granules of the present invention is based on ultrasonic quick-freezing spray drying technology, which is innovatively applied to sucrose molecules, supplemented by ultra-high pressure technology and additionally adding α-lactose to the raw materials, which synergistically improves the glass transition temperature of the sucrose granules, reduces the crystallinity, and increases the porosity. This high-porous sucrose granule with a large specific surface area has a more excellent solubility performance, which can make the outer layer of the sugar that produces sweetness quickly absorb water and dissolve in the mouth, and the complete dissolution time in saliva is 2 to 3 seconds, and the number of dissolved molecules is the same as that of ordinary crystalline sugar, that is, the same sweet taste is produced. Because of the high porosity, the part that is digested by the human body to generate heat is far less than that of ordinary sucrose crystals, which reduces the intake of sucrose to a certain extent, achieving the purpose of reducing sugar.

[0019] 3. The ultrasonic quick freezing spray drying technology adopted in the present invention can obtain sucrose particles that are nearly spherical and have a highly porous, interconnected pore network structure. This is because the liquid is dispersed into fine droplets during the atomization process. After contacting with the cold medium-liquid nitrogen, the droplets are instantly frozen, maintaining their spherical structure. Subsequently, the ice crystals in the particles are removed by sublimation during the vacuum drying process, forming porous evaporation channels that are interconnected inside the particles. This uniform porous structure increases the specific surface area of ​​the sucrose particles, allowing them to quickly absorb water, thereby showing excellent solubility properties. At the same time, the bulk density of the sucrose particles is made smaller and the overall structure is more fluffy, which reduces the intake of sucrose to a certain extent and achieves the purpose of reducing sugar. The powder form also reduces storage and transportation costs, which is of great significance for its widespread use in global food trade.

[0020] 4. The ultra-high pressure technology used in the present invention is a non-thermal processing technology that can effectively reduce the crystallinity of sucrose particles. The higher the degree of sucrose crystallinity, the lower the porosity. Since the glass transition temperature (Tg) of α-lactose is significantly higher than that of sucrose at the same humidity, adding a certain amount of α-lactose to the raw materials can synergistically reduce the crystallinity of sucrose particles, increase porosity, improve its stability, and fully ensure the rapid solubility and porosity of sucrose particles. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 The particle size distribution diagram of sucrose particles obtained in Example 1, Example 2, Comparative Example 1 and Comparative Example 2 of the present invention.

[0022] Figure 2 The figures are scanning electron microscope images of sugar particles obtained in all embodiments and comparative examples of the present invention; wherein (A) is the sucrose particles of embodiment 1, (B) is the sucrose particles of embodiment 2, (C) is the sucrose particles of comparative example 1, (D) is the sucrose particles of comparative example 2, (E) is the crystallized sucrose of comparative example 3, and (F) is the crystallized lactose of comparative example 4; the magnification of E is 100X, and the magnification of the others is 1000X.

[0023] Figure 3 It is a schematic diagram of the dynamic dissolution process of the sugar particles prepared in the present invention, wherein (A) is the sucrose particles of Example 2, (B) is the crystallized lactose of Comparative Example 4, and (C) is the crystallized sucrose of Comparative Example 3.

[0024] Figure 4 The figures are images of the dynamic dissolution process of the sugar particles prepared in the present invention, wherein Group (A) shows the dissolution process of the sucrose particles obtained in Example 2 in saliva, Group (B) shows the dissolution process of the crystalline lactose in Comparative Example 4 in saliva, and Group (C) shows the dissolution process of the crystalline sucrose in Comparative Example 3 in saliva. DETAILED DESCRIPTION

[0025] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0026] The following examples are used to illustrate the present invention but are not intended to limit the scope of the present invention.

[0027] Unless otherwise specified, the technical means used in the specification are all known in the art, and the raw materials used are all commercially available.

[0028] Example 1

[0029] A method for preparing oral fast-dissolving highly porous sucrose granules comprises the following steps:

[0030] (1) Sucrose, α-lactose (10 wt.% of the mass of sucrose) and water were mixed, and stirred at 40° C. and 800 rpm for 30 min to fully dissolve the mixture, thereby preparing a sucrose solution with a concentration of 15 wt.%;

[0031] (2) subjecting the sucrose solution to ultrahigh pressure treatment: using a vacuum sealer to seal the sucrose solution in a 10×20 cm double-layer high temperature and high pressure resistant polyethylene bag, placing it in a pressure chamber and immersing it in pressure transmitting medium water, maintaining the pressure for 15 min at a temperature of 25° C., a pressure increase rate of 100 MPa / min, and a pressure of 300 MPa, and then instantly reducing the pressure;

[0032] (3) Pressure spraying of the ultrahigh pressure treated sucrose solution: the sucrose solution is delivered to the atomizer nozzle of the nano-scale ionization spray dryer by a constant flow pump with a pump speed of 25%, and the atomizer with piezoelectric technology is precisely controlled to generate tiny droplets with an average particle size of 400 to 800 nm, and the droplets generated by the spray are sprayed into a container containing liquid nitrogen to obtain ice crystals with a particle size of less than 1 μm; the height of the nozzle from the liquid nitrogen level is 10 cm, the feed rate is 7 mL / min, the gas flow rate is 130 L / min, the pressure is 55 hPa, and the spray frequency is 110 kHz;

[0033] (4) Ultrasonic-assisted quick freezing: Place the container containing ice crystal particles and liquid nitrogen in an ultrasonic-assisted quick freezing device and perform ultrasonic quick freezing until the liquid nitrogen is completely volatilized. Set the ultrasonic frequency to 40kHz, intermittent ultrasound, single ultrasound time to 10s, and the interval between two adjacent ultrasounds to 25s. The immersion liquid is anhydrous ethanol, and the power required per liter of solution is 50W. Finally, place it in a vacuum freeze dryer for freeze drying to obtain highly porous sucrose particles. The freeze drying temperature is -80℃, the precooling time is 24h, and the drying time is 48h.

[0034] Example 2

[0035] A method for preparing oral fast-dissolving highly porous sucrose granules comprises the following steps:

[0036] (1) Sucrose, α-lactose (20 wt.% of the mass of sucrose) and water were mixed, and stirred at 40° C. and 800 rpm for 30 min to fully dissolve the mixture, thereby preparing a sucrose solution with a concentration of 15 wt.%;

[0037] (2) subjecting the sucrose solution to ultrahigh pressure treatment: using a vacuum sealer to seal the sucrose solution in a 10×20 cm double-layer high temperature and high pressure resistant polyethylene bag, placing it in a pressure chamber and immersing it in pressure transmitting medium water, maintaining the pressure for 15 min at a temperature of 25° C., a pressure increase rate of 100 MPa / min, and a pressure of 300 MPa, and then instantly reducing the pressure;

[0038] (3) Pressure spraying of the ultrahigh pressure treated sucrose solution: the sucrose solution is delivered to the atomizer nozzle of the nano-scale ionization spray dryer by a constant flow pump with a pump speed of 25%, and the atomizer with piezoelectric technology is precisely controlled to generate tiny droplets with an average particle size of 400 to 800 nm, and the droplets generated by the spray are sprayed into a container containing liquid nitrogen to obtain ice crystals with a particle size of less than 1 μm; the height of the nozzle from the liquid nitrogen level is 10 cm, the feed rate is 7 mL / min, the gas flow rate is 130 L / min, the pressure is 55 hPa, and the spray frequency is 110 kHz;

[0039] (4) Ultrasonic-assisted quick freezing: Place the container containing ice crystal particles and liquid nitrogen in an ultrasonic-assisted quick freezing device and perform ultrasonic quick freezing until the liquid nitrogen is completely volatilized. Set the ultrasonic frequency to 40kHz, intermittent ultrasound, single ultrasound time to 10s, and the interval between two adjacent ultrasounds to 25s. The immersion liquid is anhydrous ethanol, and the power required per liter of solution is 50W. Finally, place it in a vacuum freeze dryer for freeze drying to obtain highly porous sucrose particles. The freeze drying temperature is -80℃, the precooling time is 24h, and the drying time is 48h.

[0040] Comparative Example 1

[0041] A method for preparing oral fast-dissolving highly porous sucrose granules comprises the following steps:

[0042] (1) sucrose and water were mixed and stirred at 40° C. and 800 rpm for 30 min to fully dissolve the mixture, thereby preparing a sucrose solution with a concentration of 15 wt.%;

[0043] (2) subjecting the sucrose solution to ultrahigh pressure treatment: using a vacuum sealer to seal the sucrose solution in a 10×20 cm double-layer high temperature and high pressure resistant polyethylene bag, placing it in a pressure chamber and immersing it in pressure transmitting medium water, maintaining the pressure for 15 min at a temperature of 25° C., a pressure increase rate of 100 MPa / min, and a pressure of 300 MPa, and then instantly reducing the pressure;

[0044] (3) Pressure spraying of the ultrahigh pressure treated sucrose solution: the sucrose solution is delivered to the atomizer nozzle of the nano-scale ionization spray dryer by a constant flow pump with a pump speed of 25%, and the atomizer with piezoelectric technology is precisely controlled to generate tiny droplets with an average particle size of 400 to 800 nm, and the droplets generated by the spray are sprayed into a container containing liquid nitrogen to obtain ice crystals with a particle size of less than 1 μm; the height of the nozzle from the liquid nitrogen level is 10 cm, the feed rate is 7 mL / min, the gas flow rate is 130 L / min, the pressure is 55 hPa, and the spray frequency is 110 kHz;

[0045] (4) Ultrasonic-assisted quick freezing: Place the container containing ice crystal particles and liquid nitrogen in an ultrasonic-assisted quick freezing device and perform ultrasonic quick freezing until the liquid nitrogen is completely volatilized. Set the ultrasonic frequency to 40kHz, intermittent ultrasound, single ultrasound time to 10s, and the interval between two adjacent ultrasounds to 25s. The immersion liquid is anhydrous ethanol, and the power required per liter of solution is 50W. Finally, place it in a vacuum freeze dryer for freeze drying to obtain highly porous sucrose particles. The freeze drying temperature is -80℃, the precooling time is 24h, and the drying time is 48h.

[0046] Comparative Example 2

[0047] A method for preparing oral fast-dissolving highly porous lactose particles comprises the following steps:

[0048] (1) α-lactose and water were mixed and stirred at 40° C. and 800 rpm for 30 min to fully dissolve the mixture, thereby preparing a lactose solution with a concentration of 15 wt.%;

[0049] (2) subjecting the lactose solution to ultrahigh pressure treatment: using a vacuum sealer to seal the lactose solution in a 10×20 cm double-layer high temperature and high pressure resistant polyethylene bag, placing it in a pressure chamber and immersing it in pressure transmitting medium water, maintaining the pressure for 15 min at a temperature of 25° C., a pressure increase rate of 100 MPa / min, and a pressure of 300 MPa, and then instantly reducing the pressure;

[0050] (3) Pressure spraying of the ultrahigh pressure treated lactose solution: The lactose solution is delivered to the atomizer nozzle of the nano-scale ionization spray dryer by a constant flow pump with a pump speed of 25%, and the atomizer with piezoelectric technology precisely controls the generation of tiny droplets with an average particle size of 400 to 800 nm, and the droplets generated by the spray are sprayed into a container containing liquid nitrogen to obtain ice crystals with a particle size of less than 1 μm; the height of the nozzle from the liquid nitrogen level is 10 cm, the feed rate is 7 mL / min, the gas flow rate is 130 L / min, the pressure is 55 hPa, and the spray frequency is 110 kHz;

[0051] (4) Ultrasonic-assisted quick freezing: Place the container containing ice crystal particles and liquid nitrogen in an ultrasonic-assisted quick freezing device and perform ultrasonic quick freezing until the liquid nitrogen is completely volatilized. Set the ultrasonic frequency to 40kHz, intermittent ultrasound, single ultrasound time to 10s, and the interval between two adjacent ultrasounds to 25s. The immersion liquid is anhydrous ethanol, and the power required per liter of solution is 50W. Finally, place it in a vacuum freeze dryer for freeze drying to obtain highly porous lactose particles. The freeze drying temperature is -80℃, the precooling time is 24h, and the drying time is 48h.

[0052] Comparative Example 3

[0053] A method for preparing crystallized sucrose comprises the following steps:

[0054] (1) preparing a hot saturated solution of sucrose: mixing sucrose and water to prepare a hot saturated solution, stirring at 40° C. and 800 rpm for 30 min to fully dissolve the sucrose;

[0055] (2) Seal the beaker containing the solution with tin foil and place it in ice cubes for rapid cooling. Replace the ice cubes with new ones after the ice melts. Repeat this process 4 to 5 times.

[0056] (3) The cooled solution was stored in a -80°C cold storage for 48 hours, taken out, filtered under reduced pressure, and then dried in a vacuum drying oven for 24 hours at a temperature of 35°C to obtain crystalline sucrose particles.

[0057] Comparative Example 4

[0058] A method for preparing crystalline lactose, comprising the steps of:

[0059] (1) preparing a hot saturated solution of α-lactose: mixing α-lactose and water to prepare a hot saturated solution, stirring at 40° C. and 800 rpm for 30 min to fully dissolve the solution;

[0060] (2) Seal the beaker containing the solution with tin foil and place it in ice cubes for rapid cooling. Replace the ice cubes with new ones after the ice melts. Repeat this process 4 to 5 times.

[0061] (3) The cooled solution was stored in a -80°C cold storage for 48 hours, taken out, filtered under reduced pressure, and then dried in a vacuum drying oven for 24 hours at a temperature of 35°C to obtain crystalline lactose particles.

[0062] Determination of properties

[0063] The physical properties and morphological characteristics of the sugar particles obtained in all the examples and comparative examples were analyzed (see Table 1). The physical properties included water content, particle size, specific surface area, density and porosity.

[0064] The water content of sugar granules was measured by HE83 / 02 moisture meter from Mettler-Toledo Instruments (Shanghai) Co., Ltd.;

[0065] The particle size was measured using a Beckman Coulter LS I3320 particle size analyzer;

[0066] The specific surface area was determined using an ASAP 2460 series fully automatic rapid physical adsorption analyzer, where the adsorbed gas was N 2 , degassing temperature 40℃, degassing time 16h;

[0067] Bulk density bThe determination method is: take a 5ml centrifuge tube, weigh it and record it as m 1 (g) Pour the sugar granules into the centrifuge tube and shake it continuously. When the volume reaches the mark on the centrifuge tube, weigh it and record it as m. 2 (g), the bulk density can be calculated using the following formula:

[0068]

[0069] True density of sugar particles ρ TR The AccuPyc II 1340 true density meter was used for measurement, the volume was measured by gas displacement method, and inert gas helium was used as the displacement gas for non-destructive testing. The porosity was calculated by the following formula:

[0070]

[0071] The morphological characteristics analysis is to observe the microstructure of sugar particles through scanning electron microscope. The specific steps are as follows: use bamboo toothpicks to pick up a very small amount of sugar particles, stick them on the conductive double-sided tape fixed on the scanning electron microscope sample plate, gently roll the toothpick to flatten the particles in a single layer, and sputter the sample plate with Pt-Pd in ​​the MSP-1S magnetron sputtering coating machine, and analyze it at an accelerating voltage of 6kV. For easy observation between different samples, use a knife to cut the tape to make it have obvious separation marks.

[0072] Table 1 Physical properties of sugar granules obtained in various examples and comparative examples

[0073]

[0074]

[0075] Note: The same letters in the upper right corner indicate no significant difference (p>0.05); different letters indicate significant difference between different samples in the same row (p<0.05).

[0076] As can be seen from Table 1, the water content of the six samples is below 5%, with significant differences. The water content of Example 1, Example 2, Comparative Example 1 and Comparative Example 2 is between 0.75% and 2.93%, which is higher than that of Comparative Example 3 and Comparative Example 4, that is, the water content of the sucrose particles obtained by ultra-high pressure and ultrasonic quick freezing spray drying technology is higher than that of crystallized sucrose and crystallized lactose. And under the same processing method, Example 2 (lactose with 20wt.% of sucrose mass added) has the highest water content.

[0077] Compared with Comparative Example 3 and Comparative Example 4, the particle size of Example 1, Example 2, Comparative Example 1 and Comparative Example 2 is significantly reduced, the specific surface area is significantly increased, the bulk density is significantly reduced, and the porosity is significantly increased, indicating that the small molecule sucrose particles obtained by ultra-high pressure and ultrasonic quick freezing spray drying technology have more holes and are more fluffy than crystalline sucrose and crystalline lactose. Because in the process of ultra-high pressure, the structure of the particles has undergone certain changes, which reduces its crystallinity. In the process of ultrasonic quick freezing spray drying, the atomization process greatly reduces the particle size of the sucrose particles, and the quick freezing drying process will leave tiny channels inside the particles to form a uniform pore structure, which greatly increases the specific surface area of ​​the sucrose particles. Comparing Example 1 and Comparative Example 1, it can be seen that the addition of α-lactose significantly increases the porosity of the sucrose particles, because at the same humidity, the glass transition temperature of α-lactose is significantly higher than that of sucrose. Example 2 shows the highest specific surface area and porosity, further indicating that within a certain range, the higher the pressure, the more lactose content, the higher the porosity of the sugar particles, and the better the porosity.

[0078] Particle size distribution is an important indicator to measure the uniformity of granular powder. The more concentrated the particle size distribution is, the more uniform the sucrose particle size is. Figure 1 It can be seen that the particle size distributions of Example 1, Example 2, Comparative Example 1 and Comparative Example 2 are relatively concentrated, indicating that the sucrose particles obtained by ultrahigh pressure and ultrasonic quick freezing spray drying technology are very uniform in size. Among them, the particle size distribution of Example 1 is about 33 μm, and the particle size distribution of Example 2 is about 12 μm. The particle size distributions of Comparative Example 1 and Example 2 are relatively close, and the particle size distributions of Example 1 and Comparative Example 2 are relatively close.

[0079] Depend on Figure 2 It can be seen that the crystallized sucrose (Comparative Example 3) and the crystallized lactose (Comparative Example 4) show typical crystal characteristics, with relatively regular shapes, smooth surfaces, no cracks, and sharp edges and corners, while the morphology of small molecule sucrose particles obtained by ultra-high pressure and ultrasonic quick freezing spray drying technology has undergone significant changes. It can be seen from A to D that the sucrose particles are nearly spherical and have a highly porous, interconnected pore network structure. The liquid is dispersed into fine droplets during the atomization process. After contact with liquid nitrogen, the droplets are frozen into particles. The ice crystals in the particles are removed by sublimation during the drying process, thereby forming an internally interconnected porous structure. This structure greatly increases its specific surface area and reduces the mass of sucrose particles at the same volume. Comparing A to D, although the content of α-lactose in the original liquid is different, there is no obvious difference in the surface morphology of the four samples.

[0080] The dynamic dissolution process of the sugar particles obtained in all the embodiments and comparative examples was observed using a microscope with a video recording function. The specific steps were as follows: a very small amount of sugar particles were picked up with a bamboo toothpick and placed in the center of the grooved glass slide. The particles could be gently blown away with an ear bulb. The objective lens was adjusted to 40 times to make clear single sugar particles appear in the field of view. The photography mode of the microscope was turned on. A small amount of saliva was drawn with a needle syringe and slowly injected into the groove of the glass slide until the sugar particles began to dissolve. The video was stopped when the sugar particles were completely dissolved.

[0081] Depend on Figure 3 , Figure 4 It can be seen that the dissolution of sugar particles is generally divided into three stages: wetting, dispersion and dissolution. When measuring the solubility of the sample, since the two stages of dispersion and dissolution are difficult to observe independently, it is manifested as the reduction of the particle size of the sugar particles during the erosion and crushing process in the dispersant (saliva). Therefore, by recording the dissolution of the sample, capturing images at different time points, and comparing the size changes of the samples, the dissolution rate of different samples can be intuitively evaluated. Among them, the small molecule sucrose particles prepared by ultra-high pressure and ultrasonic quick freezing spray drying technology are almost completely dissolved in 2s (Example 2), while crystalline lactose (Comparative Example 4) and crystalline sucrose (Comparative Example 3) require 16s and 32s respectively to be completely dissolved. During the dissolution process, the physical and chemical properties of the liquid medium (such as surface tension, viscosity, density and temperature) and the physical and chemical properties of the sample itself (such as particle size, density, porosity and chemical composition) significantly affect the dissolution rate. Under the same liquid medium (saliva), the small molecule sucrose particles produced by ultra-high pressure and ultrasonic quick freezing spray drying technology have a uniform pore structure and a high porosity, which increases the specific surface area of ​​the particles, allowing the sucrose particles to quickly absorb water, thereby exhibiting excellent solubility properties.

[0082] Although the present invention has been described above through embodiments, those skilled in the art should understand that without departing from the spirit and substance of the present invention, all improvements and modifications made to the present invention should fall within the protection scope of the present invention.

Claims

1. An orally soluble high-porous sucrose granule, characterized in that: The oral fast-dissolving high-porous sucrose granules have a water content of 0.7% to 3.0%, a particle size of 10 to 37 μm, a porosity of ≥ 90%, and a complete dissolution time in saliva of 2 to 3 s; The preparation method comprises the following steps: (1) Mix sucrose, α-lactose (10-20 wt.% of the mass of sucrose) and water, and stir them with a stirrer at a temperature of 35-40°C and a speed of 750-850 rpm for 25-35 min to fully dissolve them, thereby preparing a sucrose solution with a concentration of 15 wt.%; (2) subjecting the sucrose solution to ultrahigh pressure treatment: using a vacuum sealer to seal the sucrose solution in a polyethylene bag, placing the bag in a pressure chamber and immersing the bag in water as a pressure transmitting medium, and subjecting the bag to ultrahigh pressure treatment for 10 to 20 minutes; the pressure of the ultrahigh pressure is 300 to 500 MPa, the pressure increase method is linear pressure increase, the speed is 100 MPa / min, and the pressure reduction method is instantaneous pressure reduction; (3) Pressure spraying of the ultra-high pressure treated sucrose solution: the sucrose solution is transported to the atomizer nozzle through a constant flow pump, so that the sucrose solution is atomized into tiny droplets, and the average particle size of the tiny droplets is controlled to be between 400 and 800 nm, and the droplets generated by the spray are sprayed into a container containing liquid nitrogen to obtain ice crystal particles with smaller particle size; the peristaltic pump speed in the constant flow pump is 25%; the spraying equipment is a nano-scale ionization spray dryer, and the tiny droplets are precisely controlled and generated by an atomizer with piezoelectric technology, the nozzle is 5 to 10 cm above the liquid nitrogen level, the feed rate is 5 to 7 mL / min, the gas flow rate is 120 to 130 L / min, the pressure is 45 to 55 hPa, and the spray frequency is 110 kHz; (4) Ultrasonic-assisted quick freezing: placing a container containing small-sized ice crystals and liquid nitrogen in an ultrasonic-assisted quick freezing device for freeze-drying to obtain highly porous sucrose particles; the conditions for the ultrasonic-assisted quick freezing are: the ultrasonic frequency is 40-50 kHz, the freezing medium includes anhydrous ethanol, propylene glycol and ethylene glycol, and the power required per liter of freezing medium is 50-60 W.

2. The oral fast-dissolving highly porous sucrose granules according to claim 1, characterized in that: In step (4), the ultrasound is performed intermittently, the time for a single ultrasound is 5 to 10 s, and the interval between two adjacent ultrasounds is 20 to 25 s.

3. The orally-soluble high-porous sucrose granules according to claim 1, characterized in that: In step (4), the freeze-drying conditions are: temperature of -80°C, precooling time of 24 h, and drying time of 48 h.

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