Preparation method of a cornus officinalis drink

Abstract

The application discloses a preparation method of a cornus officinalis drink and belongs to the technical field of food processing. The method comprises the following steps: selecting and grading materials; performing multi-stage extraction with gradient temperature change in steps, i.e., extracting in steps at 50-60 DEG C, 65-75 DEG C and 80-90 DEG C, and supplementing with intermittent ultrasonic waves; performing compound enzymolysis and clarification, i.e., performing joint enzymolysis of pectinase and cellulase and then performing membrane filtration; performing multi-component compounding and blending, i.e., compounding the cornus officinalis extract with the extract of medlar, hawthorn and red dates, and adding a compound sweetening agent to adjust the flavor; performing homogenization and degassing; and performing ultra-high temperature instant sterilization and aseptic filling. The method considers the dissolution characteristics of different active ingredients by gradient temperature change extraction, completely solves the problem of post-haze by enzymolysis and clarification, improves the taste by scientific compounding, and retains active ingredients by UHT sterilization. The obtained drink has a total content of loganin and morroniside of greater than or equal to 1.20 g / L, is clear and stable, has a long shelf life, and is suitable for industrial production.

Description

Technical Field

[0001] This invention relates to the field of food processing technology, and in particular to a method for preparing a Cornus officinalis beverage, especially a method for preparing a Cornus officinalis beverage using a stepped gradient temperature-controlled multi-stage extraction combined with a complex enzymatic hydrolysis clarification process. This invention fully utilizes the medicinal and edible properties of Cornus officinalis to prepare a Cornus officinalis beverage with high retention of active ingredients, harmonious taste, stable clarification, and long shelf life, suitable for large-scale industrial production. Background Technology

[0002] Cornus officinalis (Cornus officinalis Sieb. et Zucc.) is the mature fruit of a deciduous small tree in the Cornaceae family, and it has a long history of medicinal and edible use in my country. Li Shizhen, in his *Compendium of Materia Medica* during the Ming Dynasty, recorded that Cornus officinalis "is a fruit that nourishes the liver and kidneys, its taste is sour and its nature warm, astringent and constricting, thus it has the functions of tonifying the liver, astringing the kidneys, treating coughs, and stopping bleeding." In November 2023, the National Health Commission and the State Administration for Market Regulation issued Announcement No. 9 of 2023, officially including Cornus officinalis and nine other substances in the list of substances that are traditionally both food and medicinal materials (i.e., the list of substances with the same medicinal and edible properties), marking clear policy support for the application of Cornus officinalis in the food sector.

[0003] From a nutritional perspective, Cornus officinalis is rich in various vitamins, minerals, and active ingredients. Every 100g of Cornus officinalis pulp contains 10.2mg of vitamin C, as well as vitamins A and E, and minerals such as potassium (160mg), calcium (15mg), and phosphorus (20mg). Studies have shown that approximately 230 compounds have been isolated and identified from Cornus officinalis, among which iridoid glycosides are the most abundant active ingredients, with 103 identified. Loganin and mononoside are the two most representative compounds among the iridoid glycosides of Cornus officinalis; modern pharmacological studies have shown that they have good medicinal value in neuroprotection, treatment of diabetes and kidney disease, and inhibition of inflammatory responses and apoptosis. The polysaccharide content of Cornus officinalis can reach 7.85%~16.83%, possessing anti-aging and immune-enhancing effects. Triterpenoid components, including ursolic acid, oleanolic acid, and betulinic acid, have anti-inflammatory, antioxidant, antiviral, and immunomodulatory effects. Thirty-one flavonoids have been isolated from Cornus officinalis, with a yield of up to 2.76%, and are an important source of its antioxidant capacity. Organic acids, including 17 compounds such as citric acid, succinic acid, and malic acid, are among the key active ingredients that contribute to Cornus officinalis's anti-inflammatory and antioxidant effects.

[0004] Based on the rich nutritional value and health benefits of Cornus officinalis, the development of food and beverage products using it as a raw material has received increasing attention in recent years. Engineer Zhang Lipan's team systematically analyzed the nutritional components of Cornus officinalis fruit, discovering that it is rich in protein, polysaccharides, various vitamins, 16 amino acids, and minerals such as potassium, magnesium, calcium, and iron, offering comprehensive nutrition. They have successfully developed various products including Cornus officinalis jam, solid beverages, baked goods, and formulated wines. In the market, Jiecui Biotechnology launched Yushengning™ instant Cornus officinalis powder, which has gained significant attention in the food and beverage industry due to its patented cold-dissolving process. These market dynamics indicate that Cornus officinalis food products have excellent market prospects and industrialization potential.

[0005] However, a systematic search and analysis of existing technologies revealed that current methods for preparing Cornus officinalis beverages and similar products still have many shortcomings, mainly in the following aspects:

[0006] The extraction efficiency of active ingredients is low, and significant losses are observed. Traditional Cornus officinalis beverages mostly employ water extraction or hot water extraction processes at a single temperature. For example, CN93118132.1 discloses a method for producing Cornus officinalis juice and its beverage. Using Cornus officinalis fruit as raw material, the juice is prepared through processes such as washing, crushing, filtering and pitting, adding gum, dissolving enzymes, fine filtration, sterilization, and concentration. This juice is then blended, filtered, and sterilized to produce a beverage. While this method achieves the production of Cornus officinalis beverages, it uses a traditional crushing and juicing process, which is insufficient for protecting heat-sensitive active ingredients. Other literature reports a process using 10 times the mass of Cornus officinalis water to soak the fruit for softening and pitting before juicing, as well as a traditional extraction process using 10 times the amount of water and three extractions (6 hours each for the first two extractions, and 4 hours for the last extraction). These traditional extraction methods all have significant technical drawbacks: On the one hand, single-temperature extraction cannot simultaneously account for the dissolution patterns of active ingredients with different polarities. Low temperatures are beneficial for the protection of heat-sensitive components (such as certain flavonoids and vitamins) but result in lower extraction efficiency, while high temperatures, although improving extraction efficiency, lead to the degradation of heat-sensitive components. On the other hand, prolonged high-temperature extraction (such as 6-hour immersion) causes significant oxidative and thermal degradation of active ingredients such as loganin and monoglycosides during the extraction process, resulting in the content of effective components in the product being far lower than the theoretical content of the raw material. In recent years, although advanced technologies such as enzymatic extraction, ultrasonic extraction, and microwave extraction have emerged, microwave, ultrasonic, and enzymatic methods can significantly shorten extraction time and improve the yield of effective components, with extraction effects superior to conventional reflux extraction. However, microwave methods are not suitable for the extraction of heat-sensitive substances, and ultrasonic extraction is easily affected by ultrasonic attenuation factors, forming an ultrasonic blank zone. CN121489059A discloses a method for preparing Cornus officinalis extract using a combined ultrasonic-microwave extraction and enzymatic hydrolysis process. Although the extraction efficiency is improved compared to traditional methods, this process is designed for the preparation of extracts in compressed candies. Directly applying it to the preparation of beverages presents a process mismatch problem, and microwave treatment may have an adverse effect on the flavor of the beverage.

[0007] The beverage exhibits poor clarification stability. Cornus officinalis fruit is rich in macromolecules such as pectin, cellulose, protein, and tannins, which are prone to aggregation and sedimentation or reaction with other components during beverage processing and storage, leading to quality problems such as turbidity, sedimentation, and layering. Traditional methods often employ single-ingredient gelatin clarification (0.35% added, left to stand at room temperature for 6 hours) or multiple processes involving gelatin addition, enzyme inoculation, and fine filtration. While these methods can improve clarity to some extent, the clarification effect is incomplete, time-consuming, and animal-derived clarifying agents like gelatin pose certain food safety risks and consumer acceptance issues. In particular, the tannic acid-protein complex formed when tannins in Cornus officinalis combine with proteins is a major cause of "post-turbidity" during beverage storage, a problem that current clarification methods fail to fundamentally solve.

[0008] The formula is too simple, resulting in poor flavor. Cornus officinalis itself has a strong sour and bitter taste, mainly due to the bitter characteristics of its tannins and iridoid glycosides such as loganin and monosodium glycosides. Traditional products often use only Cornus officinalis as a single ingredient or simply add sucrose to mask off-flavors, leading to a lack of flavor complexity and depth of taste. Although some existing technologies use β-cyclodextrin to mask bitterness (addition amount 0.05%), this method only provides physical masking and does not fundamentally improve the flavor harmony and complexity of the beverage. Some patent documents disclose teas or fermented drinks made by combining Cornus officinalis with goji berries, red dates, etc., but these combinations are mostly aimed at synergistic health benefits rather than systematic optimization of flavor blending, lacking scientific consideration of the synergistic flavor effects between different excipients and Cornus officinalis.

[0009] Oxidative browning is a significant problem during processing. Cornus officinalis fruits are rich in polyphenol oxidase (PPO) and peroxidase (POD), as well as polyphenolic substrates. During processing such as crushing, juicing, and extraction, the cell structure is damaged, allowing the enzymes to come into contact with the substrates. Under aerobic conditions, this leads to a rapid enzymatic browning reaction, causing the product to darken and brown, severely impacting its appearance and consumer acceptance. Traditional processes often use boiling water for 15 minutes to deactivate the enzymes, but prolonged high-temperature blanching results in the loss of heat-sensitive active ingredients and flavor deterioration. How to effectively control browning while maximizing the preservation of active ingredients and natural flavor is a pressing technical challenge in the processing of Cornus officinalis beverages.

[0010] The sterilization process has a significant impact on product quality. Traditional Cornus officinalis beverages are mostly sterilized at atmospheric pressure or at 100°C for 300 seconds after bottling. While prolonged heat sterilization can ensure microbial safety, it leads to thermal degradation of active ingredients, darkening of color, deterioration of flavor, and severe loss of nutrients. Some literature reports the use of sterilization at 120°C for 20 seconds, but this temperature is still not ideal for protecting heat-sensitive active ingredients.

[0011] There is a lack of systematic, end-to-end process solutions suitable for continuous industrial production. Most existing technologies optimize specific steps in the processing of Cornus officinalis, lacking a complete process system encompassing raw material pretreatment, extraction, clarification, blending, homogenization, degassing, sterilization, and filling. The lack of effective coordination and parameter matching between process steps leads to large batch-to-batch fluctuations in product quality, poor stability, and low production efficiency in industrial production.

[0012] Furthermore, further research indicates that the extraction efficiency of Cornus officinalis active ingredients is not simply linearly positively correlated with extraction temperature, but rather exhibits a component-specific nonlinear relationship. Through extensive experimental research, the inventors of this application discovered that the optimal extraction temperature range for heat-sensitive flavonoids is 45-60℃; exceeding this range results in significant thermal degradation. The optimal extraction temperature range for iridoid glycosides (loganin and monoglycoside) is 65-75℃, with the extraction rate positively correlated with temperature within this range. However, above 80℃, loganin yield drops sharply due to ring-opening degradation. Polysaccharides require high temperatures of 80-90℃ for sufficient swelling and dissolution, but prolonged extraction under a single high-temperature condition leads to irreversible loss of the aforementioned heat-sensitive components. This "component-specific temperature response difference" constitutes a fundamental technical contradiction in the processing of Cornus officinalis beverages; extraction at a single temperature cannot simultaneously meet the optimal dissolution conditions for different active ingredients. The existing technologies, whether it is the single-temperature softening at 80℃ in D1, the hot scalding at 92-95℃ in D2, or the multiple extractions at the same temperature in D3, have not fundamentally solved this technical contradiction.

[0013] Furthermore, the inventors of this application discovered through research that during the clarification process, there is a structural interweaving and encapsulation relationship between pectin and cellulose in the Cornus officinalis extract. The pectin-cellulose complex matrix encapsulates the tannin-protein complex within it. Although a single pectinase can degrade pectin, the presence of the cellulose network framework prevents the enzymatic hydrolysis from fully penetrating into the matrix, resulting in incomplete clarification. This is the fundamental reason for the recurrence of turbidity after storage using the traditional single pectinase clarification method.

[0014] Furthermore, regarding flavor blending, the inventors of this application discovered through systematic sensory evaluation and electronic tongue analysis that the astringent taste of Cornus officinalis mainly originates from the synergistic effect of tannins (astringency) and iridoid glycosides (bitterness), and there is a synergistic deterioration effect between the two in terms of sensory perception; the presence of astringency significantly amplifies the perceived intensity of bitterness. Traditional β-cyclodextrin encapsulation methods only mask some small-molecule bitter substances and have almost no effect on improving the astringency of high-molecular-weight tannins.

[0015] In summary, there is currently no comprehensive method for preparing Cornus officinalis beverages that can simultaneously solve the six major technical problems mentioned above. Therefore, developing a method for preparing Cornus officinalis beverages that features high extraction rate of active ingredients, sufficient retention of effective components, good clarification stability, harmonious and palatable flavor, natural color, long shelf life, and suitability for continuous industrial production has significant technical value and market implications. Summary of the Invention

[0016] To address the shortcomings of existing technologies, the present invention aims to provide a method for preparing Cornus officinalis beverages. This method efficiently extracts and retains various active ingredients from Cornus officinalis, including loganin, monoglycosides, polysaccharides, flavonoids, and organic acids, ensuring that the total content of loganin and monoglycosides in the product is not less than 1.20 g / L and the total polysaccharide content is not less than 0.80 g / L. Through scientific multi-component formulation, the flavor harmony and palatability of the product are significantly improved. A reasonable combination of process parameters effectively solves the problems of clarification stability and oxidative browning during processing. An optimized sterilization process maximizes the retention of active ingredients and natural flavor while ensuring microbial safety, extending the product's shelf life. Furthermore, this method features a complete process route, simple operation, and suitability for continuous industrial production, providing reliable technical support for the deep processing and high-value utilization of Cornus officinalis in the beverage industry.

[0017] The above-mentioned objective of this invention is achieved through the following technical solutions:

[0018] A method for preparing a Cornus officinalis beverage includes the following steps:

[0019] Step S1, Selection and Grading: Select fresh Cornus officinalis fruits with a maturity of ≥90%, free from mold, rot, and pests. Grade the fruits according to their size and color, wash them clean, drain the water, and obtain graded fresh fruits.

[0020] The maturity of Cornus officinalis fruit directly affects the content of active ingredients and the flavor quality of beverages. Underripe fruit has lower levels of loganin and monosodium glutamate and an excessively sour and astringent taste; overripe fruit is prone to softening, browning, and microbial contamination. This invention selects fresh fruit with a maturity of ≥90%, ensuring optimal levels of active ingredients in the raw materials while maintaining a moderate acidity. Grading the fruit by size and color ensures uniform mass and heat transfer during subsequent extraction processes, reducing batch-to-batch quality variations and providing a fundamental guarantee for standardization and consistency in industrial production.

[0021] Step S2, stepped gradient temperature-variable multi-stage extraction: The graded fresh fruit obtained in step S1 is added to the extraction solvent at a material-to-liquid mass ratio of 1:(8~15), and a stepped gradient temperature-variable extraction process is adopted, which sequentially goes through: the first temperature stage 50~60℃, extraction for 30~60 minutes; the second temperature stage 65~75℃, extraction for 20~40 minutes; the third temperature stage 80~90℃, extraction for 10~20 minutes; during the extraction process, intermittent ultrasonic treatment is used, with an ultrasonic frequency of 20~40kHz and an ultrasonic power density of 30~60W / L. Each ultrasonic treatment lasts for 2~5 minutes, with an interval of 5~10 minutes. After the extraction is completed, the extract and residue are separated by coarse filtration while hot, and the extract is collected.

[0022] Step S2 is one of the key technologies of this invention. The design concept of the stepped gradient temperature-varying multi-stage extraction process of this invention is based on the following scientific understanding: Cornus officinalis contains a diverse range of active ingredients with significantly different physicochemical properties. Iridoid glycosides (such as loganin and monoglycoside) are moderately polar compounds with good solubility in warm water, but are sensitive to high temperatures; prolonged high-temperature treatment will lead to their ring-opening degradation. Flavonoid glycosides are highly polar and can be effectively dissolved at medium to low temperatures. Polysaccharides require higher temperatures to fully swell and dissolve. Triterpenoids (such as ursolic acid) are less polar and have a higher dissolution rate at higher temperatures or in alcohol-water systems. Organic acids can be rapidly dissolved at medium to low temperatures. Traditional single-temperature extraction cannot simultaneously meet the optimal dissolution conditions for active ingredients with different properties.

[0023] This invention creatively proposes a "stepped gradient temperature-controlled multi-stage extraction" strategy, which uses a gradient progression of three temperature ranges to allow active ingredients with different properties to dissolve sequentially within their respective optimal temperature ranges.

[0024] The first temperature range (50-60℃, 30-60 minutes) is the "mild initiation" stage. Under these relatively mild temperature conditions, heat-sensitive components such as vitamin C, some flavonoid glycosides, and some organic acids preferentially dissolve, while avoiding the destruction of these heat-sensitive components by high temperatures. The low-temperature mild initiation also gradually softens and loosens the cell walls of the Cornus officinalis pulp, creating favorable mass transfer conditions for the subsequent dissolution of other components at higher temperatures.

[0025] The second temperature range (65~75℃, 20~40 minutes) is the "main dissolution period." Within this temperature range, the solubility and diffusion rate of iridoid glycosides (loganin and monoglycoside) are significantly increased, representing the optimal dissolution window for these main active ingredients. Simultaneously, this temperature range falls within the thermal stability range of loganin and monoglycoside, preventing significant thermal degradation.

[0026] The third temperature range (80-90℃, 10-20 minutes) is the "deep extraction period." Under these higher temperatures, polysaccharides swell fully and dissolve more rapidly, and the dissolution rate of triterpenoids is also significantly increased. Although the temperature is high, the extraction time is short (10-20 minutes), and the main heat-sensitive components have already dissolved in the earlier stages, so the overall retention rate of active ingredients is minimally affected. Simultaneously, the appropriate high temperature also provides some sterilization and enzyme inactivation, which is beneficial to the stability of subsequent processes.

[0027] This gradient extraction mode realizes the extraction strategy of "classifying and batching, and taking advantage of each", which allows active ingredients of different properties to be dissolved in their most suitable temperature range. The overall extraction rate of active ingredients is 20% to 35% higher than that of traditional single-temperature extraction, and the proportions between the components are more balanced and coordinated.

[0028] Intermittent ultrasonic treatment during the extraction process is another important innovation of this invention. While traditional continuous ultrasonic treatment can effectively promote cell wall disruption and mass transfer, the attenuation effect of ultrasound in liquid media creates ultrasonic blank areas at the container edges and in the far-field region, leading to uneven extraction. Furthermore, continuous, prolonged ultrasound generates a thermal effect, causing localized increases in the liquid temperature, which may degrade heat-sensitive components. This invention employs intermittent ultrasonic treatment, with each ultrasonic session lasting 2-5 minutes and intermittent intervals of 5-10 minutes. This not only effectively avoids the blank areas caused by ultrasound attenuation and ensures uniform distribution of ultrasonic energy in the liquid, but also allows the extraction system to naturally restore temperature equilibrium during the intervals, preventing localized overheating. The cavitation and mechanical effects of ultrasound effectively disrupt the cell wall structure of Cornus officinalis pulp, promoting the release of intracellular active ingredients, significantly shortening extraction time, and improving extraction efficiency.

[0029] Furthermore, in this step, the material-to-liquid mass ratio is controlled within the range of 1:(8~15) (preferably 1:(10~12)). This ensures sufficient solvent volume for the full dissolution of active ingredients while avoiding increased energy consumption and costs in subsequent concentration due to excessive solvent. An excessively dilute extract will significantly increase the load and energy costs of subsequent concentration; an excessively concentrated extract will result in incomplete dissolution of active ingredients and a low extraction rate. The material-to-liquid ratio determined in this invention is the optimal balance point between extraction efficiency and process economy, obtained based on system experimental optimization.

[0030] Step S3, compound enzymatic hydrolysis clarification: Add a compound enzyme preparation to the extract obtained in step S2. The compound enzyme preparation contains pectinase and cellulase. The amount of pectinase added is 0.01%~0.05% of the extract volume, and the amount of cellulase added is 0.005%~0.02% of the extract volume. The enzymatic hydrolysis temperature is 45~55℃, and the enzymatic hydrolysis time is 60~120 minutes. After the enzymatic hydrolysis is completed, raise the temperature to 90~95℃ to inactivate the enzyme for 10~15 minutes. After cooling to room temperature, filter through diatomaceous earth or membrane filtration to obtain a clarified extract.

[0031] Step S3 solves one of the core challenges in processing Cornus officinalis beverages: clarification and stability. Cornus officinalis extract contains a large amount of macromolecules such as pectin, cellulose, hemicellulose, protein, and tannins. Pectin easily forms a gel-like precipitate under acidic conditions; cellulose and hemicellulose fragments are detached and enter the extract during extraction, forming suspended particles; proteins combine with tannins to form tannic acid-protein complexes, which continue to aggregate and settle during storage, producing a "post-turbidity" phenomenon. These macromolecules are the main causes of turbidity, sedimentation, and stratification in beverages.

[0032] This invention employs a compound enzymatic hydrolysis clarification process, utilizing the synergistic effect of pectinase and cellulase to fundamentally solve the aforementioned problems. Pectinase specifically hydrolyzes the α-1,4-glycosidic bonds of pectin molecules, degrading high-molecular-weight pectin into low-molecular-weight galacturonic acid oligomers or monomers, completely eliminating the risk of pectin gel precipitation. Cellulase specifically hydrolyzes the β-1,4-glycosidic bonds of cellulose, degrading cellulose fragments into soluble sugars, eliminating suspended particles and increasing the content of soluble dietary fiber in the beverage, thus providing a certain nutritional enhancement effect. Simultaneously, the hydrolytic action of pectinase and cellulase also disrupts the tannin-protein complex structure encapsulated in cell wall fragments, releasing tannins, which are then effectively removed in subsequent diatomaceous earth filtration or membrane filtration stages, fundamentally preventing post-turbidity problems during storage.

[0033] This invention optimized and determined the ratio of the compound enzymes and the enzymatic hydrolysis parameters through extensive experiments. The amount of pectinase added was controlled at 0.01%~0.05% of the extract volume, preferably 0.02%~0.03%; the amount of cellulase added was controlled at 0.005%~0.02%, preferably 0.008%~0.012%. Too low an enzyme addition would result in incomplete clarification; too high an addition would increase costs and potentially introduce excessive exogenous proteins, affecting product quality. The hydrolysis temperature was controlled at 45~55℃ (preferably 48~52℃), which falls within the optimal activity temperature range for both pectinase and cellulase, resulting in the highest hydrolysis efficiency. The hydrolysis time was controlled at 60~120 minutes (preferably 80~100 minutes) to ensure complete hydrolysis. After enzymatic hydrolysis, the temperature is raised to 90-95℃ for 10-15 minutes to inactivate the enzyme. This not only completely inactivates the enzyme preparation and prevents residual enzyme activity from continuing to act and causing quality deterioration in subsequent processes and product storage, but also serves as a pasteurization process, providing microbial safety assurance for subsequent processes.

[0034] The extract, after being treated with compound enzymes, is then filtered through diatomaceous earth or a membrane (preferably a microfiltration membrane with a pore size of 0.2~0.5μm) to effectively remove insoluble particles, incompletely hydrolyzed cell wall fragments, and tannin-protein aggregates that may form after enzyme inactivation. The resulting clear extract has a transmittance ≥95% (measured at 660nm wavelength using distilled water as a reference), and exhibits excellent clarification stability after 6 months of storage at room temperature without visible precipitation or turbidity.

[0035] Step S4, multi-component blending: Add one or more of the following to the clarified extract obtained in step S3: wolfberry extract, hawthorn extract, and jujube extract, wherein the clarified extract of Cornus officinalis accounts for 40% to 70% of the total material volume. Then add a sweetener and an acidity regulator. The sweetener is selected from one or more of crystalline fructose, erythritol, and xylitol, and the amount added is 2% to 8% of the total material mass. The acidity regulator is selected from one or more of citric acid, malic acid, and sodium citrate. Adjust the pH to 3.8 to 4.5, stir and mix evenly to obtain the blended solution.

[0036] Step S4 is another key technological aspect of this invention. Cornus officinalis itself has a pronounced sour and bitter taste, which is a major sensory barrier limiting its direct use as a beverage ingredient. Traditional methods often involve adding large amounts of sucrose to mask these unpleasant flavors, but excessive sucrose not only fails to meet modern consumers' demand for low-sugar, healthy beverages, but also has limited masking effects. This invention proposes the concept of "flavor synergy," introducing extracts from medicinal and edible ingredients such as goji berries, hawthorn, and red dates to create flavor complementarity and synergistic effects with the Cornus officinalis extract.

[0037] Goji berry extract has a sweet taste and is rich in goji berry polysaccharides and betaine, which have a natural sweetness-harmonizing effect, effectively neutralizing the tartness of Cornus officinalis. Hawthorn extract has a unique sweet and sour flavor and fruity aroma, and is rich in organic acids such as hawthorn acid and citric acid, as well as flavonoids. It can form a rich and complex acidity with the sourness of Cornus officinalis, avoiding the monotony and irritation of a single taste. Jujube extract has a rich jujube aroma and sweetness, and is rich in jujube polysaccharides and cyclic adenosine monophosphate (cAMP), which can provide natural sweetness and give the beverage a mellow taste and rich fruity aroma. The three extracts, combined with Cornus officinalis extract, form a multi-layered complex flavor profile of "sour-sweet-fragrant-mellow". The sourness is mellow and layered, the sweetness is natural and not cloying, the aroma is harmonious and long-lasting, and the taste is mellow and smooth, fundamentally solving the technical problem of poor flavor in Cornus officinalis beverages.

[0038] From a health benefits perspective, goji berries, hawthorn, red dates, and cornelian cherry have excellent synergistic effects in both traditional Chinese medicine theory and modern nutrition. Goji berries nourish the liver and kidneys, benefit essence and improve eyesight, complementing the liver and kidney tonifying effects of cornelian cherry; hawthorn aids digestion, strengthens the stomach, promotes qi circulation and dispels blood stasis, forming a balanced "one astringent, one dispersing" combination with the astringent and consolidating effects of cornelian cherry; red dates tonify the middle jiao, replenish qi, nourish blood and calm the mind, working together with cornelian cherry to replenish qi and nourish blood. The combination of multiple medicinal and edible ingredients allows the beverage to maintain the core health benefits of cornelian cherry while expanding its efficacy spectrum and achieving synergistic effects.

[0039] The preferred proportions of the components in this invention are: 40-55 parts of Cornus officinalis clarified extract, 15-25 parts of Lycium barbarum extract, 10-20 parts of Hawthorn extract, and 15-25 parts of Jujube extract, all by volume. This proportion range was optimized and determined through systematic sensory evaluation experiments, within which the acidity, sweetness, aroma, and taste of the beverage are optimally balanced.

[0040] Regarding sweeteners, this invention abandons the traditional strategy of adding high amounts of sucrose and instead uses a compound sweetener of crystalline fructose and erythritol. Crystalline fructose has a sweetness approximately 1.2 to 1.8 times that of sucrose, with a refreshing and pure sweetness and the characteristic of enhanced sweetness at low temperatures, making it very suitable for flavoring cold beverages. Erythritol is a zero-calorie natural sweetener with a sweetness approximately 60% to 70% that of sucrose, offering a refreshing taste and excellent synergistic sweetness effect. When used in combination with fructose, it produces a synergistic effect greater than the sum of its parts (1+1>2). The combined use of the two (preferably at a mass ratio of 1:(0.8~1.5)) effectively neutralizes the sourness and bitterness of Cornus officinalis while controlling the total calories of the product, meeting the modern consumer demand for "low-sugar / low-calorie" healthy drinks. The total amount of sweetener added is controlled at 2% to 8% (preferably 3% to 6%) of the total material mass. Within this range, an ideal balance of taste is achieved without masking the natural flavor characteristics of Cornus officinalis and other ingredients due to excessive sweetness.

[0041] Regarding acidity adjustment, the pH of the beverage is adjusted to 3.8-4.5 by adding one or more of citric acid, malic acid, and sodium citrate. This pH range has multiple technical implications: First, pH 3.8-4.5 is an unsuitable growth range for most pathogenic and spoilage bacteria, which, combined with subsequent sterilization processes, effectively ensures the microbial safety of the product. Second, this pH range is the optimal acidity range for Cornus officinalis beverages, resulting in a mild and palatable sour taste. Third, an acidic environment is beneficial to the chemical stability of iridoid glycosides such as loganin and monoglobulin, as well as polyphenolic components. Fourth, a pH value below 4.5 allows for lower-intensity heat sterilization conditions, which is beneficial for the protection of active ingredients.

[0042] Step S5, Homogenization and Degassing: The prepared solution obtained in step S4 is preheated to 55~70℃ and homogenized at 15~25MPa for 1~2 times. Then, vacuum degassing is performed at a vacuum degree of -0.06~-0.09MPa for 10~20 minutes to obtain a degassed prepared solution.

[0043] The homogenization process in step S5 plays a crucial role in the physical stability and smoothness of the beverage. Although the prepared liquid has undergone complex enzymatic hydrolysis and filtration clarification, it may still contain small fruit pulp particles, colloidal particles, and insoluble dietary fiber, among other suspended matter. Under high-pressure homogenization conditions of 15-25 MPa, the prepared liquid passes through the narrow gap of the homogenizing valve at high speed. The material is subjected to a combination of strong shear force, impact force, and cavitation effect, further pulverizing the suspended particles to the micron or even submicron level, resulting in a more uniform particle size distribution and effectively preventing particle sedimentation and stratification.

[0044] Preheating to 55-70℃ (preferably 60-65℃) before homogenization is crucial. At this temperature, the viscosity of the material decreases significantly, and its flowability increases, facilitating smooth passage of the material through the homogenizing valve gap during homogenization, reducing energy consumption, and improving efficiency. Simultaneously, preheating allows pectin and protein molecules in the material to expand more readily, promoting a more stable colloidal dispersion system after homogenization.

[0045] The homogenization pressure of 15~25MPa (preferably 18~22MPa) is the optimal range determined through experiments. If the pressure is too low, the pulverization effect will be insufficient, and sedimentation and stratification will easily occur during product storage; if the pressure is too high, it will not only increase energy consumption and equipment wear, but may also cause excessive pulverization of particles, resulting in an excessively large specific surface area and excessively high surface energy, which will increase the tendency of particle agglomeration and sedimentation. At the same time, excessive shear force may damage the molecular structure of some active ingredients.

[0046] After homogenization, vacuum degassing is performed at a vacuum level of -0.06 to -0.09 MPa (preferably -0.07 to -0.08 MPa) for 10 to 20 minutes (preferably 12 to 16 minutes). This degassing process has multiple benefits: first, it removes dissolved oxygen and air bubbles from the preparation liquid, significantly reducing browning, flavor degradation, and active ingredient degradation caused by oxidation during processing and storage; second, it eliminates foam generated during bottling, ensuring filling accuracy and net content compliance; third, degassed beverages exhibit more uniform heat transfer during sterilization, resulting in more reliable sterilization; and fourth, degassing reduces the oxidative corrosion of packaging materials (such as metal can lids) by dissolved oxygen in the beverage, extending the product's shelf life.

[0047] Step S6, sterilization and filling: The deaerated preparation liquid obtained in step S5 is subjected to ultra-high temperature instantaneous sterilization at a temperature of 130~140℃ for 3~8 seconds. After sterilization, it is rapidly cooled to 25~35℃ and filled and sealed under aseptic conditions to obtain the Cornus officinalis beverage.

[0048] Step S6, employing ultra-high temperature (UHT) sterilization combined with aseptic filling, is another core technical feature of this invention. Traditional Cornus officinalis beverages typically use sterilization processes at 100°C under normal pressure for 300 seconds or at 120°C for 20 seconds. While prolonged high-temperature treatment can meet the requirements for microbial elimination, it leads to significant degradation of heat-sensitive active ingredients such as loganin and monosodium glutamate, substantial loss of vitamin C, deepening of color and browning, and volatilization and deterioration of flavor compounds.

[0049] This invention raises the sterilization temperature to 130-140℃ (preferably 135-138℃) while significantly shortening the sterilization time to 3-8 seconds (preferably 4-6 seconds). The theoretical basis for this process selection is the difference in temperature coefficients between microbial lethality kinetics and chemical reaction kinetics. The temperature coefficient (Z-value) for microbial lethality is typically in the range of 5-10℃, meaning that the lethality rate increases by 1-2 times for every 10℃ increase in temperature; while the temperature coefficient (Q-value) for chemical reactions (such as vitamin C degradation, browning reaction, and degradation of active ingredients)... 10 The ΔE value is typically 2-3, meaning that the reaction rate increases 2-3 times for every 10°C increase in temperature. This implies that under high-temperature, short-duration conditions, the increase in the lethality rate of microorganisms is significantly greater than the acceleration rate of chemical reactions. Therefore, ultra-high temperature (UHT) instantaneous sterilization can minimize the damage to active ingredients, nutrients, color, and flavor in products while achieving the same sterilization effect (commercial sterility). After UHT treatment, the retention rates of loganin and monosodium glutamate in the product are increased by 15%-25% compared to traditional pasteurization, the vitamin C retention rate is increased by 20%-30%, and the color change ΔE value is reduced by more than 40%.

[0050] Rapid cooling to 25-35℃ (preferably 28-32℃) after sterilization is a crucial step in ensuring product quality. Rapid cooling quickly terminates the residual heat effect in the material after heat sterilization, preventing further degradation of active ingredients and flavor deterioration caused by "post-heating." Aseptic filling and sealing are performed in a Class 100 cleanroom environment. Packaging containers are pre-sterilized, and glass or PET bottles are used for cold aseptic filling or hot filling to ensure the product is packaged without secondary contamination.

[0051] The Cornus officinalis beverage prepared through the above steps S1~S6 shall have a total content of loganin and monoglycosides of not less than 1.20 g / L, a total polysaccharide content of not less than 0.80 g / L, a soluble solids content of 8%~15%, a total acid content (calculated as citric acid) of 0.20%~0.45%, a pH value of 3.8~4.5, a light transmittance of ≥95%, and a shelf life of not less than 12 months at room temperature (25℃), meeting the relevant requirements of GB / T31121-2014 "Fruit and Vegetable Juices and Their Beverages" and GB7101-2022 "National Food Safety Standard for Beverages".

[0052] In summary, compared with the prior art, the present invention includes at least one of the following beneficial technical effects:

[0053] A stepped, gradient, variable-temperature multi-stage extraction process for Cornus officinalis beverages was proposed and successfully applied for the first time. This three-stage gradient extraction strategy—extracting heat-sensitive components in the first temperature range (50-60℃), efficiently extracting the main active components of iridoid glycosides in the second temperature range (65-75℃), and deeply extracting polysaccharides and triterpenoids in the third temperature range (80-90℃)—achieves optimal batch extraction of active components with different polarities and thermal stabilities. Combined with intermittent ultrasonic treatment (2-5 minutes per session, 5-10 minute intervals), it effectively avoids the attenuation gap and localized overheating problems of traditional continuous ultrasonic treatment. The overall extraction efficiency is 20%-35% higher than traditional single-temperature extraction, and the retention rates of loganin and mononoside are more than 25% higher than traditional high-temperature, long-term extraction, providing a novel technical approach for the efficient retention of active components in Cornus officinalis beverages.

[0054] A composite enzymatic hydrolysis clarification process specifically designed for the characteristics of Cornus officinalis extract has been developed. Utilizing the synergistic effect of pectinase and cellulase, under mild conditions of 45-55℃ and 60-120 minutes, the turbidity-causing macromolecules such as pectin and cellulose in the Cornus officinalis extract are specifically hydrolyzed into soluble small molecules. Combined with subsequent diatomaceous earth filtration or microfiltration membrane filtration, this fundamentally solves the clarification and stability problem of Cornus officinalis beverages. Compared to traditional gelatin clarification methods, this composite enzymatic hydrolysis clarification process avoids the introduction of animal-derived clarifying agents, shortens the clarification time by more than 70%, and achieves a more thorough and stable clarification effect—the resulting product has a light transmittance of ≥95%, and exhibits no visible sediment or turbidity after 6 months of storage at room temperature, solving the long-standing technical problem of post-turbidity in Cornus officinalis beverage processing.

[0055] A multi-component blending system based on the concept of flavor synergy was constructed. Through systematic research on the blending rules of Cornus officinalis extract with Lycium barbarum extract, Hawthorn extract, and Jujube extract, the optimal blending ratio of 40-55 parts Cornus officinalis clarified extract, 15-25 parts Lycium barbarum extract, 10-20 parts Hawthorn extract, and 15-25 parts Jujube extract (all by volume) was determined. These four medicinal and edible ingredients formed a multi-layered complex flavor profile of "sour-sweet-fragrant-mellow," with a mellow and layered sourness, a natural and not cloying sweetness, a harmonious and lasting aroma, and a mellow and smooth taste, fundamentally solving the technical bottleneck of sour and astringent taste and monotonous flavor in Cornus officinalis beverages. Simultaneously, the use of a compound sweetener of crystalline fructose and erythritol to replace the traditional high-sucrose formula significantly reduced the product's calorie load while maintaining a balanced taste, meeting the modern consumer demand for healthy, low-sugar beverages.

[0056] The sterilization process for Cornus officinalis beverages has been optimized. Ultra-high temperature (UHT) instantaneous sterilization (130-140℃, 3-8 seconds) combined with aseptic filling fully utilizes the difference in temperature coefficients between microbial lethality kinetics and chemical reaction kinetics. This significantly reduces the thermal degradation loss of heat-sensitive active ingredients while ensuring commercial sterility. Compared to traditional sterilization at 100℃ and atmospheric pressure for 300 seconds, the retention rates of loganin and monosodium glutamate are increased by 15%-25%, vitamin C retention by 20%-30%, browning is significantly reduced, and flavor is more fully preserved, achieving an optimal balance between sterilization effectiveness and quality protection.

[0057] This invention establishes a complete, standardized, and industrially sustainable production process, encompassing the entire chain from raw material pretreatment to finished product bottling. The invention includes a complete process chain encompassing material selection and grading, gradient temperature multi-stage extraction, compound enzymatic hydrolysis and clarification, scientific formulation and blending of multiple components, homogenization and degassing, and ultra-high temperature instantaneous sterilization and aseptic bottling. The parameters are matched closely between each step, and the processes are tightly integrated, providing reliable technical support for the large-scale industrial production of Cornus officinalis beverages. The product meets the requirements of national standards such as GB / T31121-2014 and GB7101-2022, has a shelf life of no less than 12 months at room temperature, and possesses excellent market application prospects and industrialization promotion value.

[0058] In summary, this invention effectively solves a series of technical problems existing in the preparation methods of Cornus officinalis beverages, such as low extraction efficiency of active ingredients, poor clarification stability, unpleasant flavor, severe browning, significant sterilization damage, and lack of systematic industrial process solutions. It provides a method for preparing Cornus officinalis beverages with high retention of active ingredients, stable clarification, harmonious taste, natural color, long shelf life, and suitability for continuous industrial production. This opens up a new technical path for the deep processing and high-value utilization of Cornus officinalis in the food and beverage field, and has significant economic and social benefits. Attached Figure Description

[0059] Figure 1 This is a process flow diagram of the preparation method of Cornus officinalis beverage in an embodiment of the present invention. Detailed Implementation

[0060] The technical solutions in the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, and not all embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of this application without creative effort are within the scope of protection of this application.

[0061] Example 1

[0062] Reference Figure 1This embodiment provides a method for preparing a Cornus officinalis beverage, including the following steps:

[0063] Step S1, Material Selection and Grading:

[0064] Harvest fresh Cornus officinalis fruits at approximately 92% maturity, removing moldy, rotten, insect-infested, unripe, and impurity fruits. The fruits are then manually graded according to size and color, selecting medium-sized fruits with a uniform, bright red color. The graded Cornus officinalis fruits are then washed twice with running water to remove surface dust and microorganisms, and drained of excess water to obtain the graded fresh fruits.

[0065] Step S2, stepped gradient temperature-varying multi-stage extraction:

[0066] Weigh 100 kg of the graded fresh fruit obtained in step S1 and place it in a multi-functional extraction tank. Add 1000 kg of pure water as the extraction solvent at a material-to-liquid mass ratio of 1:10. Start stirring and heat to 55°C, maintaining a stable temperature for the first stage of extraction, which takes 45 minutes. After the first stage of extraction, continue heating to 70°C, maintaining a stable temperature for the second stage of extraction, which takes 30 minutes. After the second stage of extraction, heat again to 85°C, maintaining a stable temperature for the third stage of extraction, which takes 15 minutes.

[0067] Intermittent ultrasonic treatment was used throughout the extraction process: within each temperature range, ultrasonic treatment was performed every 8 minutes, with each session lasting 3 minutes. The ultrasonic frequency was 30 kHz, and the ultrasonic power density was 45 W / L. The ultrasonic probe was placed in the middle of the extraction tank to ensure that the ultrasonic energy propagated fully in the liquid.

[0068] After extraction, while still hot (temperature not lower than 60℃), the extract is coarsely filtered through a 100-mesh stainless steel sieve to separate the extract from the residue. The residue is discarded, and approximately 980 kg of the combined extract is collected.

[0069] Step S3, compound enzymatic hydrolysis clarification:

[0070] Transfer the extract obtained in step S2 to an enzymatic hydrolysis vessel and cool to 50°C. Add the compound enzyme preparation to the extract: first, add food-grade acidic pectinase (enzyme activity 35000 U / g), at a volume of 0.025% of the extract volume; then add food-grade neutral cellulase (enzyme activity 12000 U / g), at a volume of 0.010% of the extract volume. After stirring evenly, enzymatically hydrolyze at a constant temperature of 50°C for 90 minutes.

[0071] After enzymatic hydrolysis, the temperature was raised to 92℃ for 12 minutes to inactivate the enzyme. After enzyme inactivation, the solution was rapidly cooled to room temperature (around 25℃) using a cooling coil. The cooled hydrolysate was then filtered through a 0.3μm pore size polypropylene microfiltration membrane, and the clear filtrate was collected to obtain approximately 960 kg of clear extract.

[0072] The contents of loganin and monoglycine in the clarified extract were 0.72 g / L and 0.58 g / L, respectively, with a total content of 1.30 g / L, as determined by high performance liquid chromatography (HPLC). The total polysaccharide content was 0.92 g / L, determined by the phenol-sulfuric acid method. The transmittance was 96.5%, determined by spectrophotometry (660 nm, with distilled water as a reference).

[0073] Step S4, multiple groups of allocation and deployment:

[0074] First, prepare wolfberry extract, hawthorn extract, and jujube extract separately:

[0075] Preparation of wolfberry extract: Weigh 20 kg of dried wolfberries, wash them, add 200 kg of pure water at a material-to-liquid mass ratio of 1:10, heat to 90℃ and maintain extraction for 45 minutes, filter through a 100-mesh filter, and collect about 190 kg of filtrate for later use.

[0076] Preparation of hawthorn extract: Weigh 15kg of dried hawthorn slices, wash them, add 150kg of pure water at a material-to-liquid mass ratio of 1:10, heat to 90℃ and maintain extraction for 40 minutes, filter through a 100-mesh filter, and collect about 142kg of filtrate for later use.

[0077] Preparation of jujube extract: Weigh 20kg of dried jujube slices, wash them, add 200kg of pure water at a material-to-liquid mass ratio of 1:10, heat to 90℃ and maintain extraction for 50 minutes, filter through a 100-mesh filter, and collect about 188kg of filtrate for later use.

[0078] Add the Cornus officinalis clarified extract obtained in step S3, the Lycium barbarum extract, the hawthorn extract and the jujube extract prepared above into a mixing tank in a volume ratio of 48:20:15:17, and stir well.

[0079] Add the compound sweetener to the mixing tank: 3.2 kg of crystalline fructose and 3.8 kg of erythritol, the total amount of which accounts for approximately 5.0% of the total mass of the mixed material. Stir until completely dissolved.

[0080] Add acidity regulators to the mixing tank: 0.6 kg citric acid and 0.3 kg sodium citrate, to adjust the pH of the beverage to 4.0 ± 0.1. Continue stirring for 15 minutes to ensure all components are thoroughly mixed, yielding approximately 1400 L of the prepared liquid.

[0081] Step S5, homogenization and degassing:

[0082] The prepared liquid obtained in step S4 was preheated to 62°C using a plate heat exchanger. The preheated liquid was then fed into a high-pressure homogenizer and homogenized twice at 20 MPa. After homogenization, the material was transferred to a vacuum degassing tank, with the vacuum level controlled at -0.075 MPa for 15 minutes. After degassing, samples were taken for testing, confirming that the gas content had decreased to below 0.5%, thus obtaining the degassed prepared liquid.

[0083] Step S6, sterilization and filling:

[0084] The degassed preparation liquid obtained in step S5 is fed into a tubular ultra-high temperature instantaneous sterilization system. The sterilization temperature is set to 137℃, and the sterilization time is set to 5 seconds. After sterilization, the material is rapidly cooled to 30±2℃ via a plate heat exchanger. The cooled material is then filled into pre-sterilized PET bottles using an aseptic filling machine in a Class 100 clean filling room. The filling capacity is 350mL / bottle. After filling, the bottles are immediately capped and sealed to obtain the finished Cornus officinalis beverage.

[0085] Product testing results:

[0086] The Cornus officinalis beverage prepared in Example 1 was tested, and the results are as follows:

[0087] (1) Sensory indicators: The beverage is orange-red to reddish-brown, with a uniform and natural color. It has a complex aroma of cornus officinalis, wolfberry, hawthorn and red dates, and the aroma is harmonious and pleasant. The taste is sweet and sour, mellow and smooth, without bitterness, and without visible impurities and sediment.

[0088] (2) Physicochemical properties: soluble solids content (20℃, refractometer method) was 10.5%; total acid content (calculated as citric acid, acid-base titration method) was 0.32%; pH value was 4.02; total content of loganin and monoglycine (HPLC method) was 1.24 g / L; total polysaccharide content (phenol-sulfuric acid method) was 0.88 g / L; transmittance (660 nm, with distilled water as reference) was 96.2%.

[0089] (3) Microbiological indicators: total bacterial count ≤10 CFU / mL, coliform bacteria ≤1 CFU / mL, mold and yeast ≤1 CFU / mL, pathogenic bacteria (Salmonella, Staphylococcus aureus, Shigella) not detected, which meets the requirements of GB7101-2022 National Food Safety Standard for Beverages.

[0090] (4) Stability test: After the product was stored at room temperature (25℃) for 12 months, the sensory quality remained good, with no layering, no precipitation, and no abnormal color change; the total content retention rate of loganin and monosodium glutamate was 92.5%, the total polysaccharide content retention rate was 89.3%, and all physicochemical and microbiological indicators met the product standard requirements.

[0091] This invention relates to a stepped temperature gradient multi-stage extraction process. In the field of food extraction, it is generally preferred to find a single "optimal temperature" for extraction using orthogonal experiments or response surface methodology. The three-temperature gradient progressive design employed in this invention is a creative concept based on in-depth research into the physicochemical properties of different active ingredients. Heat-sensitive flavonoids are preferentially dissolved in the low-temperature range, iridoid glycosides are efficiently dissolved in the medium-temperature range, and polysaccharides and triterpenoids are deeply dissolved in the high-temperature range. Existing technologies do not teach or suggest dividing the extraction process into three sequential temperature zones, nor do they provide guidance on combining gradient temperature changes with intermittent ultrasound.

[0092] Regarding the clarification of Cornus officinalis beverages using compound enzymatic hydrolysis, existing technologies often employ a single pectinase plus gelatin process. However, gelatin poses animal-derived safety risks and the clarification effect is not thorough. This invention utilizes a combined enzymatic hydrolysis of pectinase and cellulase, coupled with membrane filtration. This not only eliminates the use of animal-derived clarifying agents but also fundamentally solves the post-turbidity problem. The synergistic clarification effect produced by pectinase and cellulase in the Cornus officinalis extract system is a non-obvious combination.

[0093] Regarding multi-component compounding, the scheme of combining four medicinal and edible ingredients in a specific ratio to form a synergistic flavor effect is not a simple "addition and matching", but a non-obvious technical solution obtained through systematic sensory evaluation and formula optimization experiments.

[0094] Regarding UHT sterilization, although the UHT sterilization technology itself is known, its application to Cornus officinalis beverages and the determination of specific parameter ranges of 130-140℃ / 3-8s are aimed at maximizing the retention rate of active ingredients.

[0095] Table 1: Comparison of the effects of the present invention and the prior art

[0096]

[0097] This invention adopts an overall technical solution of "stepped gradient temperature multi-stage extraction + compound enzymatic hydrolysis clarification + multi-component compounding and blending + UHT sterilization". The core stepped temperature multi-stage extraction (three temperature ranges + intermittent ultrasound) has not been disclosed or shown in the prior art. The combination of the various technical features produces a synergistic effect, which can be obviously derived by those who are not skilled in the art based on the prior art.

[0098] The overall extraction efficiency of this invention is 20%-35% higher than that of traditional single-temperature extraction, and the retention rates of loganin and monoglycosides are increased by more than 25%. The compound enzymatic hydrolysis clarification process makes the product transmittance ≥95%, and there is no precipitation after 12 months of storage at room temperature. The clarification time is shortened by more than 70% compared with the traditional gelatin method. The total content of loganin and monoglycosides in the product reaches 1.24g / L, which is far higher than the level of similar products in the prior art.

[0099] Example 2

[0100] The difference between this embodiment and Embodiment 1 is that in step S2, a combination of water and an aqueous ethanol solution is used as the extraction solvent. The specific steps are as follows:

[0101] Step S2, stepped gradient temperature-controlled multi-stage extraction: Weigh 100 kg of graded fresh fruit obtained in step S1. For the first temperature range (55℃) and the second temperature range (70℃), use pure water as the extraction solvent, with a material-to-liquid mass ratio of 1:5. For the third temperature range (85℃), use a 40% (v / v) ethanol aqueous solution as the extraction solvent, with a material-to-liquid mass ratio of 1:5. Other process parameters are the same as in Example 1.

[0102] Extraction was performed using a combination of water and ethanol-water solutions. The third temperature stage utilized the excellent solubility of ethanol-water solutions for weakly polar components such as triterpenoids, further improving the extraction rate of ursolic acid and other triterpenoid active ingredients. Testing showed that the ursolic acid content in the clarified extract obtained using this method was approximately 18% higher than that in Example 1.

[0103] The other steps are the same as in Example 1. In addition to possessing the excellent qualities described in Example 1, the resulting beverage has a higher content of triterpenoid active ingredients and a more comprehensive spectrum of health benefits.

[0104] Example 3

[0105] The difference between this embodiment and Embodiment 1 lies in the adjustment of the proportions of each group and the sweetener formulation in step S4, as detailed below:

[0106] The volume ratio of each component in step S4 is as follows: 42 parts of Cornus officinalis clarified extract, 22 parts of Lycium barbarum extract, 18 parts of Hawthorn extract, and 18 parts of Jujube extract.

[0107] The sweetener is a compound sweetener of crystalline fructose and xylitol. The amount of crystalline fructose added is 2.0 kg and the amount of xylitol added is 4.5 kg. The total amount of the two added accounts for about 4.5% of the total mass of the mixed material.

[0108] The other steps are the same as in Example 1. The resulting beverage has a sweet and refreshing flavor and is about 15% lower in calories than in Example 1, making it suitable for consumers who have high requirements for controlling their calorie intake.

[0109] Example 4

[0110] The difference between this embodiment and Embodiment 1 lies in the adjustment of the sterilization parameters and filling method in step S6, as detailed below:

[0111] Step S6: Sterilization and Filling: The sterilization temperature is adjusted to 135℃, and the sterilization time is adjusted to 6 seconds. Hot filling is used. After sterilization, the material is not rapidly cooled; instead, it is kept at approximately 85℃ and directly filled into pre-cleaned and sterilized heat-resistant glass bottles in a clean filling environment. Immediately after filling, the bottles are screwed on and sealed. The bottles are then inverted to utilize the residual heat of the material to sterilize the inside of the caps. After maintaining the inverted position for 3 minutes, the bottles are rapidly cooled to room temperature.

[0112] Hot filling does not require a strictly aseptic filling environment, and the equipment investment and operating costs are relatively low, making it suitable for small to medium-scale production. The resulting product has essentially the same specifications as in Example 1, and a shelf life of no less than 12 months at room temperature.

[0113] Comparative Example 1 (Contrast with Traditional Hot Water Extraction Process)

[0114] Cornus officinalis extract was prepared using a traditional hot water extraction process: 100 kg of fresh Cornus officinalis fruit was added to 1000 kg of pure water, and the mixture was heated to 90°C for 6 hours, with stirring every hour during the extraction. After extraction, the extract was filtered. Subsequent preparation, homogenization, degassing, and sterilization processes were the same as in Example 1.

[0115] Testing revealed that the total content of loganin and monoglucoside in the extract was 0.85 g / L, and the total polysaccharide content was 0.61 g / L, which were only 65.4% and 66.3% of those in Example 1, respectively. The resulting beverage had a slightly sour and astringent taste, a light transmittance of 82.3%, and visible precipitation appeared after 3 months of storage at room temperature.

[0116] Comparative Example 2 (Single Temperature Extraction Control)

[0117] A single-temperature (70℃) extraction process was used: 100kg of fresh Cornus officinalis fruit was added to 1000kg of pure water and extracted at a constant temperature of 70℃ for 90 minutes, supplemented by intermittent ultrasonic treatment as in Example 1. Subsequent processes were the same as in Example 1.

[0118] The results showed that the total content of loganin and monoglycine in the extract was 1.02 g / L, and the total polysaccharide content was 0.71 g / L, which were 78.5% and 77.2% of those in Example 1, respectively. The results indicate that although single-temperature extraction is an improvement over traditional hot water extraction, it still cannot achieve the comprehensive extraction efficiency of the stepped gradient temperature-varying multi-stage extraction method of this invention.

[0119] Comparative Example 3 (Traditional Gelatin Clarification Control)

[0120] The Cornus officinalis extract was treated using a traditional gelatin clarification process: 0.35% (by mass / volume) gelatin solution was added to the extract obtained in step S2 of Example 1, and the mixture was slowly stirred and allowed to stand at room temperature for 6 hours. The clarified extract was then filtered. Subsequent processes were the same as in Example 1.

[0121] Testing revealed that the transmittance of the obtained extract was 88.7%, lower than the 96.2% in Example 1; slight turbidity and trace precipitation appeared after 6 months of storage at room temperature. This comparative example demonstrates that the clarification effect and stability of the traditional gelatin clarification method are significantly inferior to the composite enzymatic hydrolysis clarification process of this invention.

[0122] Comparative Example 4 (Traditional sterilization process control)

[0123] Traditional pasteurization process was used: the degassed preparation solution obtained in step S5 of Example 1 was filled into glass bottles, sealed, and then sterilized in a water bath autoclave at a temperature of 100°C for 300 seconds (5 minutes). After sterilization, the solution was cooled to room temperature.

[0124] Testing revealed that the total content of loganin and monoglucoside in the sterilized beverage was 0.97 g / L, a decrease of approximately 21.8% compared to 1.24 g / L in Example 1; the vitamin C retention rate was approximately 28% lower than in Example 1; the beverage color was significantly darker than in Example 1 (ΔE value reached 4.8); and the flavor quality was significantly lower than in Example 1 after 12 months of storage at room temperature.

[0125] Example 5: Validation of the synergistic effect of gradient temperature multi-stage extraction and intermittent ultrasound

[0126] This embodiment aims to verify whether there is a synergistic effect between stepped gradient temperature-controlled multi-stage extraction and intermittent ultrasound.

[0127] 5.1 Experimental Group Design

[0128] Using 100 kg of graded fresh fruit obtained in step S1 as raw material, the following 4 sets of experiments were designed:

[0129] Table 2: Experimental Design for Verifying Synergistic Effects of Extraction Processes

[0130]

[0131] 5.2 Experimental Results

[0132] Table 3: Results of the experimental verification of the synergistic effect of gradient temperature variation and intermittent ultrasound (g / L, n=3)

[0133]

[0134] 5.3 Synergy Enhancement Index (SI) Calculation and Analysis

[0135] Using the total amount of diglycosides as an indicator, the synergistic index (SI) of each process combination was calculated:

[0136] SI = Measured value / Algebraic sum of the effects of each factor acting alone

[0137] The calculation method for the individual effects of each factor is as follows:

[0138] The individual contribution of gradient temperature variation = Group 2 - Group 4 = 0.87 - 0.68 = 0.19 g / L;

[0139] The individual contribution of intermittent ultrasound = Group 3 - Group 4 = 1.02 - 0.68 = 0.34 g / L;

[0140] The sum of individual contributions = 0.19 + 0.34 = 0.53 g / L;

[0141] The combined theoretical value = base value of group 4 + sum of individual contributions = 0.68 + 0.53 = 1.21 g / L;

[0142] The measured value after combination (Group 1) = 1.30 g / L;

[0143] Synergy enhancement index SI = 1.30 / 1.21 = 1.074;

[0144] SI>1 indicates a positive synergistic effect. SI=1.074 indicates that the combined use of gradient temperature multi-stage extraction and intermittent ultrasound produces a significantly greater effect than the simple sum of the effects of the two alone, with an improvement of approximately 7.4%.

[0145] 5.4 Synergistic Effect Mechanism Analysis

[0146] The synergistic effect of gradient temperature and intermittent ultrasound is mainly reflected in the following aspects: (1) Gradient temperature causes the cell wall structure to undergo thermal relaxation to different degrees in different temperature ranges, increasing the permeability of the cell wall and creating more favorable physical conditions for the ultrasound cavitation effect; (2) Intermittent ultrasound destroys the cell wall structure through cavitation and mechanical effects, accelerating the release of intracellular active components, while the thermodynamic driving force provided by temperature variation further promotes the diffusion of released components into the solvent body; (3) The "work-rest" cycle mode of intermittent ultrasound is exactly matched with the heating rhythm of gradient temperature variation, and the ultrasound treatment in each temperature range can achieve the best cavitation effect at that temperature. The combined effect of the above factors forms a synergistic effect of 1+1>2.

[0147] Example 6: Validation of the synergistic effect of pectinase and cellulase in the compound enzymatic hydrolysis clarification process

[0148] This embodiment aims to quantitatively verify the synergistic effect of pectinase and cellulase in the clarification of Cornus officinalis extract and to eliminate interference from possible impurities in the enzyme preparation.

[0149] 6.1 Experimental Design

[0150] Using the extract obtained in step S2 of the same batch as raw material, the following 6 groups of experiments were designed, with each group repeated 3 times:

[0151] Table 4: Experimental Design for Verifying the Synergistic Effect of Pectinase and Cellulase

[0152]

[0153] 6.2 Experimental Results

[0154] Table 5: Results of the experimental verification of synergistic effect of compound enzymes

[0155]

[0156] 6.3 Quantitative Analysis of Synergistic Effects

[0157] Using initial transmittance as an indicator, the synergistic effect of pectinase and cellulase was calculated:

[0158] The effect of 0.025% pectinase alone (compared to the control without enzyme) = 91.2 - 80.5 = 10.7 percentage points;

[0159] The effect of 0.010% cellulase alone is 85.6 - 80.5 = 5.1 percentage points;

[0160] The sum of the individual effects = 10.7 + 5.1 = 15.8 percentage points;

[0161] The combined effect of the enzyme complex (C1 vs C6) = 96.5 - 80.5 = 16.0 percentage points;

[0162] The excess of synergistic efficiency = 16.0 - 15.8 = 0.2 percentage points (exceeding approximately 1.3%).

[0163] Using light transmittance after 6 months of storage as an indicator, the synergistic effect is even more significant:

[0164] The combined effect of the enzyme complex = 95.8 - 72.3 = 23.5 percentage points;

[0165] The sum of the individual effects = (86.2 - 72.3) + (80.5 - 72.3) = 13.9 + 8.2 = 22.1 percentage points;

[0166] The excess of synergistic efficiency = 23.5 - 22.1 = 1.4 percentage points (exceeding approximately 6.3%).

[0167] It is worth noting that C1 (compound enzyme, pectinase 0.025% + cellulase 0.010%) was more effective than C4 (doubled pectinase 0.050% used alone) and C5 (doubled cellulase 0.020% used alone), indicating that the effect of the compound enzyme cannot be replaced by increasing the dosage of the single enzyme, and there is a real synergistic effect between the two enzymes.

[0168] Furthermore, the compound enzyme treatment produced unexpected technical effects, significantly increasing the soluble dietary fiber content (C1 at 1.45 g / L, C2 at only 1.02 g / L, and C3 at only 1.35 g / L). This is because cellulase partially degrades insoluble cellulose fragments into soluble oligosaccharides and dietary fiber, unexpectedly enhancing the product's nutritional value while improving clarity. This "win-win" effect is something that those skilled in the art could not have foreseen during the design phase.

[0169] The method for preparing Cornus officinalis beverage provided by this invention organically combines four core technologies: step-gradient temperature-controlled multi-stage extraction (three-temperature-segment progression + intermittent ultrasound), pectinase-cellulase complex enzymatic hydrolysis clarification, a four-ingredient compound of Cornus officinalis, Lycium barbarum, Hawthorn, and Jujube, and ultra-high temperature instantaneous sterilization. This forms a complete and synergistic end-to-end process. The core technologies are not simply parallel but rather intrinsically synergistic. Gradient temperature extraction provides a suitable substrate structure for complex enzymatic hydrolysis, which removes turbidity and astringency-causing substances for flavor blending, thus optimizing the sensory quality of the beverage. UHT sterilization maximizes the preservation of active ingredients accumulated throughout the entire process. Experimental verification shows that the resulting beverage has a total content of loganin and monosodium glutamate of over 1.24 g / L, a total polysaccharide content of over 0.88 g / L, a light transmittance ≥96%, and a shelf life of at room temperature of no less than 12 months. All indicators meet national standards. This invention provides a novel technical approach for the deep processing and high-value utilization of Cornus officinalis in the food and beverage industry, with significant economic and social benefits.

[0170] The method for preparing Cornus officinalis beverage provided by this invention requires mainly general-purpose equipment for the food industry, including multi-functional extraction tanks, ultrasonic-assisted extraction devices, enzymatic hydrolysis tanks, microfiltration membrane / diatomaceous earth filtration equipment, blending tanks, high-pressure homogenizers, vacuum degassing machines, ultra-high temperature instantaneous sterilization systems, aseptic filling machines, etc. The equipment is mature and reliable, and procurement and maintenance costs are controllable. The operating conditions for each step in the process flow are clearly defined, and the parameter ranges are reasonable, facilitating process control and quality management in continuous industrial production.

[0171] This invention uses ingredients that are both food and medicine, such as Cornus officinalis, wolfberry, hawthorn, and jujube, as raw materials. These raw materials are widely available and have a stable supply. Cornus officinalis is mainly distributed in Henan, Shaanxi, Zhejiang, and Sichuan provinces, with the production and quality of Cornus officinalis from mountainous areas such as Luoyang and Nanyang in Henan province ranking among the top in the country. After Cornus officinalis was officially included in the list of food and medicine homologous ingredients in November 2023, policy obstacles to its use as a food ingredient have been completely eliminated, providing strong policy support and a broad market prospect for the large-scale industrial production of Cornus officinalis beverages.

[0172] The product complies with national standards such as GB / T31121-2014 "Fruit and Vegetable Juices and Beverages" and GB7101-2022 "National Food Safety Standard for Beverages". Based on an annual production of 30 million bottles (350mL / bottle) of Cornus officinalis beverage, it is estimated that approximately 2,100 tons of fresh Cornus officinalis fruit will be consumed annually, which can support approximately 10,000 mu of Cornus officinalis planting bases. This demonstrates significant economic and social benefits and is crucial for promoting the intensive processing of local specialty agricultural and forestry products, increasing farmers' income, and meeting consumer demand for nutritious and healthy beverages.

[0173] The implementation principle of this invention is as follows: This invention discloses a method for preparing a Cornus officinalis beverage, belonging to the field of food processing technology. The method includes: raw material selection and grading; multi-stage extraction with gradient temperature variation, sequentially extracted at 50-60℃, 65-75℃, and 80-90℃, supplemented by intermittent ultrasound; compound enzymatic hydrolysis clarification, using a combination of pectinase and cellulase followed by membrane filtration; multi-component compounding and blending, combining the Cornus officinalis extract with extracts of wolfberry, hawthorn, and jujube, adding a compound sweetener to adjust the flavor; homogenization and degassing; ultra-high temperature instantaneous sterilization and aseptic filling. This invention, through gradient temperature variation extraction, takes into account the dissolution characteristics of different active ingredients; enzymatic hydrolysis clarification thoroughly solves the post-turbidity problem; scientific compounding improves the taste; and UHT sterilization preserves active ingredients. The resulting beverage has a total content of loganin and monoglycoside ≥1.20g / L, is clear and stable, has a long shelf life, and is suitable for industrial production.

[0174] The embodiments described herein are preferred embodiments of the present invention and are not intended to limit the scope of protection of the present invention. Therefore, all equivalent changes made in accordance with the structure, shape, and principle of the present invention should be covered within the scope of protection of the present invention.

Claims

1. A method for preparing a Cornus officinalis beverage, characterized in that, Includes the following steps: Step S1, Selection and Grading: Select fresh Cornus officinalis fruits with a maturity of ≥90%, free from mold, rot, and pests, and grade them according to fruit size and color. Wash them clean, drain the water, and obtain graded fresh fruits. Step S2, stepped gradient temperature-variable multi-stage extraction: The graded fresh fruit obtained in step S1 is added to the extraction solvent at a material-to-liquid mass ratio of 1:(8~15), and a stepped gradient temperature-variable extraction process is adopted, which sequentially goes through: the first temperature section 50~60℃, extraction for 30~60 minutes; the second temperature section 65~75℃, extraction for 20~40 minutes; the third temperature section 80~90℃, extraction for 10~20 minutes; during the extraction process, intermittent ultrasonic treatment is used, with an ultrasonic frequency of 20~40kHz and an ultrasonic power density of 30~60W / L. Each ultrasonic treatment lasts for 2~5 minutes, with an interval of 5~10 minutes. After the extraction is completed, the extract and residue are separated by coarse filtration while hot, and the extract is collected. Step S3, compound enzymatic hydrolysis clarification: Add a compound enzyme preparation to the extract obtained in step S2. The compound enzyme preparation contains pectinase and cellulase. The amount of pectinase added is 0.01%~0.05% of the extract volume, and the amount of cellulase added is 0.005%~0.02% of the extract volume. The enzymatic hydrolysis temperature is 45~55℃, and the enzymatic hydrolysis time is 60~120 minutes. After the enzymatic hydrolysis is completed, the temperature is raised to 90~95℃ to inactivate the enzyme for 10~15 minutes. After cooling to room temperature, the extract is filtered through diatomaceous earth or membrane filtration to obtain a clarified extract. Step S4, Multi-component blending: Add one or more of the following to the clarified extract obtained in step S3: wolfberry extract, hawthorn extract, and jujube extract, wherein the clarified extract of Cornus officinalis accounts for 40% to 70% of the total material volume. Then add a sweetener and an acidity regulator. The sweetener is selected from one or more of crystalline fructose, erythritol, and xylitol, and the amount added is 2% to 8% of the total material mass. The acidity regulator is selected from one or more of citric acid, malic acid, and sodium citrate. Adjust the pH to 3.8 to 4.5, stir and mix evenly to obtain the blended solution. Step S5, Homogenization and Degassing: The prepared solution obtained in step S4 is preheated to 55~70℃ and homogenized at 15~25MPa for 1~2 times. Then, it is degassed under vacuum at a vacuum of -0.06~-0.09MPa for 10~20 minutes to obtain a degassed prepared solution. Step S6, sterilization and filling: The deaerated preparation liquid obtained in step S5 is subjected to ultra-high temperature instantaneous sterilization at a temperature of 130~140℃ for 3~8 seconds. After sterilization, it is rapidly cooled to 25~35℃ and filled and sealed under aseptic conditions to obtain the Cornus officinalis beverage.

2. The method for preparing a Cornus officinalis beverage according to claim 1, characterized in that, The extraction solvent in step S2 is selected from water, an aqueous ethanol solution with a volume fraction of 20% to 60%, or a combination of water and an aqueous ethanol solution with a volume fraction of 20% to 60%. When a combination of water and an aqueous ethanol solution is used, water is used as the extraction solvent in the first and second temperature ranges, and an aqueous ethanol solution with a volume fraction of 30% to 50% is used as the extraction solvent in the third temperature range.

3. The method for preparing a Cornus officinalis beverage according to claim 1, characterized in that, In step S2, the preferred material-to-liquid mass ratio for the stepped gradient temperature-controlled multi-stage extraction is 1:(10~12), wherein the first temperature range is 53~57℃ for 40~50 minutes, the second temperature range is 68~72℃ for 25~35 minutes, and the third temperature range is 83~87℃ for 12~18 minutes; the intermittent ultrasonic treatment uses an ultrasonic frequency of 25~35kHz and an ultrasonic power density of 40~50W / L, with each ultrasonic treatment lasting 3~4 minutes and an interval of 7~8 minutes.

4. The method for preparing a Cornus officinalis beverage according to claim 1, characterized in that, In step S3, the pectinase is a food-grade acidic pectinase with an enzyme activity ≥30000 U / g, and the amount added is 0.02%~0.03% of the extraction liquid volume; the cellulase is a food-grade neutral cellulase with an enzyme activity ≥10000 U / g, and the amount added is 0.008%~0.012% of the extraction liquid volume; the enzymatic hydrolysis temperature is 48~52℃, and the enzymatic hydrolysis time is 80~100 minutes; the membrane filtration adopts a microfiltration membrane with a pore size of 0.2~0.5μm.

5. The method for preparing a Cornus officinalis beverage according to claim 1, characterized in that, The preparation methods for the wolfberry extract, hawthorn extract, and jujube extract mentioned in step S4 are all water extraction methods. Specifically, take dried wolfberry fruit / dried hawthorn slices / dried jujube slices, add water at a material-to-liquid mass ratio of 1:(8~12), extract at 85~95℃ for 30~60 minutes, filter to obtain the extract, and set aside for later use.

6. The method for preparing a Cornus officinalis beverage according to claim 1, characterized in that, When preparing the multi-component combination in step S4, the clarified extract of Cornus officinalis accounts for 40-55 parts, the extract of Lycium barbarum accounts for 15-25 parts, the extract of Hawthorn accounts for 10-20 parts, and the extract of Jujube accounts for 15-25 parts, all of which are by volume. The sweetener is preferably a compound sweetener of crystalline fructose and erythritol, wherein the mass ratio of crystalline fructose to erythritol is 1:(0.8-1.5), and the total amount added is 3%-6% of the total material mass.

7. The method for preparing a Cornus officinalis beverage according to claim 1, characterized in that, In step S5, the preheating temperature for homogenization is 60~65℃, the homogenization pressure is 18~22MPa, and homogenization is performed twice; the vacuum degree for vacuum degassing is -0.07~-0.08MPa, and the degassing time is 12~16 minutes.

8. The method for preparing a Cornus officinalis beverage according to claim 1, characterized in that, The ultra-high temperature instantaneous sterilization in step S6 is 135~138℃ and the sterilization time is 4~6 seconds; after sterilization, it is cooled to 28~32℃, and the filling is carried out in a Class 100 clean environment using glass bottles or PET bottles for hot filling or cold aseptic filling.

9. The method for preparing a Cornus officinalis beverage according to claim 1, characterized in that, The process also includes the following pretreatment of fresh Cornus officinalis fruit before step S1: within 4 hours of harvesting, the fresh Cornus officinalis fruit is pre-cooled at 0-4℃ for 2-4 hours to inactivate enzyme activity and reduce browning; during washing, it is first washed with running water 2-3 times, and then soaked in a 0.1%-0.3% food-grade ascorbic acid aqueous solution for 5-10 minutes for color protection.

10. A method for preparing a Cornus officinalis beverage according to claim 1, characterized in that, In the clarified extract obtained in step S3, the total content of loganin and monoglycine is not less than 1.20 g / L, and the total polysaccharide content is not less than 0.80 g / L; in the Cornus officinalis beverage obtained in step S6, the soluble solids content is 8%~15%, the total acid content (calculated as citric acid) is 0.20%~0.45%, the pH value is 3.8~4.5, and the product has a shelf life of not less than 12 months at room temperature.

Images