FDP cyclic adenosine monophosphate compound oral liquid and production process thereof

Abstract

The invention relates to the technical field of nutritional health-care drinks, in particular to FDP cyclic adenosine monophosphate compound oral liquid and a production process thereof. The invention relates to an FDP cyclic adenosine monophosphate compound oral liquid, which is prepared from the following raw materials by mass: 8 g of water, 2 g of a red date extract, 0.15 g of 1, 6-fructose diphosphate trisodium salt, 0.1 g of deer myocardial peptide powder, 0.1 g of anhydrous citric acid, 0.004 g of potassium sorbate, 0.00003 g of vitamin B1, 0.00003 g of vitamin B2, and 0.00003 g of vitamin B6. The production process of the FDP cyclic adenosine monophosphate compound oral liquid comprises the following steps: dynamic enzymolysis; coupling processing; carrying out nanometer stabilization; and filling at low temperature. According to the FDP cyclic adenosine monophosphate compound oral liquid and the production process thereof, the industrialization process of the compound myocardial protection oral liquid is improved, and the clinical application value of the compound myocardial protection oral liquid is increased.

Description

Technical Field

[0001] The present invention relates to the technical field of nutritional and health care beverages, and particularly to an FDP cyclic adenosine monophosphate compound drink oral liquid and its production process. Background Art

[0002] The high incidence of cardiovascular diseases and the irreversibility of myocardial injury have made the development of nutritional preparations with myocardial protection functions a research hotspot in the interdisciplinary field of modern medicine and food science. Based on the intervention strategy of regulating myocardial cell energy metabolism, the synergistic application of fructose diphosphate (FDP) and bioactive peptides shows unique advantages. Among them, FDP improves cell energy supply by promoting glycolysis, while myocardial peptides can directly participate in cell repair and antioxidant processes. Currently, the oral liquid dosage form occupies an important position in the development of functional beverages due to its fast absorption and strong compliance characteristics. However, how to achieve the efficient delivery and stable coexistence of active ingredients remains the key direction for technological breakthroughs.

[0003] In the prior art, oral liquid-based myocardial protection products often face multiple technical bottlenecks during the preparation process: First, the directional cutting efficiency of traditional enzymatic hydrolysis process for bioactive peptides is insufficient, prone to generating ineffective fragments and having the risk of enzyme residues; Second, the physical mixing of FDP and peptide substances is difficult to achieve stable binding at the molecular level, resulting in the dissociation and inactivation of components in the gastrointestinal environment; Third, nano-scale active ingredients in the liquid system are prone to aggregation and sedimentation, and conventional dispersion techniques cannot maintain the long-term uniformity of the system. In addition, heat-sensitive ingredients are easily affected by temperature fluctuations during filling and storage, causing the degradation of active ingredients, directly affecting the shelf-life stability and clinical effectiveness of the product. Summary of the Invention

[0004] The present invention provides an FDP cyclic adenosine monophosphate compound drink oral liquid and its production process, which improves the industrialization process and clinical application value of the compound myocardial protection oral liquid.

[0005] The technical solution adopted by the present invention is as follows: An FDP cyclic adenosine monophosphate compound drink oral liquid is made from the following raw materials in mass ratio: water accounts for 8 grams, red date extract accounts for 2 grams, trisodium 1,6-diphosphate fructose accounts for 0.15 grams, deer myocardial peptide powder accounts for 0.1 grams, anhydrous citric acid accounts for 0.1 grams, potassium sorbate accounts for 0.004 grams, vitamin B1 accounts for 0.00003 grams, vitamin B2 accounts for 0.00003 grams, and vitamin B6 accounts for 0.00003 grams.

[0006] A production process of an FDP cyclic adenosine monophosphate compound drink oral liquid includes the following steps:

[0007] S1, Dynamic enzymatic hydrolysis: Mix deer myocardial peptide powder with an immobilized papain-neutral protease complex enzyme system, and perform enzymatic hydrolysis for 10 - 14 hours under the conditions of pH 6.8 - 7.2 and 6 - 8°C. After enzymatic hydrolysis, inactivate it instantaneously by microwave (power 500 - 800W, time 10 - 20 seconds);

[0008] S2, Coupling treatment: Mix the enzymatic hydrolysis product with a pretreated trisodium 1,6-diphosphate solution, control the mixing rate, temperature and ultrasonic frequency, and protect with nitrogen throughout the process;

[0009] S3, Nano-steady state: Homogenize the mixture by high-pressure microfluidization (pressure 180 - 220 MPa, cycle 5 - 7 times), and add a nanoscale silica dispersant (0.001 - 0.003 grams);

[0010] S4, Low-temperature filling: Fill the final product into light-proof ampoules under nitrogen at -5°C to 0°C, and store at a temperature ≤ 4°C.

[0011] As a further improvement of the present invention, in the step S1, the enzyme activity ratio of the immobilized papain-neutral protease complex enzyme system is 1:1.5 - 2.0, the total enzyme activity is 10000 - 15000 U / g, and the addition amount is 1.2 - 1.8% of the mass of the deer myocardial peptide powder.

[0012] As a further improvement of the present invention, in the step S2, the mixing rate is 150 - 300 rpm, the temperature is 4 - 8°C, the ultrasonic frequency is 30 kHz, and the time is 80 - 120 minutes.

[0013] As a further improvement of the present invention, the nanoscale silica dispersant added in the step S3 is surface-modified, and the modifier is a polyethylene glycol-phospholipid complex (PEG2000-DSPE), and the modification ratio is 1:0.2 - 0.5 (w / w).

[0014] As a further improvement of the present invention, after microwave inactivation in the step S1, low-temperature centrifugal purification is added: Centrifuge at 4°C and 8000 - 10000 rpm for 15 minutes, collect the supernatant and filter it through a 0.1μm ceramic membrane.

[0015] As a further improvement of the present invention, the vitamin B complex component is added through an atomization spraying system in the third stage of the step S2, the atomization particle size is 5 - 10μm, the spraying rate is 0.3 - 0.6 mL / min, and after spraying, it is left to adsorb for 10 minutes.

[0016] As a further improvement of the present invention, the filling process in the step S4 adopts a two-step precooling method: First, cool the mixture at 2°C / min to -15°C and hold for 30 minutes, then heat it at 1°C / min to -5°C and then perform sub-packaging. After filling, seal it immediately and attach a moisture-proof film.

[0017] Advantages of the present invention: The present invention realizes the high-activity retention of cardiotrophin through the combination of immobilized double-enzyme directional enzymatic hydrolysis and microwave-centrifugation purification technology, constructs a molecular-level stable complex by combining ultrasonic coupling and PEG-DSPE modified nano-dispersion system, and cooperates with a two-step pre-cooling filling process and an atomization precise addition process, so that FDP and cardiotrophin maintain the targeted release characteristics in gastrointestinal fluid, the bioavailability of vitamin B group is increased by 2.1 times, and the retention rate of active ingredients is ≥96% after 6 months of storage at room temperature in the liquid system, realizing the spatio-temporal synergistic expression of triple effects of enhanced energy metabolism, antioxidant and cell repair. Specific embodiments

[0018] In order to make the technical problems, technical solutions and beneficial effects to be solved by the present application clearer, the present application will be further described in detail below with reference to embodiments. It should be understood that the embodiments described herein are only used to explain the present application and are not used to limit the present application.

[0019] The present invention provides an FDP cyclic adenosine monophosphate compound drink oral liquid, which is made from raw materials with the following mass ratios: water accounts for 8 grams, red date extract accounts for 2 grams, trisodium 1,6-diphosphate fructose accounts for 0.15 grams, deer cardiotrophin powder accounts for 0.1 gram, anhydrous citric acid accounts for 0.1 gram, potassium sorbate accounts for 0.004 gram, vitamin B1 accounts for 0.00003 gram, vitamin B2 accounts for 0.00003 gram, and vitamin B6 accounts for 0.00003 gram.

[0020] A production process of an FDP cyclic adenosine monophosphate compound drink oral liquid includes the following steps: [[ID=I5]]

[0021] S1, Dynamic enzymatic hydrolysis: Mix deer cardiotrophin powder with an immobilized papain-neutral protease complex enzyme system, and perform enzymatic hydrolysis at pH 6.8 - 7.2 and 6 - 8 °C for 10 - 14 hours. After enzymatic hydrolysis, inactivate it instantaneously with microwave (power 500 - 800W, time 10 - 20 seconds);

[0022] S2, Coupling treatment: Mix the enzymatic hydrolysis product with a pretreated trisodium 1,6-diphosphate fructose solution, control the mixing rate, temperature and ultrasonic frequency, and protect with nitrogen throughout the process;

[0023] S3, Nano-steady state: Homogenize the mixture by high-pressure microfluidization (pressure 180 - 220 MPa, cycle 5 - 7 times), and add a nano-level silica dispersant (0.001 - 0.003 grams);

[0024] S4, Low-temperature filling: Fill the final product into light-proof ampoules under the condition of -5 °C to 0 °C with nitrogen filling, and the storage temperature ≤ 4 °C.

[0025] In step S1 of the present invention, the enzyme activity ratio of the immobilized papain-neutral protease complex enzyme system is 1:1.5 - 2.0, the total enzyme activity is 10,000 - 15,000 U / g, and the addition amount is 1.2 - 1.8% of the mass of deer myocardial peptide powder.

[0026] In step S2 of the present invention, the mixing rate is 150 - 300 rpm, the temperature is 4 - 8 °C, the ultrasonic frequency is 30 kHz, and the time is 80 - 120 minutes.

[0027] In step S3 of the present invention, the added nano-silica dispersant is surface-modified, and the modifier is polyethylene glycol-phospholipid complex (PEG2000-DSPE), and the modification ratio is 1:0.2 - 0.5 (w / w).

[0028] In step S1 of the present invention, low-temperature centrifugation purification is added after microwave inactivation: centrifuge at 4 °C and 8000 - 10,000 rpm for 15 minutes, collect the supernatant and filter it through a 0.1 μm ceramic membrane.

[0029] In the present invention, the vitamin B component is added through an atomization spraying system in the third stage of step S2, the atomization particle size is 5 - 10 μm, the spraying rate is 0.3 - 0.6 mL / min, and after spraying, it is left to adsorb for 10 minutes.

[0030] The filling process of step S4 of the present invention adopts a two-step precooling method: first cool the mixed solution at 2 °C / min to -15 °C and hold for 30 minutes, then warm it up to -5 °C at 1 °C / min and then carry out sub-packaging. After filling, it is immediately sealed and covered with a moisture-proof film.

[0031] Example:

[0032] Weigh 10 grams of deer myocardial peptide powder, mix it with the immobilized papain-neutral protease complex enzyme system (enzyme activity ratio 1:1.8, total enzyme activity 12,000 U / g) according to a mass ratio of 1.5%, add phosphate buffer solution with pH 7.0, and carry out enzymatic hydrolysis at a constant temperature of 6 °C for 12 hours. After the enzymatic hydrolysis is completed, use microwave instantaneous inactivation (power 650 W, time 15 seconds), then centrifuge at 4 °C and 9000 rpm for 15 minutes, collect the supernatant and filter it through a 0.1 μm ceramic membrane to obtain a clear enzymatic hydrolysate (peptide content ≥ 85%, enzyme residue < 0.05 U / mL).

[0033] Dissolve 15 grams of pre-treated fructose 1,6-diphosphate trisodium salt in deionized water, and transfer it to an ultrasonic coupling reaction tank (nitrogen environment, oxygen content < 0.5%) together with the enzymatic hydrolysate. Control the mixing rate at 200 rpm and the temperature at 6 °C, and start ultrasonic treatment at 30 kHz for 100 minutes to form a homogeneous composite solution. Subsequently, accurately add the vitamin B complex solution (containing 0.003 grams of B1, 0.003 grams of B2, and 0.003 grams of B6) through an atomization spraying system (atomization particle size 8 ± 2 μm, spraying rate 0.45 mL / min). After standing and adsorbing for 10 minutes, the particle size distribution of the composite solution is detected to be 200 - 500 nm.

[0034] Process the mixed solution through a high-pressure microfluidic homogenizer (pressure 200 MPa, 6 cycles), and simultaneously add a nano-silica dispersant modified with PEG2000-DSPE (addition amount 0.002 grams, modification ratio 1:0.35). Transmission electron microscopy of the treated system shows that the active ingredient is embedded in the silica network in a core-shell structure, the average particle size is reduced to 80 - 150 nm, and the Zeta potential is -28.5 mV.

[0035] Use a two-step precooling method for filling: First, cool the final product at 2 °C / min to -15 °C and hold for 30 minutes to form a microcrystalline protective layer; then heat it at 1 °C / min to -5 °C, and immediately fill it with nitrogen into amber ampoules (10 mL per single ampoule). After sealing, attach a composite moisture-proof film (water vapor transmission rate < 0.01 g / m 2 ·24h).

[0036] Test results

[0037] (1) Activity retention rate: HPLC detection shows that the FDP retention rate is 98.3% and the myocardial peptide activity retention rate is 97.6% (compared with the raw materials);

[0038] (2) Gastrointestinal release characteristics: The release rate in simulated gastric juice is 8.7% in 2 hours, and the cumulative release rate in intestinal juice is 93.5% in 4 hours (ultraviolet spectrophotometry);

[0039] (3) Stability: After 6 months of accelerated testing at 40 °C, the particle size growth ≤ 10%, and there is no visible precipitation (laser particle size analyzer);

[0040] (4) Function verification: In vitro cardiomyocyte experiments show that the ATP synthesis amount is increased by 2.9 times, and the LDH leakage amount is reduced by 67% (compared with the control group).

[0041] As can be seen from the above embodiments, through a unique production process, the present invention has successfully overcome many technical bottlenecks of oral liquid-based myocardial protection products in the prior art, and achieved the efficient delivery and stable coexistence of the active ingredients of the FDP cyclic adenosine monophosphate compound drink oral liquid. This oral liquid not only performs excellently in terms of the retention rate of active ingredients, gastrointestinal release characteristics, and stability, but also shows a significant effect of enhancing myocardial cell energy metabolism and protecting cells in functional verification, providing a reliable and effective product choice for the nutritional intervention of cardiovascular diseases, and is expected to promote the further development and application of myocardial protection nutritional health drinks.

[0042] In summary, the FDP cyclic adenosine monophosphate compound drink oral liquid of the present invention and its production process are innovative and practical in addressing the technical challenges of nutritional health drinks related to cardiovascular diseases. By precisely controlling the parameters of each production step, from enzymatic hydrolysis, coupling to nano-steady state and low-temperature filling, the synergistic stability and efficient utilization of multiple active ingredients are achieved. Its precise setting of the raw material mass ratio, combined with a series of advanced treatment processes, ensures the excellent performance of the product in enhancing myocardial protection function. This innovative process not only provides a feasible solution for enterprises to produce high-quality myocardial protection oral liquids, but also provides consumers with a better, more reliable product in terms of nutritional choices for cardiovascular health maintenance, and is of great significance for promoting the technological upgrading and product optimization of the entire nutritional health drink industry in the field of myocardial protection.

[0043] The above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that they can still modify the technical solutions described in the foregoing embodiments, or perform equivalent replacements for some of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A kind of FDP cyclic adenosine monophosphate compound drink oral liquid, characterized in that, It is made from the following raw materials with the following mass ratios: water accounts for 8 grams, red date extract accounts for 2 grams, trisodium 1,6-diphosphate fructose accounts for 0.15 grams, deer cardiac myopeptide powder accounts for 0.1 gram, anhydrous citric acid accounts for 0.1 gram, potassium sorbate accounts for 0.004 gram, vitamin B1 accounts for 0.00003 gram, vitamin B2 accounts for 0.00003 gram, and vitamin B6 accounts for 0.00003 gram.

2. The production process of an FDP cyclic adenosine monophosphate compound drink oral liquid is characterized in that, It includes the following steps: S1, Dynamic enzymatic hydrolysis: Mix deer cardiac myopeptide powder with an immobilized papain-neutral protease complex enzyme system, and perform enzymatic hydrolysis at pH 6.8 - 7.2 and 6 - 8 °C for 10 - 14 hours. After enzymatic hydrolysis, inactivate it instantaneously by microwave (power 500 - 800 W, time 10 - 20 seconds); S2, Coupling treatment: Mix the enzymatic hydrolysis product with a pretreated trisodium 1,6-diphosphate fructose solution, control the mixing rate, temperature, and ultrasonic frequency, and protect with nitrogen throughout the process; S3, Nano-steady state formation: Subject the mixed solution to high-pressure microfluidic homogenization treatment (pressure 180 - 220 MPa, cycle 5 - 7 times), and add a nano-scale silica dispersant (0.001 - 0.003 grams); S4, Low-temperature filling: Fill the final product into light-proof ampoules under nitrogen filling at -5 °C to 0 °C, and the storage temperature ≤ 4 °C.

3. The production process of an FDP cyclic adenosine monophosphate compound drink oral liquid according to claim 2, characterized in that, In the step S1, the enzyme activity ratio of the immobilized papain-neutral protease complex enzyme system is 1:1.5 - 2.0, the total enzyme activity is 10000 - 15000 U / g, and the addition amount is 1.2 - 1.8% of the mass of deer cardiac myopeptide powder.

4. The production process of an FDP cyclic adenosine monophosphate composite drink oral liquid according to claim 2, characterized in that, In the step S2, the mixing rate is 150 - 300 rpm, the temperature is 4 - 8 °C, the ultrasonic frequency is 30 kHz, and the time is 80 - 120 minutes.

5. The production process of an FDP cyclic adenosine monophosphate compound drink oral liquid according to claim 2, characterized in that, The nano-scale silica dispersant added in the step S3 is surface-modified, and the modifier is polyethylene glycol-phospholipid complex (PEG2000-DSPE), and the modification ratio is 1:0.2 - 0.5 (w / w).

6. The production process of an FDP cyclic adenosine monophosphate composite drink oral liquid according to claim 2, characterized in that, After microwave inactivation in the step S1, add low-temperature centrifugation purification: Centrifuge at 4 °C and 8000 - 10000 rpm for 15 minutes, collect the supernatant and filter it through a 0.1 μm ceramic membrane.

7. The production process of an FDP cyclic adenosine monophosphate compound drink oral liquid according to claim 2, characterized in that, The vitamin B complex components are added through an atomization spraying system in the third stage of the step S2, the atomization particle size is 5 - 10 μm, the spraying rate is 0.3 - 0.6 mL / min, and after spraying, let it stand and adsorb for 10 minutes.

8. The production process of an FDP adenosine cyclic phosphate composite drink oral liquid according to claim 2, characterized in that, The filling process in the step S4 adopts a two-step pre-cooling method: First, cool the mixed solution at 2 °C / min to -15 °C and hold for 30 minutes, then heat it up to -5 °C at 1 °C / min and then perform sub-packaging. After filling, seal it immediately and attach a moisture-proof film.