A kind of Noni fruit enzyme sustained-release microcapsule powder and preparation method thereof

Abstract

A noni fruit enzyme sustained-release microcapsule powder and a preparation method thereof, which relates to a noni fruit enzyme microcapsule and a preparation method thereof. The purpose of the present invention is to solve the problems that the processed products of noni fruit on the market are in a single form, the taste of noni fruit fresh fruit juice is poor, the biologically active ingredients are low, the biologically active ingredients of noni fruit enzyme fermentation products are easily inactivated during storage, transportation or sales, and the noni fermented concentrated juice is viscous and syrupy or hard block-like after drying, easy to gel and return to moisture, difficult to brew, and has extremely poor sensory properties. Method: 1. Prepare noni fruit enzyme slurry; 2. Prepare wall material mixture; 3. Prepare noni fruit enzyme emulsion; 4. Freeze-dry once; 5. Freeze-dry twice. The noni fruit enzyme sustained-release microcapsule powder prepared by the present invention has excellent thermal stability, the noni fruit enzyme will not denature within the temperature range of daily brewing and consumption, and the stability is significantly improved; it is slowly released under the gastric environment and has a directional long-acting sustained-release characteristic.

Description

Technical Field

[0001] The invention relates to a noni fruit enzyme microcapsule and a preparation method thereof. Background Art

[0002] Noni Morindacitrifolia L ), also known as seaside wood Morinda officinalis, four-season fruit, Chinese toon root and Indian mulberry, Morinda officinalis shrubs and small trees. As a tropical plant, Morinda officinalis is susceptible to cold damage. The precipitation in its suitable planting area should be 600mm~1500 mm, the annual sunshine hours should be 1900h~2200h, the annual average temperature should not be lower than 20℃~28℃, the average temperature of the coldest month should not be lower than 13℃, the absolute minimum temperature should be above 5℃, and the altitude should be 300m~600m (generally not more than 700m). In addition, high temperature and humid climate conditions may lead to the occurrence of pathogens and pests, especially serious damage to leaves and fruits. At present, the main planting areas of Noni in my country are limited to Hainan, Xishuangbanna, Yunnan, and Taiwan, China, with very small-scale planting.

[0003] The fruit of Noni is called Noni fruit. The mature Noni fruit has a strong special smell and is also called "cheese fruit". Noni fruit is rich in more than 100 kinds of nutrients and phytochemicals that are beneficial to human health, including more than ten kinds of vitamins and mineral elements, several essential amino acids and amino acids, and a variety of polysaccharides, polyphenols, flavonoids, alkaloids and other biologically active substances with antioxidant stress. It is a super combination of nutrients in natural plants. The residents of the producing area regard it as a health fruit and it is also known as the "holy fruit". Therefore, it is very necessary to process and promote Noni fruit and related products.

[0004] First-grade noni fruit is planted 1km~15km away from the coastline, second-grade noni fruit is planted 15km~40km away from the coastline, and third-grade noni fruit is planted 40km~80km away from the coastline. Although the fruit ripens from August to November every year, noni fruit blooms and bears fruit at the same time, and the fruit ripens inconsistently. The same tree often has ripe fruit, green fruit, and young fruit at the same time. Ripe fruit is very easy to rot, difficult to store, has a special smell, tastes bitter, and is difficult to eat immediately. Therefore, people make ripe noni fruit into noni fresh fruit juice, but noni fresh fruit juice also has the problem of high bitter acid content, sour and smelly flavor, and is difficult to be accepted by consumers. At present, the main form of noni fruit products commonly seen on the market is artificial formula noni fruit powder and derivative products using noni fresh fruit as raw materials, which are mainly used in food compound formulas (milk tea, biscuits, jelly, etc.), tablet dried fruit, daily chemical products, etc.

[0005] Since the fresh noni fruit juice is liquid, it has the problems of single product form, difficult to carry and store, low bioactive substances and easy inactivation of bioactive substances; the bioactive substances in the artificial formula noni fruit powder and its derivative products using fresh noni fruit as raw materials are lower than those in the fresh noni fruit juice, and also have the problem of easy inactivation of bioactive substances. Therefore, the fresh noni fruit juice and the artificial formula noni fruit powder and its derivative products using fresh noni fruit as raw materials on the market are not recognized by people;

[0006] After fermentation, the content of active ingredients and antioxidant capacity in noni fruit are significantly improved, and the obtained noni fermented juice is rich in nutrition and soft in flavor. In addition, the antioxidant activity of noni enzyme liquid is higher than that of commercial fruit wines such as dry white wine, apple wine, pineapple wine and lychee wine, and is second only to dry red wine. Therefore, noni fruit fermentation stock and derivative products have appeared on the market. Noni juice is fermented by pure or compound bacteria, and then filtered, concentrated, mixed and other post-processing processes to obtain noni fruit enzyme liquid. The enzyme mainly contains bioactive ingredients such as polyphenols and flavonoids, which have better antioxidant, anti-cancer and anti-inflammatory biological effects than fresh fruit juice; at the same time, some of the pungent acid evaporates after fermentation, which improves the flavor to a certain extent. Therefore, noni fruit fermentation processing juice has gradually occupied a certain market share. Noni fermented juice is mainly reflected in noni wine and noni pulp. Noni pulp mainly uses noni enzyme flavored juice that is diluted or compound blended in large quantities. The main storage method and product form of noni fruit enzyme fermentation products are liquid products. The biologically active ingredients are easily inactivated by external environments such as light, heat, and oxygen during storage, transportation, or sales, and effective protection of the biologically active ingredients cannot be achieved.

[0007] Technicians have also tried to dry the fermented noni concentrated juice into solid products, but they have not been successful and have not been able to be put on the market as a product. This is mainly because it contains a lot of highly viscous substances such as pectin polysaccharides. After drying and losing water, the original juice will appear as a sticky syrup or hard block-like product, and it is easy to gel and return to moisture, difficult to dissolve, and has extremely poor sensory properties. As a result, the current noni fruit product market is in an embarrassing situation where various liquid products dominate and the product form is single.

[0008] Therefore, the noni enzyme market is in urgent need of developing new technologies to solve the current development potential of noni enzymes, and in urgent need of effective processing technologies to reduce and protect the biological efficacy components of noni enzyme products, improve sensory properties such as flavor, solve the problems of single product form, and develop diversified product forms. Therefore, the powderization of fermented noni enzyme juice has become a bright hope that can be expected, but there is little research on product market development at home and abroad. Summary of the invention

[0009] The purpose of the present invention is to solve the problems that the processed products of noni fruit on the market are in a single form, the fresh noni fruit juice has a poor taste and low biologically active ingredients, the biologically active ingredients of noni fruit enzyme fermentation products are easily inactivated during storage, transportation or sales, and the noni fermented concentrated juice appears sticky and syrupy or hard block-like after drying, is easy to gel and return to moisture, is difficult to be brewed, and has extremely poor sensory properties, and to provide a noni fruit enzyme sustained-release microcapsule and a preparation method thereof.

[0010] A method for preparing a noni fruit enzyme sustained-release microcapsule powder is specifically completed by the following steps:

[0011] 1. Preparation of concentrated Noni enzyme puree:

[0012] ①, wash fresh and ripe noni fruit, drain the water, put it in a fermentation tank, seal the fermentation tank, put it in a cool place, and ferment it anaerobically at room temperature for 1 to 3 years to obtain fermented noni fruit pulp;

[0013] ②, subjecting the fermented noni fruit pulp to ultrasonic treatment to obtain ultrasonic noni fruit pulp;

[0014] ③. Filter and remove the coarse impurities in the ultrasonic noni fruit pulp under normal pressure, then centrifuge the filtrate at low temperature, collect the supernatant, and obtain the clarified noni fruit enzyme pulp;

[0015] ④. Under the condition of 35℃~50℃, concentrate the clarified Noni fruit enzyme puree to 1 / 3~1 / 5 of the original volume to obtain concentrated Noni fruit enzyme puree;

[0016] 2. Preparing a wall material mixed solution: placing maltodextrin and gum arabic in deionized water, controlling the water bath temperature to 65°C-85°C, and stirring with a magnetic force until they are completely dissolved to obtain a uniform mixed solution I; cooling the mixed solution I to a final temperature of 45°C by program cooling to obtain a wall material mixed solution;

[0017] 3. Preparation of Noni Fruit Enzyme Emulsion:

[0018] Add the wall material mixture and glucono-δ-lactone into the Noni fruit enzyme stock, keep the water bath temperature at 45°C to 55°C, stir and react to obtain the Noni fruit enzyme emulsion;

[0019] 4. Freeze-drying:

[0020] The noni fruit enzyme emulsion is pre-frozen at -20°C, then vacuum-freeze-dried, and finally ground to obtain a primary freeze-dried product;

[0021] 5. Secondary freeze drying:

[0022] The primary freeze-dried product, white sugar powder and silicon dioxide are mixed evenly to obtain a composite powder; the composite powder is pre-frozen at -20°C, vacuum freeze-dried, and finally ground to obtain the noni fruit enzyme sustained-release microcapsule powder.

[0023] Advantages of the present invention:

[0024] 1. The present invention takes Hainan tropical noni fruit enzyme puree as the research object, and focuses on the research and development of the preparation process of noni fruit enzyme microencapsulation products with high biological activity potential for noni fruit series products, aiming at the key technical obstacles that have always existed in the noni fruit processing industry, such as the lack of powder products with good properties. Through the above-mentioned research, the problem of the single form of noni fruit processing products in the current market is solved, and the biological activity of the products is reduced and protected, so as to create a variety of noni fruit enzyme new products with long shelf life, excellent sensory properties, and active in vivo sustained release based on new technologies, and provide technical support for the sustainable development of Hainan tropical berry economy.

[0025] Second, the present invention uses noni fruit enzyme as the core material, maltodextrin and gum arabic as the wall material, and adopts microcapsule technology to prepare noni fruit enzyme sustained-release microcapsules, thereby retaining the activity of noni fruit enzyme to the maximum extent; microcapsule technology is a preparation technology for encapsulating trace substances in polymer films, and is also a micro-encapsulation technology for storing solids, liquids and gases. The encapsulated substances are released at a controlled rate only under specific conditions, that is, the efficacy of the encapsulated substances is controlled and sustained-released; the principle is to completely encapsulate a certain target object (core material) with a continuous film (wall material) of various natural or synthetic polymer compounds, without damaging the chemical properties of the active ingredients of the original target object, and then gradually induce the functional components of the target object to be released through certain external environmental stimulation or sustained-release effects and to present their efficacy externally again, and the protection of the core material is achieved by relying on the shielding effect of the wall material;

[0026] 3. The noni enzyme sustained-release microcapsules prepared by the present invention have good dispersion, uniform particle size distribution of 1.5 μm to 3 μm, and high solubility, which solves the problems that the biologically active ingredients of noni enzyme fermentation products on the market are easily inactivated during storage, transportation or sales, and the noni fermented concentrated juice after drying is sticky and syrupy or hard and lumpy, easy to gel and return to moisture, difficult to be diluted, and has extremely poor sensory properties;

[0027] Fourth, the noni enzyme sustained-release microcapsules prepared by the present invention have excellent thermal stability, and the noni enzyme will not denature within the temperature range of daily preparation and consumption, thus solving the problem that the biologically active ingredients of noni enzyme fermentation products on the market are easily inactivated during storage, transportation or sales;

[0028] 5. The noni enzyme sustained-release microcapsules prepared by the present invention have excellent storage stability. Compared with the noni enzyme puree, the stability is significantly improved under continuous sunlight and atmospheric exposure, which solves the problem that the biologically active ingredients of noni enzyme fermentation products on the market are easily inactivated during storage, transportation or sales;

[0029] 6. The noni enzyme sustained-release microcapsules prepared by the present invention are released slowly in the gastric environment, and most of the active substances are released in the intestinal environment, with directional long-acting sustained-release characteristics, which solves the problems of poor taste and low biologically active ingredients of noni fresh fruit juice on the market. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] Figure 1 This is a full-wavelength ultraviolet scanning image of the noni fruit enzyme puree obtained in step 1 of Example 1;

[0031] Figure 2 This is a physical picture of the noni fruit enzyme puree obtained in step 1 of Example 1 after vacuum freeze drying;

[0032] Figure 3 This is a physical picture of the Noni fruit enzyme sustained-release microcapsule powder obtained in step 5 of Example 1;

[0033] Figure 4 This is a physical picture of the noni enzyme sustained-release microcapsule powder obtained in step 5 of Example 1 after rehydration;

[0034] Figure 5 is a particle size distribution diagram of the Noni enzyme sustained-release microcapsule powder obtained in step 5 of Example 1;

[0035] Figure 6 This is a scanning electron microscope image of the Noni enzyme sustained-release microcapsule powder obtained in step 5 of Example 1 at a magnification of 20k times;

[0036] Figure 7 is an infrared spectrum, in which a represents the infrared spectrum of the Noni fruit enzyme puree obtained in step 1 of Example 1, and b represents the infrared spectrum of the Noni fruit enzyme sustained-release microcapsule powder obtained in step 5 of Example 1;

[0037] Figure 8 is an X-ray diffraction spectrum, in which a represents the X-ray diffraction spectrum of the Noni fruit enzyme puree obtained in step 1 of Example 1, and b represents the X-ray diffraction spectrum of the Noni fruit enzyme sustained-release microcapsule powder obtained in step 5 of Example 1;

[0038] Fig. 9 This is the ultraviolet full wavelength scanning image of the noni fruit enzyme sustained-release microcapsule powder obtained in step 5 of Example 1;

[0039] Fig.10 is a differential scanning calorimetry spectrum, in which a represents the differential scanning calorimetry spectrum of the Noni fruit enzyme puree obtained in step 1 of Example 1, and b represents the differential scanning calorimetry spectrum of the Noni fruit enzyme sustained-release microcapsule powder obtained in step 5 of Example 1;

[0040] Fig.11 Graphs a and b are thermogravimetric spectra of the noni enzyme puree obtained in step 1 of Example 1, and graphs b and b are thermogravimetric spectra of the noni enzyme sustained-release microcapsule powder obtained in step 5 of Example 1;

[0041] Fig.12 : is a light stability graph, in which ■ represents the absorbance change curve of the Noni fruit enzyme puree obtained in step 1 of Example 1 under 8 days of continuous sunlight, and ● represents the absorbance change curve of the Noni fruit enzyme sustained-release microcapsule powder obtained in step 5 of Example 1 under 8 days of continuous sunlight;

[0042] Fig.13 : is a thermal stability graph, in which ■ represents the absorbance change curve of the Noni fruit enzyme puree obtained in step one of Example 1 under 60°C, ◆ represents the absorbance change curve of the Noni fruit enzyme puree obtained in step one of Example 1 under 80°C, ● represents the absorbance change curve of the Noni fruit enzyme puree obtained in step one of Example 1 under 100°C, □ represents the absorbance change curve of the Noni fruit enzyme sustained-release microcapsule powder obtained in step five of Example 1 under 60°C, ◇ represents the absorbance change curve of the Noni fruit enzyme sustained-release microcapsule powder obtained in step five of Example 1 under 80°C, and ○ represents the absorbance change curve of the Noni fruit enzyme sustained-release microcapsule powder obtained in step five of Example 1 under 100°C;

[0043] Fig.14 is an atmospheric stability diagram, in which ■ represents the absorbance change curve of the Noni fruit enzyme puree obtained in step 1 of Example 1 exposed to the atmosphere for 8 days, and ● represents the absorbance change curve of the Noni fruit enzyme sustained-release microcapsule powder obtained in step 5 of Example 1 exposed to the atmosphere for 8 days;

[0044] Fig.15 is the cumulative release rate of the Noni enzyme sustained-release microcapsule powder obtained in step 5 of Example 1 in artificial gastric juice and artificial intestinal juice;

[0045] Fig.16 These are digital photos of the Noni fruit enzyme sustained-release microcapsule powder prepared in Example 1 and the Noni fruit enzyme powder prepared in Comparative Example 1, wherein 0 is the Noni fruit enzyme powder prepared in Comparative Example 1, and 1 is the Noni fruit enzyme sustained-release microcapsule powder prepared in Example 1. DETAILED DESCRIPTION

[0046] Specific implementation method 1: This implementation method is a noni fruit enzyme sustained-release microcapsule powder, which is characterized in that it uses noni fruit enzyme as the core material, maltodextrin and gum arabic as the wall material, forms noni fruit enzyme microcapsule emulsion at a mild temperature, and obtains noni fruit enzyme sustained-release microcapsule powder by vacuum freeze-drying.

[0047] Specific implementation method 2: This implementation method is a method for preparing a noni enzyme sustained-release microcapsule powder, which is specifically completed by the following steps:

[0048] 1. Preparation of concentrated Noni enzyme puree:

[0049] ①, wash fresh and ripe noni fruit, drain the water, put it in a fermentation tank, seal the fermentation tank, put it in a cool place, and ferment it anaerobically at room temperature for 1 to 3 years to obtain fermented noni fruit pulp;

[0050] ②, subjecting the fermented noni fruit pulp to ultrasonic treatment to obtain ultrasonic noni fruit pulp;

[0051] ③. Filter and remove the coarse impurities in the ultrasonic noni fruit pulp under normal pressure, then centrifuge the filtrate at low temperature, collect the supernatant, and obtain the clarified noni fruit enzyme pulp;

[0052] ④. Under the condition of 35℃~50℃, concentrate the clarified Noni fruit enzyme puree to 1 / 3~1 / 5 of the original volume to obtain concentrated Noni fruit enzyme puree;

[0053] 2. Preparing a wall material mixed solution: placing maltodextrin and gum arabic in deionized water, controlling the water bath temperature to 65°C-85°C, and stirring with a magnetic force until they are completely dissolved to obtain a uniform mixed solution I; cooling the mixed solution I to a final temperature of 45°C by program cooling to obtain a wall material mixed solution;

[0054] 3. Preparation of Noni Fruit Enzyme Emulsion:

[0055] Add the wall material mixture and glucono-δ-lactone into the Noni fruit enzyme stock, keep the water bath temperature at 45°C to 55°C, stir and react to obtain the Noni fruit enzyme emulsion;

[0056] 4. Freeze-drying:

[0057] The noni fruit enzyme emulsion is pre-frozen at -20°C, then vacuum-freeze-dried, and finally ground to obtain a primary freeze-dried product;

[0058] 5. Secondary freeze drying:

[0059] The primary freeze-dried product, white sugar powder and silicon dioxide are mixed evenly to obtain a composite powder; the composite powder is pre-frozen at -20°C, vacuum freeze-dried, and finally ground to obtain the noni fruit enzyme sustained-release microcapsule powder.

[0060] Specific implementation method 3: The difference between this implementation method and specific implementation method 2 is that in step 1②, the fermented noni fruit pulp is ultrasonically treated for 60 min to 120 min at a temperature of 30°C to 40°C and a frequency of 500W to 1000W. The other steps are the same as those in specific implementation method 2.

[0061] Specific embodiment 4: This embodiment differs from specific embodiments 2 to 3 in that: in step 1 ③, the coarse impurities in the ultrasonicated noni fruit pulp are filtered out under normal pressure, and then the filtrate is centrifuged at low temperature for 10 min to 30 min at 4°C and 8000 r / s to 10000 r / s, and the supernatant is collected to obtain a clarified noni fruit enzyme pulp. The other steps are the same as those of specific embodiments 2 to 3.

[0062] Specific embodiment 5: This embodiment differs from specific embodiments 2 to 4 in that: in step 2, the mixed solution I is cooled to a final temperature of 45° C. by programmed cooling for 30 minutes. The other steps are the same as those of specific embodiments 2 to 4.

[0063] Specific embodiment 6: This embodiment differs from specific embodiments 2 to 5 in that the concentration of maltodextrin in the mixed solution I described in step 2 is 0.01 g / mL to 0.04 g / mL, and the concentration of gum arabic is 0.02 g / mL to 0.04 g / mL. The other steps are the same as those of specific embodiments 2 to 5.

[0064] Specific embodiment 7: This embodiment differs from specific embodiments 2 to 6 in that the stirring reaction time in step 3 is 30 min to 90 min. The other steps are the same as those in specific embodiments 2 to 6.

[0065] Specific embodiment 8: This embodiment differs from specific embodiments 2 to 7 in that the volume ratio of the wall material mixture to the Noni fruit enzyme puree in step 3 is 1:10; the mass ratio of glucono-δ-lactone to the Noni fruit enzyme puree is 1.5:100. The other steps are the same as specific embodiments 2 to 7.

[0066] Specific embodiment 9: This embodiment differs from specific embodiments 2 to 8 in that: in step 4, the noni enzyme emulsion is pre-frozen at -20°C for 8h to 12h, then vacuum freeze-dried for 24h to 48h, and finally ground for 0.1h to 0.3h to obtain a primary freeze-dried product. The other steps are the same as those of specific embodiments 2 to 8.

[0067] Specific embodiment 10: The difference between this embodiment and specific embodiments 2 to 9 is that: in step 5, the mass ratio of the primary freeze-dried product, white sugar powder and silicon dioxide is 30:40:1; in step 5, the composite powder is pre-frozen at -20°C for 8h~12h, then vacuum freeze-dried for 24h~48h, and finally ground for 0.1h~0.3h to obtain the noni fruit enzyme sustained-release microcapsule powder. The other steps are the same as specific embodiments 2 to 9.

[0068] The following test is used to verify the beneficial effects of the present invention:

[0069] Embodiment 1: A method for preparing a noni enzyme sustained-release microcapsule powder is specifically completed by the following steps:

[0070] 1. Preparation of concentrated Noni enzyme puree:

[0071] ①, wash fresh and ripe noni fruit, drain the water, put it in a fermentation tank, seal the fermentation tank, put it in a cool place, and ferment it anaerobically at room temperature for 3 years to obtain fermented noni fruit pulp;

[0072] ②, subjecting the fermented noni fruit pulp to ultrasonic treatment for 90 minutes at a temperature of 38° C. and a frequency of 500 W to obtain ultrasonic noni fruit pulp;

[0073] ③. Filter under normal pressure to remove the coarse impurities in the ultrasonic noni fruit pulp, then centrifuge the filtrate at 4°C and 10,000 r / s for 10 minutes, collect the supernatant, and obtain the clarified noni fruit enzyme pulp;

[0074] ④. At 45°C, the clarified Noni fruit enzyme puree was concentrated to 1 / 4 of the original volume to obtain concentrated Noni fruit enzyme puree;

[0075] 2. Preparation of wall material mixed solution: maltodextrin and gum arabic are placed in deionized water, the water bath temperature is controlled at 75°C, and magnetic stirring is performed for 10 minutes until they are completely dissolved to obtain a uniform mixed solution I; the mixed solution I is slowly cooled for 30 minutes to a final temperature of 45°C by program cooling to obtain a wall material mixed solution;

[0076] The concentration of maltodextrin in the mixed solution I described in step 2 is 0.012 g / mL, and the concentration of gum arabic is 0.024 g / mL;

[0077] 3. Preparation of Noni Fruit Enzyme Emulsion:

[0078] Add the wall material mixture and glucono-δ-lactone into the Noni fruit enzyme slurry, keep the water bath temperature at 45°C, and stir for 60 minutes to obtain the Noni fruit enzyme emulsion;

[0079] The volume ratio of the wall material mixture described in step 3 to the Noni fruit enzyme puree is 1:10;

[0080] The mass ratio of glucono-δ-lactone to noni enzyme puree described in step 3 is 1.5:100;

[0081] 4. One-time freeze-drying:

[0082] The noni enzyme emulsion was pre-frozen at -20°C for 12 hours, then vacuum-freeze-dried for 48 hours, and finally ground for 0.2 hours to obtain a primary freeze-dried product;

[0083] 5. Secondary freeze drying:

[0084] The primary freeze-dried product, white sugar powder and silicon dioxide are mixed evenly to obtain a composite powder; the composite powder is pre-frozen at -20°C for 12 hours, vacuum freeze-dried for 48 hours, and finally ground for 0.2 hours to obtain a noni enzyme sustained-release microcapsule powder;

[0085] In step 5, the mass ratio of the primary freeze-dried product, white sugar powder and silicon dioxide is 30:40:1.

[0086] Figure 1 This is a full-wavelength ultraviolet scanning image of the noni fruit enzyme puree obtained in step 1 of Example 1;

[0087] from Figure 1 It can be seen that there is an obvious absorption peak at 283nm, which can determine that the characteristic absorption wavelength of noni fruit enzyme puree is 283nm.

[0088] Figure 2 This is a physical picture of the noni fruit enzyme puree obtained in step 1 of Example 1 after vacuum freeze drying;

[0089] Figure 3 This is a physical picture of the Noni fruit enzyme sustained-release microcapsule powder obtained in step 5 of Example 1;

[0090] Figure 4 This is a physical picture of the noni enzyme sustained-release microcapsule powder obtained in step 5 of Example 1 after rehydration;

[0091] Depend on Figures 2~4 It can be seen that the product of Noni fruit enzyme puree has strong adhesion after freeze-drying, and the Noni fruit enzyme sustained-release microcapsule powder is dry and has good rehydration property. The solution is clear after being diluted with water.

[0092] Figure 5 is a particle size distribution diagram of the Noni enzyme sustained-release microcapsule powder obtained in step 5 of Example 1;

[0093] Depend on Figure 5It can be seen that the particle size distribution of the Noni fruit enzyme sustained-release microcapsule powder is uniform, with a particle size of 1.5~3μm.

[0094] Figure 6 This is a scanning electron microscope image of the Noni enzyme sustained-release microcapsule powder obtained in step 5 of Example 1 at a magnification of 20k times;

[0095] Depend on Figure 6 It can be seen that the noni enzyme sustained-release microcapsule powder has good dispersion and no aggregation occurs. Vacuum freeze drying is used in the preparation of noni enzyme microcapsules. Since liquid water forms ice crystals during the pre-freezing process, the original emulsified structure is destroyed, so the morphology of the microcapsules changes; in addition, noni enzyme has a high viscosity and is difficult to form a regular sphere during the emulsification process, so the noni enzyme microcapsules are rod-shaped.

[0096] Figure 7 is an infrared spectrum, in which a represents the infrared spectrum of the Noni fruit enzyme puree obtained in step 1 of Example 1, and b represents the infrared spectrum of the Noni fruit enzyme sustained-release microcapsule powder obtained in step 5 of Example 1;

[0097] Depend on Figure 7 It can be seen that 576cm -1 is the skeletal vibration of the pyran ring of maltodextrin, 1371 cm -1 is the bending vibration peak of maltodextrin OH, 1457 cm -1 is the bending vibration peak of CH2, 1582 cm -1 and 2945 cm -1 They are the C=C vibration and CH vibration peaks of gum arabic, indicating that the microcapsules contain two wall materials, gum arabic and maltodextrin. A comparison between a and b shows that the main substances of noni enzyme have not changed after encapsulation, and the encapsulation method has not destroyed the structure of noni enzyme.

[0098] Figure 8 is an X-ray diffraction spectrum, in which a represents the X-ray diffraction spectrum of the Noni fruit enzyme puree obtained in step 1 of Example 1, and b represents the X-ray diffraction spectrum of the Noni fruit enzyme sustained-release microcapsule powder obtained in step 5 of Example 1;

[0099] Depend on Figure 8 It can be seen that a short and wide dispersion band is produced at 12° before and after embedding, indicating that the microcapsules are amorphous structures.

[0100] Fig. 9 This is the ultraviolet full wavelength scanning image of the noni fruit enzyme sustained-release microcapsule powder obtained in step 5 of Example 1;

[0101] and Figure 1In comparison, the maximum absorption wavelength of the noni enzyme microcapsule powder did not change, indicating that this encapsulation method would not destroy the activity of the noni enzyme.

[0102] Fig.10 is a differential scanning calorimetry spectrum, in which a represents the differential scanning calorimetry spectrum of the Noni fruit enzyme puree obtained in step 1 of Example 1, and b represents the differential scanning calorimetry spectrum of the Noni fruit enzyme sustained-release microcapsule powder obtained in step 5 of Example 1;

[0103] Depend on Fig.10 From a, we can see that since the noni enzyme is a mixture, there is a large exothermic peak at 600℃~800℃; Fig.10 As shown in Figure b, the exothermic peak at 600℃~800℃ weakened after microencapsulation, indicating that the encapsulation of noni fruit enzyme was successful and microencapsulation improved the thermal stability of noni fruit enzyme.

[0104] Fig.11 Graphs a and b are thermogravimetric spectra of the noni enzyme puree obtained in step 1 of Example 1, and graphs b and b are thermogravimetric spectra of the noni enzyme sustained-release microcapsule powder obtained in step 5 of Example 1;

[0105] Depend on Fig.11 It can be seen that during the heating process from room temperature to about 110°C, the thermogravimetric curve of the microcapsules is relatively flat, and the mass decreases slightly. This is due to the slow evaporation of the small amount of water remaining in the microcapsules. The overall mass retention rate is still above 95%, indicating that the microcapsules are not thermally damaged at this stage and have good thermal stability. When the temperature exceeds 110°C, the curve drops sharply due to the rapid decomposition of the microcapsules. Within the temperature range of daily consumption and storage, the microcapsules have excellent thermal stability.

[0106] Fig.12 : is a light stability graph, wherein ■ in the graph represents the absorbance change curve of the Noni fruit enzyme puree obtained in step 1 of Example 1 under 8 days of continuous sunlight, and ● in the graph represents the absorbance change curve of the Noni fruit enzyme sustained-release microcapsule powder obtained in step 5 of Example 1 under 8 days of continuous sunlight;

[0107] Depend on Fig.12 It can be seen that after 8 days of sunlight irradiation, the absorbance of Noni fruit enzyme puree decreased by 0.17, and the polyphenol preservation rate was 82.95%. The absorbance of Noni fruit enzyme sustained-release microcapsules decreased by 0.09, and the preservation rate was 91.66%, indicating that the light stability of Noni fruit enzyme was significantly improved after microencapsulation.

[0108] Fig.13: is a thermal stability graph, in which ■ represents the absorbance change curve of the Noni fruit enzyme puree obtained in step one of Example 1 under 60°C, ◆ represents the absorbance change curve of the Noni fruit enzyme puree obtained in step one of Example 1 under 80°C, ● represents the absorbance change curve of the Noni fruit enzyme puree obtained in step one of Example 1 under 100°C, □ represents the absorbance change curve of the Noni fruit enzyme sustained-release microcapsule powder obtained in step five of Example 1 under 60°C, ◇ represents the absorbance change curve of the Noni fruit enzyme sustained-release microcapsule powder obtained in step five of Example 1 under 80°C, and ○ represents the absorbance change curve of the Noni fruit enzyme sustained-release microcapsule powder obtained in step five of Example 1 under 100°C;

[0109] Depend on Fig.13 It can be seen that when the temperature exceeds 60℃, the absorbance of the Noni enzyme pulp gradually decreases with time, and the absorbance decreases more significantly with the increase of temperature, indicating that the polyphenol groups of the Noni enzyme liquid are oxidized and destroyed after heating, and the activity decreases. Under the conditions of 100℃ and 120 min, the absorbance of the Noni enzyme sustained-release microcapsules decreased by 0.11, and the preservation rate was 89.32%, while the absorbance of the unencapsulated Noni enzyme pulp decreased by 0.53, and the polyphenol preservation rate of the enzyme liquid was only 47.43%. It shows that microencapsulation significantly improves the thermal stability of Noni enzyme.

[0110] Fig.14 is an atmospheric stability diagram, in which ■ represents the absorbance change curve of the Noni fruit enzyme puree obtained in step 1 of Example 1 exposed to the atmosphere for 8 days, and ● represents the absorbance change curve of the Noni fruit enzyme sustained-release microcapsule powder obtained in step 5 of Example 1 exposed to the atmosphere for 8 days;

[0111] Depend on Fig.14 It can be seen that after the noni fruit enzyme puree was exposed to the atmosphere for 8 days, the absorbance decreased by 0.54, the polyphenol preservation rate was 46.44%, most of it was denatured and the activity decreased; the absorbance of the noni fruit enzyme sustained-release microcapsule powder decreased by 0.22 after 8 days, and the preservation rate was 77.67%. Microencapsulation significantly improved the atmospheric stability of noni fruit enzyme and significantly increased its activity.

[0112] Fig.15 is the cumulative release rate of the Noni enzyme sustained-release microcapsule powder obtained in step 5 of Example 1 in artificial gastric juice and artificial intestinal juice;

[0113] Depend on Fig.15It can be seen that during the simulated gastric digestion process (0min~120min), the release rate of polyphenols in the noni enzyme microcapsules showed a small burst release within 0min~20min, which may be mainly due to the migration of some enzymes from the inner water phase to the outer water phase during the freeze-drying process. Subsequently, during the process from 20min to 120min, the release rate of polyphenols in the noni enzyme microcapsules decreased, and the cumulative release rate tended to be flat, which was because the maltodextrin / arabic gum wall material had good acid resistance. During the entire simulated gastric digestion process, the polyphenols of the microencapsulated noni enzyme powder were released less, and the cumulative release rate only reached 31.01%. In the simulated intestinal environment digestion stage (120min~240min), the release rate of polyphenols in the noni enzyme powder increased, and then tended to be flat, and the cumulative release rate continued to increase, and the cumulative release rate was 73.77%, indicating that the microcapsule wall material structure can selectively release a large amount of sustained release in the intestinal environment, protecting the bioactive components in the noni enzyme that are sensitive to the gastric environment.

[0114] Comparative Example 1: A method for preparing noni enzyme powder, which is specifically completed by the following steps:

[0115] 1. Preparation of Noni Fruit Enzyme Puree:

[0116] ①, wash fresh and ripe noni fruit, drain the water, put it in a fermentation tank, seal the fermentation tank, put it in a cool place, and ferment it anaerobically at room temperature for 3 years to obtain fermented noni fruit pulp;

[0117] ②, subjecting the fermented noni fruit pulp to ultrasonic treatment for 90 minutes at a temperature of 38° C. and a frequency of 500 W to obtain ultrasonic noni fruit pulp;

[0118] ③. Filter under normal pressure to remove the coarse impurities in the ultrasonic noni fruit pulp, then centrifuge the filtrate at 4°C and 10,000 r / s for 10 minutes, collect the supernatant, and obtain the clarified noni fruit enzyme pulp;

[0119] 2. Preparation of wall material mixed solution: maltodextrin and gum arabic were placed in deionized water, the water bath temperature was controlled at 75°C, and magnetic stirring was performed for 10 minutes until they were completely dissolved to obtain a uniform mixed solution I; the mixed solution I was slowly cooled for 30 minutes to a final temperature of 45°C by program cooling to obtain a wall material mixed solution;

[0120] The concentration of maltodextrin in the mixed solution I described in step 2 is 0.012 g / mL, and the concentration of gum arabic is 0.024 g / mL;

[0121] 3. Preparation of Noni Fruit Enzyme Emulsion:

[0122] Add the wall material mixture into the Noni fruit enzyme slurry, keep the water bath temperature at 45°C, and stir for 60 minutes to obtain the Noni fruit enzyme emulsion;

[0123] The volume ratio of the wall material mixture described in step 3 to the Noni fruit enzyme puree is 1:10;

[0124] 4. Preparation of Noni Fruit Enzyme Microcapsules:

[0125] The noni fruit enzyme emulsion was pre-frozen at -20°C for 12 hours, and then vacuum freeze-dried for 48 hours to obtain the noni fruit enzyme powder.

[0126] The taste, smell and powder state of the Noni fruit enzyme sustained-release microcapsule powder prepared in Example 1 and the Noni fruit enzyme powder prepared in Comparative Example 1 are listed in Table 1;

[0127] Table 1

[0128] Taste odor Powder state Example 1 Acceptable sweet and sour taste Slight fragrance The powder has good fluidity and maintains good properties after long-term storage Comparative Example 1 Obvious sour feeling There is a distinct pungent odor The powder has poor fluidity and sticks together after being placed for a period of time

[0129] As can be seen from Table 1, compared with Comparative Example 1, Example 1 uses glucono-δ-lactone, which is a surfactant and has an enhanced emulsifying effect. After using glucono-δ-lactone, the irritating smell of the product powder is masked; Example 1 uses white sugar, and the sour and astringent taste of the product powder is significantly improved; Silicon dioxide is used in Example 1, and silicon dioxide is an anti-caking agent. After adding it, the flow stability of the product powder is enhanced.

[0130] Fig.16 The digital photos of the Noni fruit enzyme sustained-release microcapsule powder prepared in Example 1 and the Noni fruit enzyme powder prepared in Comparative Example 1, wherein 0 is the Noni fruit enzyme powder prepared in Comparative Example 1, and 1 is the Noni fruit enzyme sustained-release microcapsule powder prepared in Example 1;

[0131] from Fig.16 It can be seen that the appearance of the Noni fruit enzyme sustained-release microcapsule powder prepared in Example 1 is significantly improved. Compared with the Noni fruit enzyme powder prepared in Comparative Example 1, the powder is finer and has no lumps, and has better sensory properties.

Claims

1. A method for preparing a noni enzyme sustained-release microcapsule powder, characterized in that It uses noni fruit enzyme as the core material, maltodextrin and gum arabic as the wall material, forms noni fruit enzyme microcapsule emulsion at a mild temperature, and obtains noni fruit enzyme sustained-release microcapsule powder by vacuum freeze-drying. The preparation method is specifically completed in the following steps:

1. Preparation of concentrated Noni enzyme puree: ①, wash fresh and ripe noni fruit, drain the water, put it in a fermentation tank, seal the fermentation tank, put it in a cool place, and ferment it anaerobically at room temperature for 1 to 3 years to obtain fermented noni fruit pulp; ②, subjecting the fermented noni fruit pulp to ultrasonic treatment to obtain ultrasonic noni fruit pulp; ③. Filter and remove the coarse impurities in the ultrasonic noni fruit pulp under normal pressure, then centrifuge the filtrate at low temperature, collect the supernatant, and obtain the clarified noni fruit enzyme pulp; ④. Under the condition of 35℃~50℃, concentrate the clarified Noni fruit enzyme puree to 1 / 3~1 / 5 of the original volume to obtain concentrated Noni fruit enzyme puree; 2. Preparing a wall material mixed solution: placing maltodextrin and gum arabic in deionized water, controlling the water bath temperature to 65°C-85°C, and stirring with a magnetic force until they are completely dissolved to obtain a uniform mixed solution I; cooling the mixed solution I to a final temperature of 45°C by program cooling to obtain a wall material mixed solution; The concentration of maltodextrin in the mixed solution I described in step 2 is 0.01 g / mL to 0.04 g / mL, and the concentration of gum arabic is 0.02 g / mL to 0.04 g / mL; 3. Preparation of Noni Fruit Enzyme Emulsion: Add the wall material mixture and glucono-δ-lactone into the Noni fruit enzyme stock, keep the water bath temperature at 45°C to 55°C, stir and react to obtain the Noni fruit enzyme emulsion; The volume ratio of the wall material mixture described in step 3 to the Noni fruit enzyme puree is 1:10; the mass ratio of glucono-δ-lactone to the Noni fruit enzyme puree is 1.5:100; 4. Freeze-drying: The noni fruit enzyme emulsion is pre-frozen at -20°C, then vacuum freeze-dried, and finally ground to obtain a primary freeze-dried product; 5. Secondary freeze drying: The primary freeze-dried product, white sugar powder and silicon dioxide are mixed evenly to obtain a composite powder; the composite powder is pre-frozen at -20°C, vacuum freeze-dried, and finally ground to obtain the noni fruit enzyme sustained-release microcapsule powder.

2. The method for preparing a Noni enzyme sustained-release microcapsule powder according to claim 1, characterized in that In step 1②, the fermented noni fruit pulp is ultrasonically treated for 60min~120min at a temperature of 30℃~40℃ and a frequency of 500W~1000W.

3. The method for preparing a Noni enzyme sustained-release microcapsule powder according to claim 1, characterized in that In step 2, the mixed solution I is cooled to a final temperature of 45° C. by programmed cooling for 30 minutes.

4. The method for preparing a Noni enzyme sustained-release microcapsule powder according to claim 1, characterized in that The stirring reaction time in step 3 is 30 min to 90 min.

5. The method for preparing a Noni enzyme sustained-release microcapsule powder according to claim 1, characterized in that In step 4, the noni fruit enzyme emulsion is pre-frozen at -20°C for 8h~12h, then vacuum freeze-dried for 24h~48h, and finally ground for 0.1h~0.3h to obtain a primary freeze-dried product.

6. The method for preparing the Noni fruit enzyme sustained-release microcapsule powder according to claim 1, characterized in that In step 5, the mass ratio of the primary freeze-dried product, white sugar powder and silicon dioxide is 30:40:1; in step 5, the composite powder is pre-frozen at -20°C for 8h~12h, then vacuum freeze-dried for 24h~48h, and finally ground for 0.1h~0.3h to obtain noni fruit enzyme sustained-release microcapsule powder.

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