Microcapsule powder stable in gastric acid, preparation method and use

Abstract

The present invention discloses a microcapsule powder stable in gastric acid, and a preparation method and use thereof. The microcapsule powder comprises a core material and an encapsulant material coated on the outside of the core material, the melting point of the encapsulant material is higher than 42°C, and the encapsulant material is not decomposed or dissolved by proteases and gastric acid, but is decomposed by intestinal digestive enzymes. By coating the core material with the encapsulant, the microcapsule powder can efficiently coat the core material with a single component, and at the same time, it solves the problem that the stability in the stomach is good in an open environment at room temperature, while the stability in the stomach is poor in an open environment at room temperature, as can be achieved only by the conventional embedding method.

Description

[Technical field]

[0001] The present invention relates to the food and / or pharmaceutical technical field, in particular to a microcapsule powder stable in gastric acid and a method for its preparation and use. [Background technology]

[0002] As important physiological substances in the human body, reduced nicotinamide adenine dinucleotide (NADH) and reduced nicotinamide adenine dinucleotide phosphate (NADPH) are involved in thousands of physiological and metabolic reactions in the human body, playing important roles in gene repair, improving immunity, antioxidant and improving sleep, etc., and sufficient NADH or NADPH can better protect the body, prevent and control diseases, and ensure the health of the body. Therefore, replenishing NADH or NADPH outside the body is helpful in promoting the optimal maintenance of various physiological functions of the body. However, NADH and NADPH are biological forms of hydrogen, and light, acidic environments, or oxygen and moisture in the air destroy the molecular structure of NADH and NADPH, making their chemical properties extremely unstable (and need to be prepared immediately when necessary). In addition, due to the characteristic that NADH and NADPH are weak to acid, NADH and NADPH taken from outside will lose their activity under the influence of stomach acid, making it difficult to obtain the desired effect.

[0003] In the prior art, NADH and NADPH are generally stabilized by adding antioxidants. However, the method of adding antioxidants cannot ensure that NADH and NADPH are not decomposed in the stomach, that is, the oral preparations containing NADH or NADPH in the prior art cannot ensure that NADH or NADPH are not decomposed in the stomach. Summary of the Invention [Problem to be solved by the invention]

[0004] Based on this, there is a need to provide a microcapsule powder and its preparation method and use that can solve the above problems. [Means for solving the problem]

[0005] The microcapsule powder is stable in gastric acid and comprises a core material and an encapsulation material coated on the outside of the core material, the encapsulation material having a melting point of greater than 42°C, and the encapsulation material is not decomposed or dissolved by proteases and gastric acid, but is decomposed by intestinal digestive enzymes.

[0006] In one embodiment, the melting point of the encapsulant is between 60°C and 140°C.

[0007] In one embodiment, the encapsulant is selected from at least one of rice bran aliphatic alkanols and higher aliphatic alkanols having 12 or more carbon atoms.

[0008] In one embodiment, the mass ratio of the encapsulant to the core is 70-90:10-30.

[0009] In one embodiment, the encapsulant is selected from at least one of octacosanol, triacontanol, and dotriacontanol.

[0010] In one embodiment, the core material is a substance that is susceptible to destruction by gastric juices and that needs to be absorbed or function in the intestine.

[0011] In one embodiment, the core material is selected from at least one of reduced nicotinamide adenine dinucleotide and reduced nicotinamide adenine dinucleotide phosphate.

[0012] In one embodiment, the particle size of the microcapsule powder is 1 μm to 1000 μm.

[0013] The preparation method of the microcapsule powder according to the above technical solution, heating an encapsulant that has a melting point greater than 42° C., is not degraded or dissolved by proteases and gastric acid, and is degraded by intestinal digestive enzymes until melted; a step of thoroughly mixing the core material and the molten capsule material while keeping the temperature, to obtain a suspension; and spray-freeze-drying and granulating the suspension to obtain a microcapsule powder containing the core material and the capsule material coated on the outside of the core material.

[0014] The preparation method of the microcapsule powder according to the above technical solution, thoroughly mixing the core material with an encapsulant having a melting point of more than 42°C, not decomposed or dissolved by proteases and gastric acid, and decomposed by intestinal digestive enzymes to obtain a mixture; The mixture is successively heat-sealed and spray-granulated to obtain a microcapsule powder containing the core material and the capsule material coated on the outside of the core material.

[0015] The preparation method of the microcapsule powder according to the above technical solution, heating an encapsulant that has a melting point greater than 42° C., is not degraded or dissolved by proteases and gastric acid, and is degraded by intestinal digestive enzymes until melted; mixing the core material and the molten capsule material in a warm state to obtain a mixture; Shearing the mixture at a shear speed of 10,000 rpm to 16,000 rpm for a shear time of 6 min to 15 min while keeping the temperature; The method includes a step of spray-granulating the mixture after shearing in a condensate to obtain a microcapsule powder containing the core material and the capsule material coated on the outside of the core material.

[0016] The preparation method of the microcapsule powder according to the above technical solution, thoroughly mixing the core material with an encapsulant having a melting point of more than 42°C, not decomposed or dissolved by proteases and gastric acid, and decomposed by intestinal digestive enzymes to obtain a mixture; and sequentially subjecting the mixture to heat fusion press granulation and shearing to obtain the microcapsule powder, wherein the shearing speed is 8000 rpm to 10000 rpm, and the microcapsule powder includes the core material and capsule material that coats the outside of the core material.

[0017] The use of the microcapsule powder according to the above technical solution or the microcapsule powder prepared by the preparation method according to the above technical solution in preparing functional food, health food or medicine. Effect of the Invention

[0018] Compared with the prior art, the beneficial effects of the present invention are as follows: 1. The present invention coats the core material with a capsule material, limits the melting point of the capsule material to be greater than 42°C, and ensures that the capsule material will not be decomposed or dissolved by proteases and gastric acid, and the microcapsule powder will not be fused, decomposed or dissolved in the stomach, thereby preventing the core material from being released in the stomach; the capsule material will be decomposed by intestinal digestive enzymes, and after entering the intestinal tract, the microcapsule powder will be decomposed by the intestinal digestive enzymes in the intestinal tract and the internal core material will be released, thereby ensuring that the core material can be absorbed by the intestinal tract and play its role in the intestinal tract. 2. The microcapsule powder of the present invention has good stability in an open environment at room temperature, which solves the problem that the conventional embedding method can only achieve stability in the stomach and has poor stability in an open environment at room temperature. 3. When using the capsule material of the present application, a single component can be used to encapsulate the unstable core material, whereas conventional materials for encapsulating unstable core materials must be used in combination with other materials in addition to the antioxidant, which requires many raw materials and a complicated process. 4. The microcapsule powder obtained by the present invention has a high embedding rate of the product and strong stability in an open environment at room temperature. Experiments have shown that the microcapsule powder obtained by the present invention will not melt, decompose or dissolve in a gastric acid environment, and can smoothly release the core material in the intestinal environment, ensuring that the core material can be effectively absorbed by the intestinal tract and fully play its role in the intestinal tract. [Brief description of the drawings]

[0019] In order to more clearly describe the technical solutions in the embodiments of the present invention or the prior art, the drawings necessary to be used in the description of the embodiments or the prior art are briefly described below. It is obvious that the drawings described below are only some embodiments of the present invention, and those skilled in the art can further obtain other drawings based on these drawings without creative work. [Figure 1] 1 is a flow chart for preparing microcapsule powder by spray freeze drying method. [Diagram 2] 1 is a flow chart for preparing microcapsule powder by a heat fusion mixing spraying method. [Diagram 3] 1 is a flow chart for preparing microcapsule powder by a submerged condensation method. [Figure 4] 1 is a flow chart for preparing microcapsule powder by heat fusion pressing method. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0020] The following embodiments of the present invention will be described in detail with reference to the accompanying drawings, and the technical solutions in the embodiments of the present invention will be clearly and completely explained. The clearly and explained embodiments are not all the embodiments, but only some of the embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative work belong to the scope of protection of the present invention.

[0021] The present invention provides a microcapsule powder that is stable in gastric acid, which comprises a core material and an encapsulation material coated on the outside of the core material, the melting point of the encapsulation material is higher than 42°C, and the encapsulation material is not decomposed or dissolved by proteases and gastric acid, ensuring that the microcapsule powder is not fused, decomposed or dissolved in the stomach, thereby preventing the core material from being released in the stomach; the encapsulation material is decomposed by intestinal digestive enzymes, so that after the microcapsule powder enters the intestinal tract, the internal core material is released, thereby ensuring that the core material can be absorbed by the intestinal tract and perform its role in the intestinal tract.

[0022] Preferably, the melting point of the encapsulant is between 60°C and 140°C.

[0023] The melting point of the capsule material is greater than 42°C, preferably 60°C to 140°C, which ensures that the capsule material does not melt in the stomach, while allowing the capsule material to be melt-coated easily and producing high-quality microcapsule powder. Note that 60°C to 140°C is the preferred melting point range for the capsule material, and above this temperature range, the core material (e.g., NADH, NADPH) that needs to be coated will be destroyed.

[0024] The capsule material of the present invention is selected from at least one of rice bran aliphatic alkanols and higher aliphatic alkanols having 12 or more carbon atoms.

[0025] First, both higher aliphatic alkanols and rice bran aliphatic alkanols have good chemical stability, and both are not decomposed by gastric acid, but are decomposed by intestinal digestive enzymes in the intestinal tract, thereby releasing the internal core material; secondly, higher aliphatic alkanols and rice bran aliphatic alkanols also have good room temperature stability, which can ensure the storage stability of the microcapsule powder in an open environment outside the body; furthermore, higher aliphatic alkanols and rice bran aliphatic alkanols have appropriate melting points, which prevent the core material from being destroyed when it reaches a molten state, and facilitate the melt coating of the capsule material, thereby enabling the preparation of high-quality microcapsule powder; and furthermore, rice bran aliphatic alkanols and higher aliphatic alkanols, especially octacosanol, triacontanol and dotriacontanol, can be used as nutritional supplements by themselves, which not only ensures the safety of use, but also plays the role of nutritional supplementation.

[0026] When the encapsulating material is rice bran aliphatic alkanol, it has remarkable anti-fatigue, lipid-lowering and sexual function-enhancing effects, and has excellent potential for use in functional foods, health foods, medicines and cosmetics, and was listed as a new resource food on June 9, 2017. However, the solubility of rice bran aliphatic alkanol is very poor, so it cannot exert its excellent biological functions. For this reason, conventional techniques generally embed it in a water-soluble encapsulating material such as gum arabic.

[0027] This application is the first to use rice bran aliphatic alkanol as an encapsulating material for microcapsule powder because the melting point of rice bran aliphatic alkanol is 80°C to 83°C, and the powder has good fluidity at room temperature. As an encapsulating material, it protects the core material and acts as a water barrier, oxygen barrier, and gastric acid resistant material, thereby maintaining the stability of the core material, solving the problem of the core material decomposing under gastric acid conditions, and improving the absorption rate and utilization rate of the core material in the intestinal tract.

[0028] When the encapsulating material is a higher aliphatic alkanol, the higher aliphatic alkanol is preferably one or more of octacosanol, triacontanol and dotriacontanol. The properties of higher aliphatic alkanol are stable, difficult to oxidize, resistant to acid and base, not absorbing moisture, good biodegradability and bioactivity, and often exist in the form of white wax-like solid, powder or scaly crystal at room temperature. In addition, higher aliphatic alkanol is non-toxic and edible, and like many organic substances, it is insoluble in water and easily soluble in organic solvents such as ethanol and acetone. It can be used as an encapsulating material to achieve the same technical effect as rice bran aliphatic alkanol.

[0029] The core material of the present application may theoretically be any substance that needs to be absorbed in the intestine or function in the intestine.

[0030] Generally, the core material is a material that is easily destroyed by gastric juice and that needs to be absorbed or function in the intestine, and the capsule material covers the material that needs to be absorbed or function in the intestine, so that it does not decompose or melt in the stomach.

[0031] The core material is preferably at least one of reduced nicotinamide adenine dinucleotide and reduced nicotinamide adenine dinucleotide phosphate.

[0032] The mass ratio of the capsule material to the core material is preferably 70 to 90:10 to 30. Based on the ratios in the examples, a high amount of core material coverage is ensured, while in the actually manufactured product, the coverage rate of the core material can also be maintained at a high level.

[0033] In the embodiment of the present invention, the particle size of the microcapsule powder can be determined according to the actual needs and preparation methods. In the present invention, the particle size of the microcapsule powder is preferably 1 μm to 1000 μm.

[0034] Referring to FIG. 1, the present invention discloses a method for preparing the microcapsule powder described in the above technical solution, and the microcapsule powder is prepared by spray freeze drying method, which includes the following steps:

[0035] In S110, the encapsulant is heated until melted.

[0036] The melting point of the capsule material is greater than 42° C., and the capsule material is not degraded or dissolved by proteases and gastric acid, but is degraded by intestinal digestive enzymes.

[0037] In S120, the core material and the molten capsule material are thoroughly mixed while being kept warm to obtain a suspension.

[0038] Preferably, the operation of obtaining a suspension after thoroughly mixing the core material and the molten capsule material while keeping the temperature is performed by stirring at a rotation speed of 500 rpm to 1200 rpm for 3 to 10 minutes while keeping the temperature, to obtain a suspension.

[0039] In S130, the suspension is spray-freeze-dried and granulated to obtain the microcapsule powder.

[0040] The prepared microcapsule powder comprises a core material and a capsule material coated on the outside of the core material.

[0041] Preferably, the operation of spray freeze drying granulating the suspension is spray freeze drying granulating the suspension in a spray dryer.

[0042] Preferably, the parameters of the spray dryer are as follows: inlet air temperature is 2°C to 20°C, outlet air temperature is 15°C to 30°C, central chamber temperature is 5°C to 25°C, and feed rate is 100 mL / min to 1500 mL / min.

[0043] Referring to FIG. 2, the present invention further discloses a method for preparing the microcapsule powder described in other above technical solutions, which prepares the above microcapsule powder by a hot-melt mixing spraying method, and includes the following steps:

[0044] In S210, the core material and the capsule material are thoroughly mixed to obtain a mixture.

[0045] The melting point of the capsule material is greater than 42° C., and the capsule material is not degraded or dissolved by proteases and gastric acid, but is degraded by intestinal digestive enzymes.

[0046] Preferably, a mixer can be used to thoroughly mix the core material and capsule material.

[0047] Preferably, the mixer parameters are as follows: mixing frequency is 25Hz to 40Hz, and mixing time is 30min to 60min.

[0048] In S220, the mixture is successively heat-sealed and spray-granulated to obtain the microcapsule powder.

[0049] The prepared microcapsule powder comprises a core material and a capsule material coated on the outside of the core material.

[0050] Preferably, the operation of successively heat-sealing and spray-granulating the mixture is to heat-melt the mixture and then spray-granulate the heat-melted mixture in an atomization system.

[0051] Preferably, the parameters of the atomization system are as follows: the rotation speed of the atomization wheel is 15,000 rpm to 25,000 rpm, the inlet air temperature is 2°C to 15°C, the outlet air temperature is 15°C to 30°C, the middle temperature of the chamber is 5°C to 10°C, and the feed rate is 100 mL / min to 1500 mL / min.

[0052] In this embodiment, for ease of production, the operation of heat melting the mixture is accomplished by the feeding system of the heat melt extruder.

[0053] Referring to FIG. 3, the present invention further discloses a method for preparing the microcapsule powder described in the above technical solution, in which the microcapsule powder is prepared by a submerged condensation method, comprising the steps of:

[0054] In S310, the encapsulant is heated until melted.

[0055] The melting point of the capsule material is greater than 42° C., and the capsule material is not degraded or dissolved by proteases and gastric acid, but is degraded by intestinal digestive enzymes.

[0056] In S320, the core material and the molten capsule material are thoroughly mixed while being kept warm to obtain a mixture.

[0057] In S330, the mixture is sheared while being kept warm.

[0058] The shearing speed is 8000 rpm to 10000 rpm, and the shearing time is 6 minutes to 15 minutes.

[0059] In S340, the sheared mixture is spray granulated in the condensate to obtain the microcapsule powder.

[0060] The prepared microcapsule powder comprises a core material and a capsule material coated on the outside of the core material.

[0061] Preferably, the operation of spray granulating the sheared mixture in the condensate is carried out in a condensate dryer.

[0062] Preferably, the parameters of the condensation dryer are as follows: the rotation speed of the spray wheel is 15000 rpm to 25000 rpm, the condensate temperature is 10° C. to 20° C., and the feed rate is 100 mL / min to 1500 mL / min.

[0063] Referring to FIG. 4, the present invention further discloses a method for preparing the microcapsule powder described in the above technical solution, which is prepared by hot-sealing pressing method, and includes the following steps:

[0064] In S410, the core material and the capsule material are thoroughly mixed to obtain a mixture.

[0065] The melting point of the capsule material is greater than 42° C., and the capsule material is not degraded or dissolved by proteases and gastric acid, but is degraded by intestinal digestive enzymes.

[0066] Preferably, a mixer can be used to thoroughly mix the core material and capsule material.

[0067] Preferably, the mixer parameters are as follows: mixing frequency is 25Hz to 40Hz, and mixing time is 30min to 60min.

[0068] In S420, the mixture is successively heat-sealed, pressurized, granulated, and sheared to obtain the microcapsule powder.

[0069] The prepared microcapsule powder comprises a core material and a capsule material coated on the outside of the core material.

[0070] Preferably, the shear speed is from 8000 rpm to 10000 rpm.

[0071] Preferably, the operation of sequentially heat-sealing press-granulating and shearing the mixture is to heat-sealing press-granulate the mixture in a heat-sealing extruder, and then shear the cooled heat-sealing press-granulated product by a shearing system.

[0072] Preferably, the parameters of the heat-sealing extruder are as follows: the pressing temperature is 100° C. to 120° C., the diameter of the pressing die hole is 0.5 mm to 5 mm, and the pressing speed is 5 rpm to 150 rpm. EXAMPLES

[0073] The following is a specific example.

[0074] Example 1 Preparation of microcapsule powder by spray freeze drying method Accurately weigh 540g of rice bran aliphatic alkanol into a 1000mL sandwich pan, keep the temperature of the water bath pan at 80℃ until the rice bran aliphatic alkanol melts, add 60g of NADH to the molten rice bran aliphatic alkanol while keeping it warm, and stir at 500rpm for 10min to mix thoroughly to obtain a suspension. Spray freeze-dry the suspension to granulate it using a spray dryer, and adjust the operating parameters of the spray dryer to 2℃ inlet air temperature, 15℃ outlet air temperature, 5℃ middle chamber temperature, and 1500mL / min feed rate to obtain NADH microcapsule powder coated with rice bran aliphatic alkanol, which is designated as Sample 1.

[0075] Example 2 Preparation of microcapsule powder by heat fusion mixed spraying method Accurately weigh 480g of rice bran aliphatic alkanol and 120g of NADH and put them into the mixer. Start the mixer, set the mixing frequency to 25Hz, and mix for 60min to thoroughly mix the rice bran aliphatic alkanol and NADH. After mixing is completed, feed the mixture into the charging system of the heat-sealing extruder, heat-seal the mixture at 140℃, and transport it to the atomization system for spray embedding granulation. Adjust the rotation speed of the atomization wheel to 15000rpm, the inlet air temperature to 2℃, the outlet air temperature to 15℃, the middle chamber temperature to 5℃, and the feed rate to 1500mL / min to obtain NADH microcapsule powder coated with rice bran aliphatic alkanol, which is sample 2.

[0076] Example 3 Preparation of microcapsule powder by liquid condensation method Accurately weigh out 420g of rice bran aliphatic alkanol and place it in a 1000mL sandwich pan. Heat in a water bath to 90℃ to melt the rice bran aliphatic alkanol. While keeping the pan warm, add 180g of NADH to the molten rice bran aliphatic alkanol to obtain a mixture, and subject the mixture to high shear at 10000rpm. After 6min, connect a condensation dryer containing condensate to the sandwich pan to perform submerged condensation spray granulation. Adjust the rotation speed of the condensation dryer spray wheel to 25000rpm, the condensate temperature to 10℃, and the feed rate to 1500mL / min. Obtain NADH microcapsule powder coated with rice bran aliphatic alkanol and call it Sample 3.

[0077] Example 4 Preparation of microcapsule powder by spray freeze drying method Accurately weigh out 540g of triacontanol and put it into a 1000mL sandwich pan. Keep the temperature of the water bath pan at 100℃ until the rice bran aliphatic alkanol melts. While keeping warm, add 60g of NADPH to the melted triacontanol and stir at 1200rpm for 3min to mix thoroughly to obtain a suspension. Spray freeze-dry the suspension to granulate it using a spray dryer. Adjust the operating parameters of the spray dryer to 20℃ inlet air temperature, 30℃ outlet air temperature, 25℃ middle chamber temperature, and 100mL / min feed rate to obtain a triacontanol-coated NADPH microcapsule powder, designated as Sample 4.

[0078] Example 5 Preparation of microcapsule powder by heat fusion mixed spraying method Accurately weigh out 480g of triacontanol and 120g of NADPH and put them into the mixer. Start the mixer, set the mixing frequency to 40Hz, and mix for 30min to thoroughly mix triacontanol and NADPH. After mixing is completed, feed the mixture into the charging system of the heat-sealing extruder, heat-seal the mixture at 120℃, and transport it to the atomization system for spray embedding granulation. Adjust the rotation speed of the atomization wheel to 25000rpm, the inlet air temperature to 15℃, the outlet air temperature to 30℃, the middle chamber temperature to 10℃, and the feed rate to 100mL / min to obtain NADPH microcapsule powder coated with triacontanol, which is sample 5.

[0079] Example 6 Preparation of microcapsule powder by heat fusion pressing method Accurately weigh 420g of triacontanol and 180g of NADPH, put them into the mixer, mix at 40Hz frequency for 30min, then put the mixture into the feeding system of the heat-sealing extruder, heat-seal the mixture, press it, then enter the molding system to cool. After cooling, enter the shearing system to shear. Adjust the pressing temperature to 120℃, the pressing die hole diameter to 0.5mm, the pressing speed to 150rpm, and the shearing speed to 10000rpm, collect the sheared powder, and obtain the NADPH microcapsule powder coated with triacontanol, which is sample 6.

[0080] Test Example 1: Effect of mass ratio of core material to capsule material on embedding rate Since the core materials NADH and NADPH are highly soluble in water, and the capsule materials rice bran aliphatic alkanol and higher aliphatic alkanol are insoluble in water, when the microcapsule powder prepared in this application is placed in water, the unembedded core material dissolves in the water, and the embedding rate of the core material in the microcapsule powder can be calculated by detecting the content of the core material in the water. The embedding rate of the core material = (theoretical amount of embedded core material in the sample - content of the core material in the aqueous solution detected by HPLC) / theoretical amount of embedded core material in the sample, and the theoretical amount of embedded core material in the sample is the amount of added core material in the sample.

[0081] Detection of the content of the core materials NADH and NADPH by HPLC: 50 mg of sample was accurately weighed and placed in a 25 mL measuring flask, and 25 mL of sodium bicarbonate solution with a concentration of 100 mmol / L was added to the volume, and the unembedded NADH or NADPH was dissolved by ultrasonic for 30 min, and then 1 mL of the solution in the measuring flask was taken, filtered through a 0.22 μm filter membrane, and then injected into an HPLC injection bottle, and the content of NADH or NADPH in the sample solution was detected and calculated by HPLC. The analytical parameters for detection by HPLC method were Agilent 1260 Infinity II equipped with a quaternary pump, autosampler, column thermostat and variable wavelength detector (VWD), separation column ChromCore AQ C18 (5 μm) 4.6 × 250 mm, detection wavelength 260 nm, and the specific parameters for NADH and NADPH detection are shown in Table 1 below.

[0082] [Table 1]

[0083] The detection results of the amount of embedded core material in Samples 1 to 6 in the examples are shown in Table 2. When the mass percentage of the core material and capsule material was (10-30):(70-90), the embedding rate was 93% or more, indicating a good embedding effect.

[0084] [Table 2]

[0085] Test example 2: Stability experiment in an open room temperature environment 2g each of the embodiment samples 2 and 5 are left in an open environment at room temperature for 7 days, and the appearance is observed. Then, 50mg each is weighed out, and after leaving for 7 days, sample 2 and sample 5 are placed in a 50mL centrifuge tube, 45mL of xylene is poured in, the lid is tightened, and the tube is shaken continuously for 30 minutes, and the liquid in the tube is completely transferred to a 125mL separatory funnel, and about 80mL of a 100mmol / L sodium bicarbonate solution is added to the separatory funnel, and the mixture is extracted by shaking continuously for 30 minutes, and then left to stand for 5 to 10 minutes. After the liquid is completely stratified, the lower layer solution is taken and placed in a 100mL measuring flask, and the volume is adjusted to 100mL with a 100mmol / L sodium bicarbonate solution, and the mixture is shaken well. The core material content in the sample is detected by the same detection method as in Test Example 1.

[0086] The retention rate of core material = detected core material content in sample / theoretical amount of core material embedded in sample, and the theoretical amount of core material embedded in sample is the amount of core material added in the sample. The results are shown in Table 3.

[0087] [Table 3]

[0088] From the results in Table 3, it can be seen that the microcapsule powder prepared according to the present invention has a core retention rate of more than 97% after being left in an open environment at room temperature for 7 days, which shows that the microcapsule powder of the present invention can effectively block the effects of moisture and oxygen in the air on the core material, greatly improving the stability of the core material and expanding the prospects for industrial application of the core material.

[0089] Test Example 3 Simulation of release experiment in gastric acid solution The tablet tester is started and preheated, the temperature is set to 37°C, the basket shaft and basket body are attached, the positions (marks) are made with the positioning ball, and the baskets are placed in the dissolution cups (900mL of hydrochloric acid solution with a pH of 1.2 is poured into each dissolution cup) and fixed. Next, 200mg of each of the samples 2 and 5 of the embodiment are taken, wrapped in gauze, and placed in the corresponding basket body. After rotating at a rotation speed of 100r / min for 4 hours, 1mL of liquid is taken from each dissolution cup, and the core material content in each sample is detected using the same detection method as in Example 1.

[0090] Core retention rate = (theoretical amount of core embedded in sample - content of core in detected hydrochloric acid solution) / theoretical amount of core embedded in sample, where the theoretical amount of core embedded in a sample is the amount of core added in the sample, and the calculation results are shown in Table 4. After 4 hours in a strong acid environment, the core retention rates in samples 2 and 5 were still above 90%, indicating that they had excellent acid resistance and the core was not released in the gastric juice environment.

[0091] [Table 4]

[0092] Test Example 4 Release experiment in artificial intestinal fluid Measure with a tablet tester, start the tester to preheat, set the temperature to 37°C, attach the basket shaft and basket body, position (mark) with a positioning ball, and place and fix in the dissolution cup (pour 900mL of prepared artificial intestinal juice into each dissolution cup). Next, take 200mg of each of Sample 2 and Sample 5 of the embodiment and the corresponding core material, wrap them in gauze, and place them in the corresponding basket body. After rotating at a rotation speed of 100r / min for 1, 2, 3, and 4 hours, take 1mL of liquid from each dissolution cup, and detect the core material content in each sample using the same detection method as in Example 1.

[0093] Core retention rate = (theoretical amount of core embedded in sample - detected content of core in artificial intestinal fluid) / theoretical amount of core embedded in sample, where the theoretical amount of core embedded in a sample is the amount of core added in the sample, and the calculation results are shown in Table 5. After 1 hour in the artificial intestinal fluid environment, the core dissolution rates in Samples 2 and 5 were both 85% or more, and after 3 hours, the core dissolution rates in Samples 2 and 5 were both 95% or more, which means that the capsule material of the microcapsule powder of the present application can be smoothly decomposed in the intestinal tract, allowing the core material to be absorbed by the intestinal tract and to perform its role in the intestinal tract.

[0094] [Table 5]

[0095] Test example 5 Acceleration stability experiment Sample 2 and sample 5 of the embodiment are simultaneously placed in an acceleration box at 37 ° C and 75% humidity, and two sets of samples are simultaneously subjected to product stability experiments for 1 month, 2 months, and 3 months. At 0 months, 1 month, 2 months, and 3 months, 50 mg of sample 2 and 5 are weighed into a 50 mL centrifuge tube, 45 mL of xylene is poured in, the lid is tightened, and after continuous shaking for 30 minutes, the liquid in the centrifuge tube is completely transferred to a 125 mL separatory funnel, about 80 mL of a sodium bicarbonate solution with a concentration of 100 mmol / L is added to the separatory funnel, and the mixture is extracted by shaking continuously for 30 minutes, and then left to stand for 5 to 10 minutes. After the liquid is completely stratified, the lower layer solution is taken and placed in a 100 mL measuring flask, and the volume is adjusted to 100 mL with a sodium bicarbonate solution with a concentration of 100 mmol / L, and shaken well. 1 mL of the above sample is sucked up, and the core material content in the sample is detected by the same detection method as in Example 1.

[0096] Core retention rate = detected core content in sample / theoretical amount of core embedded in sample, where the theoretical amount of core embedded in sample is the amount of core added in the sample, and the results are shown in Table 6. After three months of acceleration, the core content retention rates of the two sets of samples decreased slightly, but were both above 90%, meeting the product acceptance criteria for general accelerated experiments, indicating that the stability of the microcapsule powder prepared by the present invention is good.

[0097] [Table 6]

[0098] The above examples describe some embodiments of the present invention, and the description is relatively specific and detailed, but this should not be understood as a limitation on the scope of the patent application. It should be noted that those skilled in the art can make a number of modifications and improvements without departing from the concept of the present invention, all of which are within the scope of protection of the present invention. Therefore, the scope of protection of the patent of the present invention should be based on the scope of the appended claims.

[0099] This application claims priority to a Chinese patent application submitted to the China Patent Office on July 20, 2021, bearing application number CN202110819545.5 and entitled "Microcapsule powder stable in gastric acid, preparation method, and use," the entire contents of which are incorporated herein by reference.

Claims

1. A microcapsule powder that is stable in gastric acid, comprising a core material and an encapsulant covering the outside of the core material, the encapsulant having a melting point of more than 42°C, the encapsulant not being decomposed or dissolved by proteases and gastric acid, but being decomposed by intestinal digestive enzymes; the encapsulant is rice bran fatty alkanol; The core material is selected from at least one of reduced nicotinamide adenine dinucleotide and reduced nicotinamide adenine dinucleotide phosphate; A microcapsule powder stable in gastric acid, characterized in that the particle size of the microcapsule powder is 1 μm to 1000 μm.

2. 2. The microcapsule powder according to claim 1, wherein the melting point of the encapsulant is 60°C to 140°C.

3. 2. The microcapsule powder according to claim 1, wherein a mass ratio of the capsule material to the core material is 70-90:10-30.

4. A method for preparing the microcapsule powder according to claim 1, comprising the steps of: heating the encapsulant until melted; mixing the core material and the molten encapsulant sufficiently while keeping the temperature, to obtain a suspension of particles of the core material in the molten encapsulant; and spray-freeze-drying and granulating the suspension to obtain a microcapsule powder containing the core material and the capsule material coated on the outside of the core material. The preparation method is characterized in that the melting point of the encapsulating material is greater than 42°C, and the encapsulating material is not degraded or dissolved by proteases and gastric acid, but is degraded by intestinal digestive enzymes.

5. A method for preparing the microcapsule powder according to claim 1, comprising the steps of: thoroughly mixing the core material and the encapsulant to obtain a mixture; and sequentially subjecting the mixture to heat fusion and spray granulation to obtain the microcapsule powder containing the core material and the capsule material coated on the outside of the core material. The preparation method is characterized in that the melting point of the encapsulating material is greater than 42°C, and the encapsulating material is not degraded or dissolved by proteases and gastric acid, but is degraded by intestinal digestive enzymes.

6. A method for preparing the microcapsule powder according to claim 1, comprising the steps of: heating the encapsulant until melted; a step of thoroughly mixing the core material and the molten capsule material while keeping the temperature, to obtain a mixture; shearing the mixture at a shear rate of 10,000 rpm to 16,000 rpm for a shear time of 6 min to 15 min while keeping the mixture warm; The mixture after shearing is spray-granulated in a condensate to obtain the microcapsule powder including the core material and the capsule material coated on the outside of the core material. The preparation method is characterized in that the melting point of the encapsulating material is greater than 42°C, and the encapsulating material is not degraded or dissolved by proteases and gastric acid, but is degraded by intestinal digestive enzymes.

7. A method for preparing the microcapsule powder according to claim 1, comprising the steps of: thoroughly mixing the core material and the encapsulant to obtain a mixture; and sequentially subjecting the mixture to heat fusion press granulation and shearing to obtain the microcapsule powder containing the core material and the capsule material coated on the outside of the core material, wherein the shearing speed is 8000 to 10000 rpm; The preparation method is characterized in that the melting point of the encapsulating material is greater than 42°C, and the encapsulating material is not degraded or dissolved by proteases and gastric acid, but is degraded by intestinal digestive enzymes.

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