Sugar-free polyphenol sugarcane-flavored water beverage as well as production process and production line thereof

Abstract

The invention relates to a sugar-free polyphenol sugarcane flavor water beverage, which is formed by mixing sugarcane aroma condensed raw water and sugarcane polyphenol raw water, and the production process comprises the following steps: squeezing sugarcane, filtering to obtain pretreated sugarcane juice, carrying out low-temperature high-vacuum distillation on the pretreated sugarcane juice, collecting condensed water, namely the sugarcane aroma condensed raw water, and simultaneously obtaining primary concentrated syrup; filtering the preliminarily concentrated syrup through a ceramic membrane, then adsorbing the preliminarily concentrated syrup through macroporous resin to obtain resin penetrating syrup and macroporous resin after adsorption, eluting the macroporous resin after adsorption with ethanol, and performing low-temperature high-vacuum distillation on eluent to remove ethanol to obtain sugarcane polyphenol raw water; and mixing the sugarcane aroma condensed raw water and the sugarcane polyphenol raw water. According to the present invention, the water content in the sugarcane is utilized at a high value, the processing additional value of the sugarcane resource is improved, the sugarcane polyphenol in the sugarcane is enriched and then added, the biological activity of the product is improved, and the prepared beverage has characteristics of no sugar, rich sugarcane characteristic aroma, rich sugarcane polyphenol, sugar control potential, clean ingredient and clean label.

Description

Technical Field

[0001] This invention relates to the field of beverages, specifically to a sugar-free polyphenol sugarcane-flavored water beverage and its production process and production line. Background Technology

[0002] Sugarcane (Saccharum officinarum L.) is an important sugar crop worldwide. Its stalks are pressed to extract juice, which is then purified, evaporated, crystallized, and separated to produce white sugar and raw sugar products. During this process, sucrose is effectively separated and purified, while non-sugar components (including organic acids, phenols, amino acids, minerals, and volatile flavor compounds), which account for approximately 10-15% of the dry matter in sugarcane juice, cannot be crystallized and are mostly discarded along with byproducts such as molasses and filter mud, resulting in low resource utilization.

[0003] Currently, commercially available sugarcane-flavored beverages (such as sugarcane juice drinks and sugarcane-flavored tea drinks) generally rely on the direct addition of sucrose or concentrated sugarcane juice and flavorings, resulting in high sugar content and complex ingredient lists, which do not meet the requirements of clean label consumers. With the upgrading of health-conscious eating demands, consumers' demand for sugar-free, naturally aromatic, clean-ingredient, and clean-label sugarcane beverages has increased significantly. However, existing technologies face the following bottlenecks: 1. Flavor and sugar coupling: Typical flavor compounds of sugarcane (such as volatile components like ketones and aldehydes) coexist with sucrose in the juice. Traditional sugar removal processes (such as multi-stage membrane filtration and concentration crystallization) lose a large amount of flavor compounds while removing sugar; 2. Heat-sensitive flavor loss: Many sugarcane flavor compounds are heat-instable, and conventional sterilization and concentration processes easily lead to aroma degradation; 3. Complex ingredient lists: Sugarcane flavorings and other food additives are added to maintain the sugarcane flavor; 4. Untapped value of sugarcane byproducts: Non-sugar components from sugar production are rich in natural flavor compounds and bioactive components, but there is a lack of targeted and efficient utilization technologies. Currently, there is no effective solution for the targeted preservation and enhancement of sugarcane characteristic flavors and bioactive components in sugarcane-flavored sugar-free liquid beverages. Therefore, there is an urgent need to develop a technology for the separation, enrichment, and stabilization of flavor and bioactive components based on non-sugar sugar components. This would overcome the technical contradiction of achieving both "sugar-free" and "flavor and activity retention," providing technical support for the production of sugar-free, naturally aromatic, clean-ingredient, and label-safe sugarcane beverages. Summary of the Invention

[0004] This invention addresses the shortcomings of existing technologies by providing a sugar-free polyphenol sugarcane-flavored water beverage and its production process. It makes high-value use of the water in sugarcane juice, increases the added value of sugarcane resource processing, and enhances the bioactivity of the product by enriching and re-adding sugarcane polyphenols. The result is a sugar-free beverage with a rich sugarcane aroma, rich in sugarcane polyphenols, with sugar control potential, and clean ingredients and labeling.

[0005] To achieve the above objectives, the present invention adopts the following technical solution: A sugar-free polyphenol sugarcane-flavored water beverage is made by mixing sugarcane aroma condensate and sugarcane polyphenol water. The sugarcane aroma condensate is the condensate obtained by low-temperature high-vacuum distillation of sugarcane juice. The sugarcane polyphenol water is the liquid phase obtained by removing ethanol from macroporous resin eluent by low-temperature high-vacuum distillation. The macroporous resin eluent is obtained by eluting and collecting macroporous resin after adsorbing sugarcane syrup with ethanol as the eluent.

[0006] A production process for a sugar-free polyphenol sugarcane flavored water beverage includes the following steps: (1) After pressing the sugarcane, filter it to obtain pretreated sugarcane juice. (2) Pretreated sugarcane juice is distilled at low temperature and high vacuum. The collected condensate is the sugarcane aroma condensate. At the same time, a preliminary concentrated syrup is obtained. (3) The preliminary concentrated syrup is filtered through a ceramic membrane. The ceramic membrane filtrate is adsorbed through a macroporous resin to obtain resin permeate syrup and adsorbed macroporous resin. (4) The adsorbed macroporous resin is first washed with water to remove impurities, and then eluted with ethanol. The eluent is collected. (5) After removing ethanol from the eluent by low temperature and high vacuum distillation, sugarcane polyphenol raw water is obtained. (6) Sugarcane aroma condensate and sugarcane polyphenol raw water are mixed to obtain a sugar-free polyphenol sugarcane flavored water beverage.

[0007] The production process of the sugar-free polyphenol sugarcane flavored water beverage is described above. In step (1), the material is filtered through a 20-300 mesh sieve; in step (2), the process parameters for the low-temperature high-vacuum distillation are a temperature below 65 ℃ and a pressure below 8000 Pa; the preliminary concentrated syrup is 30-50 °Brix; in step (3), the ceramic membrane has an average pore size of 50-500 nm and the macroporous resin is XAD-2, D101, HPD-100, or AB-8 resin; in step (4), the ethanol is 50-75% ethanol; in step (5), the process parameters for the low-temperature high-vacuum distillation are a temperature below 65 ℃ and a pressure below 25000 Pa.

[0008] In the production process of the sugar-free polyphenol sugarcane flavored water beverage, step (6) involves mixing sugarcane aroma condensed raw water and sugarcane polyphenol raw water at a weight ratio of 1:1000 to 1000:1.

[0009] The production process of the sugar-free polyphenol sugarcane flavored water beverage is described in which the 50-75% ethanol is obtained by diluting 95% or more ethanol with condensed sugarcane water, and the condensed sugarcane water is collected when the syrup is passed through a low-temperature high-vacuum distillation resin.

[0010] A sugar-free polyphenol sugarcane flavored water beverage production line includes a sugarcane aroma condensed raw water preparation unit, a sugarcane polyphenol raw water preparation unit, and a mixing unit. The outlet of the sugarcane aroma condensed raw water preparation unit is connected to the inlet of the mixing unit, and the outlet of the sugarcane polyphenol raw water preparation unit is connected to the inlet of the mixing unit.

[0011] The sugar-free polyphenol sugarcane flavored water beverage production line includes a sugarcane aroma condensate preparation unit comprising a sugarcane juice preliminary filtration device, a first low-temperature high-vacuum distillation device, and a sugarcane aroma condensate storage tank. The outlet of the sugarcane juice preliminary filtration device is connected to the inlet of the first low-temperature high-vacuum distillation device, the steam outlet of the first low-temperature high-vacuum distillation device is connected to the inlet of the sugarcane aroma condensate storage tank, and the outlet of the sugarcane aroma condensate storage tank is connected to the inlet of the mixing unit.

[0012] The sugar-free polyphenol sugarcane flavored water beverage production line includes a sugarcane polyphenol raw water preparation unit comprising a sugarcane juice preliminary filtration device, a first low-temperature high-vacuum distillation device, a ceramic membrane module, a resin adsorption module, a first ethanol storage tank, a third low-temperature high-vacuum distillation device, and a sugarcane polyphenol raw water storage tank. The outlet of the sugarcane juice preliminary filtration device is connected to the inlet of the first low-temperature high-vacuum distillation device. The liquid phase outlet of the first low-temperature high-vacuum distillation device is connected to the syrup inlet of the ceramic membrane module. The syrup outlet of the ceramic membrane module is connected to the syrup inlet of the resin adsorption module. The outlet of the first ethanol storage tank is connected to the eluent inlet of the resin adsorption module. The eluent outlet of the resin adsorption module is connected to the inlet of the third low-temperature high-vacuum distillation device. The liquid phase outlet of the third low-temperature high-vacuum distillation device is connected to the inlet of the sugarcane polyphenol raw water storage tank. The outlet of the sugarcane polyphenol raw water storage tank is connected to the inlet of the mixing unit.

[0013] The sugar-free polyphenol sugarcane flavored beverage production line further includes a resin-permeable syrup storage tank, a second low-temperature high-vacuum distillation device, and a condensed sugarcane water storage tank. The syrup outlet of the resin adsorption component is connected to the inlet of the resin-permeable syrup storage tank, the outlet of the resin-permeable syrup storage tank is connected to the syrup inlet of the second low-temperature high-vacuum distillation device, the steam outlet of the second low-temperature high-vacuum distillation device is connected to the inlet of the condensed sugarcane water storage tank, and the outlet of the condensed sugarcane water storage tank is connected to the inlet of the first ethanol storage tank.

[0014] In the sugar-free polyphenol sugarcane flavored water beverage production line, a preliminary concentrated syrup storage tank is provided between the first low-temperature high-vacuum distillation device and the ceramic membrane module. The liquid phase outlet of the first low-temperature high-vacuum distillation device is connected to the inlet of the preliminary concentrated syrup storage tank, and the outlet of the preliminary concentrated syrup storage tank is connected to the syrup inlet of the ceramic membrane module. An eluent storage tank is provided between the resin adsorption module and the third low-temperature high-vacuum distillation device. The eluent outlet of the resin adsorption module is connected to the inlet of the eluent storage tank, and the outlet of the eluent storage tank is connected to the inlet of the third low-temperature high-vacuum distillation device.

[0015] The sugar-free polyphenol sugarcane flavored water beverage production line further includes a filling and packaging unit and a sterilization component; the outlet of the mixing unit is connected to the inlet of the filling and packaging unit, and the outlet of the filling and packaging unit is connected to the sterilization component; or, the outlet of the mixing unit is connected to the inlet of the sterilization component, and the outlet of the sterilization component is connected to the filling and packaging unit.

[0016] In step (6), after mixing, the mixture is sterilized and then filled and packaged, or filled and packaged and then sterilized, to obtain the finished sugar-free polyphenol sugarcane flavored water beverage.

[0017] Eluent refers to the solvent system flowing through the stationary phase (such as macroporous resin) to desorb the target substance adsorbed on the stationary phase. Eluent is the solution containing the eluted target substance that flows out of the chromatography column.

[0018] The sugarcane juice preliminary filtration device includes a sugarcane pressing device and a filtration device connected in sequence.

[0019] Compared with existing technologies, this invention offers the following advantages: Compared to multi-stage membrane treatment technologies, this invention requires less equipment investment. Employing aroma recovery and simultaneous distillation and sugar-water separation technology, the product exhibits a richer sugarcane aroma compared to conventional methods. Compared to the high operating pressure and energy consumption of reverse osmosis, this invention does not use reverse osmosis to separate sugar water, resulting in lower production costs. Furthermore, while reverse osmosis technology not only separates sucrose and water but also retains most sugarcane polyphenols, this solution employs a concentration-enrichment-re-addition technique, increasing the total polyphenol content in the product by 11.39% compared to sugarcane juice, and the total flavonoid content by 7.80%. The sugarcane polyphenol content far exceeds that of commercially available products, exhibiting stronger biological activity and potential for sugar control. Compared to ozone pre-oxidation treatment of sugarcane plant water, which oxidizes and destroys flavor substances and polyphenols, this solution's sugarcane water beverage is not only sugar-free and has a rich sugarcane aroma but is also rich in sugarcane polyphenols, possessing sugar control potential. It also features clean ingredients and meets food hygiene labeling requirements. More than 60% of the plant water in sugarcane juice can be utilized in a high-value manner, thereby increasing the added value of sugarcane resource processing. Attached Figure Description

[0020] Figure 1 This is a process flow diagram of the production process of the sugar-free polyphenol sugarcane flavored water beverage.

[0021] Figure 2 The total ion chromatogram (TIC chromatogram) of the four-stage samples is shown.

[0022] Figure 3 This represents the common volatile compound information for the four-stage samples.

[0023] Figure 4 Sensor response radar plots for volatile compounds in four-stage samples obtained by electronic nose measurement.

[0024] Figure 5 This is a standard curve prepared based on the absorbance and concentration of gallic acid series standard working solutions.

[0025] Figure 6 A standard curve was prepared based on the absorbance and concentration of the rutin series standard working solutions.

[0026] Figure 7 A standard curve was prepared based on the absorbance and concentration of fructose series standard working solutions.

[0027] Figure 8 A standard curve was prepared based on the absorbance and concentration of a series of glucose standard working solutions.

[0028] Figure 9 A standard curve was prepared based on the absorbance and concentration of the sucrose series standard working solutions.

[0029] Figure 10 This is a schematic diagram of the equipment connection for a sugar-free polyphenol sugarcane flavored beverage production line. In the diagram, the components are: 1. Sugarcane juice preliminary filtration device; 2. First low-temperature high-vacuum distillation device; 3. Preliminary concentrated syrup storage tank; 4. Ceramic membrane assembly; 5. Resin adsorption assembly; 6. Resin permeation syrup storage tank; 7. Second low-temperature high-vacuum distillation device; 8. White sugar production line; 9. Condensed sugarcane water storage tank; 10. First ethanol storage tank; 11. Eluent storage tank; 12. Third low-temperature high-vacuum distillation device; 13. Sugarcane polyphenol raw water storage tank; 14. Mixing unit; 15. Filling and packaging unit; 16. HPP sterilization assembly; 17. Sugarcane aroma condensed raw water storage tank; and 18. Second ethanol storage tank. Detailed Implementation

[0030] The technical solution of the present invention will be further illustrated below through embodiments.

[0031] First, Example 1 provides a specific method for a single production process; second, Examples 2 and 3 conduct detailed studies on the effect of maintaining sugarcane flavor in intermediate products and final products during the production process; third, Examples 4-6 conduct detailed studies on the extraction of polyphenols from sugarcane and their contribution to the blood sugar control ability of the final product; fourth, Example 7 measures the sugar content of the three-stage products; Examples 8 and 9 provide two production lines for implementing the production process described in Example 1.

[0032] Example 1: Production process of sugar-free polyphenol sugarcane water beverage A production process for the aforementioned sugar-free polyphenol sugarcane flavored water beverage, the process flow diagram is as follows: Figure 1 As shown, the specific steps are as follows: 1. Preparation of pretreated sugarcane juice: Sugarcane juice is extracted and filtered through a 200-mesh screen to obtain pretreated sugarcane juice for later use.

[0033] 2. Pre-treated sugarcane juice distillation: The pre-treated sugarcane juice is placed in the first low-temperature vacuum distillation apparatus for distillation and separation. The equipment parameters are: 60 ℃, 4000 Pa. The distillation ends when the pre-treated sugarcane juice is concentrated to 40 °Brix. The sugarcane aroma condensate is recovered from the distillation, and 40 °Brix syrup is obtained for later use.

[0034] Note: 100 kg of sugarcane juice yields approximately 50 kg of sugarcane aroma condensate and 50 kg of 40 ° Brix syrup.

[0035] 3. Ceramic membrane filtration: 40 ° Brix syrup was filtered through a 50 nm ceramic membrane, and the ceramic membrane filtrate was collected for later use.

[0036] 4. Resin adsorption: ① Preparation of chromatography column: The chromatography column is packed with XAD-2 macroporous resin with a diameter-to-height ratio of 1:7.5; ② Adsorption: The ceramic membrane filtrate is adsorbed through XAD-2 macroporous resin. Parameters: sample loading flow rate 1.5 BV / h. The resin is collected and permeated with syrup for later use.

[0037] 5. Resin permeation through syrup distillation: The resin is permeated through the syrup and placed in a second low-temperature vacuum distillation apparatus for distillation. The equipment parameters are: 60 ℃, 4000 Pa. The distillation ends when the syrup is concentrated to 65 °Brix. The distilled condensed sugarcane water is recovered, and 65 °Brix syrup is obtained for the production of sulfur-free sugar.

[0038] 6. Prepare the eluent: Dilute 95% ethanol to 60% ethanol with condensed sugarcane water.

[0039] 7. Desorption: ① Water washing to remove impurities: Rinse the adsorbed XAD-2 macroporous resin with pure water at a rate of 2 BV / h for 1.0 h to remove excess syrup from the resin; ② Desorption: Elute the water-washed XAD-2 macroporous resin with 60% ethanol at a rate of 2 BV / h for 3 h, and collect all the eluent.

[0040] 8. Eluent distillation: The eluent is placed in the third low-temperature vacuum distillation apparatus for distillation. The equipment parameters are: 60 ℃, 19000 Pa. Distillation is completed when all the ethanol in the eluent has been evaporated. The liquid phase is the raw water containing sugarcane polyphenols. Note: 50 kg of 40 °Bx sugarcane syrup produces approximately 14 kg of sugarcane polyphenol-rich water. In this step, by controlling the vacuum and temperature, conditions are created where ethanol boils while water barely boils (or boils very slowly), allowing ethanol to continuously evaporate and be removed until no ethanol is detected in the liquid phase. Distillation is stopped when the water in the liquid phase is found to contain no ethanol, as determined by an alcohol meter.

[0041] 9. Mixing: Mix the sugarcane aroma condensate and sugarcane polyphenol condensate at a volume ratio of 3:1 to obtain sugar-free polyphenol sugarcane flavored water for later use.

[0042] 10. Bottling and HPP sterilization: After bottling the sugar-free polyphenol sugarcane flavored water, it enters the HPP ultra-high pressure sterilization equipment with parameters of 600 MPa for 5 minutes.

[0043] 11. Finished product: Bottled sugar-free polyphenol sugarcane flavored water sterilized by HPP ultra-high pressure, which is then labeled and coded to obtain the finished sugar-free polyphenol sugarcane flavored water beverage.

[0044] During the production process according to the above method, samples were taken from the pretreated sugarcane juice obtained in step 1, numbered DFGZZWS_1; samples were taken from the sugarcane aroma condensate obtained in step 2, numbered DFGZZWS_2; samples were taken from the 40 °Bx sugarcane syrup, numbered DFGZZWS_3; samples were taken from the finished sugar-free polyphenol sugarcane flavored water beverage obtained in step 11, numbered DFGZZWS_4; and samples were taken from the sugarcane polyphenol condensate obtained in step 8, numbered DFGZZWS_5.

[0045] Example 2 Characteristic Aroma Analysis 1. Introduction to the Experiment The HS-SPME-OrbitrapExploris GC / MS analysis platform was used to analyze the volatile aroma compounds in the four-stage samples collected in Example 1. The volatile substances were qualitatively identified by matching the NIST-2023 database, the gc-orbitrap flavorandfragrances v1.0 database, and the database built by Shanghai Meiji, and the retention index (RI). The volatile substances were quantitatively identified by the internal standard method, and the information data of volatile aroma compounds were finally obtained.

[0046] 2. Main equipment and reagents NewClassic MS electronic balance (manufacturer METTLERTOLEDO, model NewClassicMFMS105DU); Gas chromatograph-mass spectrometer (manufacturer Thermo, Germany, model OrbitrapExplorisGC).

[0047] 3. Experimental Methods 3.1 Preparation of n-alkane standard solution: Take 770 μL of n-hexane and transfer it to a 1.5 mL centrifuge tube. Add appropriate amounts of C10-C25 commercial mixed standard, C26, C27, C28, and C29 n-alkane standards sequentially, and vortex to mix well to obtain a mixed standard stock solution of C10-C29 n-alkanes (50 μg / mL). Dilute the above stock solution to 10 μg / mL and analyze it in the same batch as the sample.

[0048] 3.2 Sample pretreatment: Take 0.5 mL of sample and place it in a 20 mL headspace vial. Add 2.5 µL of internal standard (naphthalene-d820 µg / mL, n-pentadecane-d3250 µg / mL) and 4 mL of saturated sodium chloride aqueous solution, and seal the headspace vial immediately.

[0049] 3.3 SPME conditions: Extraction head SPMEArrowFiber (120 μm, Thermo, DVB / CarbonWR / PDMS); extraction head aging time 20 min, aging temperature 240℃; incubation and extraction temperature 80℃, incubator shaking speed 500 rpm, incubation time 20 min; extraction stirrer speed 200 rpm, extraction time 10 min; desorption time 5 min.

[0050] 3.4 Chromatographic conditions: Samples were injected into the GC-MS system in split mode with a split ratio of 10:1. After separation on a VF-WAXms capillary column (25 m × 0.25 mm × 0.2 µm, Agilent CP9204), samples were detected by mass spectrometry. The injection port temperature was 240 ℃, the carrier gas was high-purity helium at a flow rate of 1.0 mL / min, and the septum purge flow rate was 3 mL / min. Temperature program: initial temperature 40 ℃, increased to 120 ℃ at a rate of 8 ℃ / min, then increased to 230 ℃ at a rate of 20 ℃ / min and held for 4.5 min, for a total run time of 20 min.

[0051] 3.5 Mass spectrometry conditions: Scan mode: FullScan; Scan range (m / z): 35-500; Resolution: 30000; Ion source temperature (°C): 250; Ion source type: EI; Repulsion electrode (V): 10; Default ion source voltage (V): 5; Lens 1 (V): -50; Lens 2 (V): -0.5; Lens 3 (V): -35; Electron lens (V): 15; Electron energy (eV): 70; Emission current (μA): 50.

[0052] 4. Experimental Results 4.1 Total Ion Chromatogram: The components eluted from the sample after chromatographic separation continuously enter the mass spectrometer. Data is acquired through continuous mass spectrometry scanning, with each scan yielding a mass spectrum. The total ion intensities are summed from all mass spectra to obtain a total ion current intensity, such as... Figure 2 As shown, the total ion chromatogram is plotted with time on the x-axis and the sum of ion intensities on the y-axis.

[0053] 4.2 Types of volatile substances: A total of 226 volatile substances were detected in the four-stage samples. The types of volatile substances are shown in Table 1 (Note: blank cells in the table indicate no detection). It can be seen that DFGZZWS_1 detected 191 types, DFGZZWS_2 detected 179 types, DFGZZWS_3 detected 156 types, and DFGZZWS_4 detected 176 types.

[0054] Table 1. Types of volatile substances in the four-stage samples

[0055] 4.3 Common Situation of Volatile Compounds Figure 3The common volatile compounds among the four-stage samples are as follows: 117 volatile compounds are common to the four-stage samples. DFGZZWS_2, DFGZZWS_4 and DFGZZWS_1 have 166 and 159 common volatile compounds, respectively. DFGZZWS_3 and DFGZZWS_1 have 137 common volatile compounds. The types of volatile compounds in DFGZZWS_2 and DFGZZWS_4 are closer to those in DFGZZWS_1 than in DFGZZWS_3.

[0056] 4.4 Overall analysis of all volatile compounds All volatile compounds in the four-stage samples were classified into 11 categories for overall analysis, including 34 esters, 39 alcohols, 34 hydrocarbons, 26 ketones, 24 terpenes, 23 organic heterocyclic compounds, 22 aldehydes, 10 phenols, 8 other compounds, 4 nitrogen-containing organic compounds, and 2 acids. As shown in Table 2, the volatile components of the four-stage samples mainly consisted of esters, alcohols, and aldehydes. The relative contents of esters in DFGZZWS_1 were 57.84%, aldehydes 9.27%, and alcohols 15.14%; in DFGZZWS_3, the relative contents of esters were 69.31%, aldehydes 4.18%, and alcohols 11.68%; and in DFGZZWS_4, the relative contents of esters were 60.28%, aldehydes 10.12%, and alcohols 17.70%. Compared to DFGZZWS_3, DFGZZWS_4 and DFGZZWS_1 have relatively similar contents of esters, aldehydes and alcohols.

[0057] Table 2. Relative contents (%) of 11 types of volatile substances in the four-stage samples.

[0058] 4.5 Odor Activity Value Odor Activity Value (OAV) is an important indicator for measuring the contribution of volatile compounds to the overall odor of food. A higher OAV indicates a greater contribution to odor. Volatile components with an OAV ≥ 1 are considered to play a key role in overall aroma, while those with an OAV ≥ 0.1 (1 > OAV) are considered to play a key modifying role. The OAV value is calculated as the ratio of the content of an odor component in the food to the odor threshold of that component. The calculation formula is as follows:

[0059] In the formula: A The compounds in the sample to be tested; T The odor threshold of this compound in aqueous medium (unit: same concentration unit, database needs to be consulted). CThe concentration of the compound in the sample to be tested (unit: μg / kg or μg / L).

[0060] As shown in Table 3, DFGZZWS_1 contains 12 volatile compounds with odor activity values ​​greater than 1, namely: damascene, 1-octen-3-one, trans-cis-2,6-nonadienal, 2,4- Nonadienal, 2,4-decadienal, dodecanal, β-ionone, nonanal, octanal, guaiacol, hexanal, and phenylacetaldehyde, including 8 aldehydes, 2 ketones, 1 terpene, and 1 phenol, are the main material basis for the characteristic aroma of sugarcane juice and make significant contributions to its presentation. DFGZZWS_1 contains 8 volatile compounds with odor activity values ​​less than 1 and greater than or equal to 0.1, namely methyl 2-methylbutyrate, 1-octen-3-ol, butyl acetate, pentanal, heptanal, cis-5-octen-1-ol, p-cymene, and 2-acetylthiazole. These compounds play a key modifying role in the presentation of the characteristic aroma of sugarcane juice and effectively increase its aroma richness. The number and types of volatile compounds with an odor activity value greater than 1 in DFGZZWS_4 are consistent with those in DFGZZWS_1. There are 7 volatile substances with an odor activity value less than 1 and greater than or equal to 0.1, namely methyl 2-methylbutyrate, 1-octen-3-ol, butyl acetate, pentanal, cis-5-octen-1-ol, 2-acetylthiazole, and decanal. Compared with DFGZZWS_1, it lacks heptanal (the heptanal OAV of DFGZZWS_4 is 0.04, presenting a citrus and grassy aroma) and p-cymene (the heptanal OAV of DFGZZWS_4 is 0.05, presenting a citrus and woody aroma), and has added decanal (presenting a citrus and sweet aroma). The aroma properties of these three volatile compounds are all citrus freshness, and they have similar effects in modifying the characteristic aroma of sugarcane juice. In summary, DFGZZWS_4 and DFGZZWS_1 have similar aroma characteristics.

[0061] Table 3. OAV values ​​and odor characteristics of major volatile aroma compounds.

[0062] Example 3: Electronic nose measurement Odor analysis of four-stage samples was performed using the ODP3 electronic nose system (Gerstel, Germany). Method: 6.00 g of sample was placed in a 30 ml headspace vial, 0.6 g of electrolyte NaCl was added, the vial was tightly capped, and the vial was incubated in a 50 ℃ water bath for 20 min before immediate detection. Data acquisition time was 120 s, with clean, dry air as the carrier gas. Needle cleaning time was 100 s. Each sample was collected three times, and the three data points after stabilization were used. Results are shown below. Figure 4It can be seen that sensors R(7), R(4), and R(3) have high response values ​​to the volatile odors of the four samples. The odor radar response curves of DFGZZWS_4 and DFGZZWS_1 have a high degree of overlap, indicating that their overall volatile odors are similar and their aroma characteristics are similar.

[0063] Example 4: Study on total polyphenol content Principle: Phenolic compounds are oxidized by Folin-Ciocalteu under alkaline conditions to produce a blue compound. Within a certain concentration range, the absorbance is directly proportional to the content of the phenolic compound, conforming to the Lambert-Beer Law. Instruments: UV-Vis spectrophotometer, analytical balance. Reagents: Unless otherwise specified, all reagents used in this example are analytical grade; Preparation of 7% sodium carbonate solution: Weigh 7 g (accurate to 0.01 g) of anhydrous sodium carbonate, dissolve in water, and bring the volume to 100 mL; Preparation of gallic acid standard stock solution (200 mg / L): Accurately weigh 20 mg (accurate to 0.1 mg) of gallic acid standard, dissolve in water, and bring the volume to 100 mL, then shake well. Prepare fresh before use and store protected from light.

[0064] Gallic acid standard working solutions: Accurately pipette 0 mL, 0.04 mL, 0.08 mL, 0.12 mL, 0.16 mL, and 0.20 mL of gallic acid standard stock solution, respectively, and add water to a final volume of 0.20 mL. Shake well to prepare a series of standard working solutions with concentrations of 0 mg / L, 40 mg / L, 80 mg / L, 120 mg / L, 160 mg / L, and 200 mg / L. Prepare fresh solutions before use.

[0065] Sample preparation: Weigh 5.5 g (accurate to 0.1 mg) of sample into a volumetric flask, add water to make up to volume and mix well, ready for testing.

[0066] Assay method: Accurately pipette 0.2 mL each of gallic acid series standard working solutions and sample solutions into graduated test tubes. Add 1.8 mL of distilled water and 0.2 mL of Folin-Ciocalteu reagent to each test tube, shake well, and allow to react for 5 min. When the color in the test tube turns light green, add 2 mL of 7% sodium carbonate solution and 0.8 mL of distilled water, and shake well. Let stand at room temperature for 90 min, and measure the absorbance at 750 nm using a spectrophotometer with a 10 mm cuvette. Construct a standard curve based on the absorbance (A) and concentration of the gallic acid series standard working solutions, see [reference needed]. Figure 5 The total polyphenol content (calculated as gallic acid) is calculated using the following formula:

[0067] In the formula: X The total polyphenol content in the sample (calculated as gallic acid) is expressed in grams per kilogram (g / kg).C The concentration of gallic acid in the test solution, calculated from the standard curve, is expressed in milligrams per liter (mg / L). V The volume is constant, and the unit is milliliters (mL). K This refers to the sample dilution factor. m The sample size is expressed in grams (g); 1000 is the conversion factor from milliliters (mL) to liters (L).

[0068] The results are shown in Table 4. (1) If 100 kg of pretreated sugarcane juice is used for subsequent production, 14 kg of sugarcane polyphenol raw water is obtained. The total polyphenol content in 100 kg of pretreated sugarcane juice is 55.3 g, and the total polyphenol content in 14 kg of sugarcane polyphenol raw water is 34.636 g. The total polyphenol extraction rate is 62.63%. (2) The total polyphenol content in the sugar-free polyphenol sugarcane flavored water beverage prepared by concentration and mixing is 0.616 g / kg, which is 11.39% higher than the total polyphenol content of 0.553 g / kg in pretreated sugarcane juice.

[0069] Table 4. Results of total polyphenol content determination

[0070] Example 5: Study on total flavonoid content Principle: After pretreatment to remove impurities, the sample is extracted with methanol or 60% ethanol solution to extract flavonoids. The flavonoids can be reduced by sodium nitrite and form a complex with aluminum nitrate. Under alkaline conditions of sodium hydroxide solution, the complex opens to form 2-hydroxychalcone, which gives the solution a characteristic orange-red color. The absorbance is measured at a wavelength of 510 nm using spectrophotometry. Rutin is used as a reference standard, and the total flavonoid content in the sample is calculated using the standard curve method. Reagents: Unless otherwise specified, all reagents used in this embodiment are of analytical grade; 5% sodium nitrite solution: Weigh 5.0 g of sodium nitrite and dissolve in water to make 100 mL; 10% aluminum nitrate solution: Weigh 17.6 g of aluminum nitrate and dissolve in water to make 100 mL; Sodium hydroxide test solution: Weigh 4.3 g of sodium hydroxide and dissolve in water to make 100 mL; 60% ethanol: Measure 60 mL of anhydrous ethanol and add water to make 100 mL; Rutin standard stock solution: Accurately weigh 20 mg (accurate to 0.01 mg) of rutin standard sample after constant weight in an oven at 102 ℃, dissolve in methanol, and transfer to a 100 mL volumetric flask, then dilute to the mark. The concentration of this solution is 0.2 mg / mL.

[0071] Sample preparation: Accurately pipette an appropriate amount of the sample into a 25 mL volumetric flask, add 60% ethanol to dissolve and dilute to the mark, shake well, and use as the test solution.

[0072] Preparation of the standard curve: Accurately pipette 0.0, 1.0, 2.0, 3.0, 4.0, 5.0, and 6.0 mL of rutin standard stock solution into 25 mL volumetric flasks, add water to 6 mL, add 1 mL of 5% sodium nitrite solution, shake well, and let stand for 6 min. Add 1 mL of 10% aluminum nitrate solution, shake well, and let stand for 6 min. Add 10 mL of sodium hydroxide solution, shake well, add water to the mark, shake well, and let stand for 15 min to prepare a series of standard working solutions with rutin concentrations of 0.0 μg / mL, 8.0 μg / mL, 16 μg / mL, 24 μg / mL, 32 μg / mL, 40 μg / mL, and 48 μg / mL. Use the solvent prepared from 0.0 mL of the standard stock solution as a blank, and measure the absorbance at a wavelength of 510 nm. Plot the standard curve with absorbance as the ordinate and the standard concentration as the abscissa. See [reference needed]. Figure 6 .

[0073] Determination of the sample solution: Accurately pipette 2 mL of the test solution into a 25 mL volumetric flask; add water to 6 mL, add 1 mL of 5% sodium nitrite solution, shake well, let stand for 6 min, add 1 mL of 10% aluminum nitrate solution, shake well, let stand for 6 min, add 10 mL of sodium hydroxide solution, shake well, add water to the mark, shake well, let stand for 15 min, and measure the absorbance at 510 nm. Read the concentration of total flavonoids in the test solution from the standard curve, and calculate the total flavonoid content in the sample. The total flavonoid content in the sample is calculated using the following formula:

[0074] In the formula: X The total flavonoid content in the sample is expressed as rutin (C 27 H 30 O 16 ) is calculated in g / 100g; C The concentration of total flavonoids in the test solution is read from the standard curve, in mg / mL. V 1 represents the final volume of the sample, in milliliters (mL). V 2 represents the volume of the sample solution taken, in milliliters (mL); V 3 represents the volume of the colorimetric final volume, in milliliters (mL); M The sample size is expressed in grams (g). The calculation result is expressed as the arithmetic mean of two independent determinations obtained under repeatability conditions.

[0075] The results are shown in Table 5. It can be seen that (1) if 100 kg of pretreated sugarcane juice is used for subsequent production, 14 kg of sugarcane polyphenol raw water is obtained. The total flavonoid content in 100 kg of pretreated sugarcane juice is 48.7 g, and the total flavonoid content in 14 kg of sugarcane polyphenol raw water is 29.764 g, with a total flavonoid extraction rate of 61.12%; (2) the total flavonoid content in the sugar-free polyphenol sugarcane flavored water beverage prepared by concentration and mixing is 0.0525 g / 100g, which is 7.80% higher than the total flavonoid content of 0.0487 g / 100g in pretreated sugarcane juice.

[0076] Table 5 Results of total flavonoid content determination

[0077] Example 6: Study on the ability of in vitro enzymes to inhibit glucose-related enzyme activity Carbohydrate hydrolysis is the main source of blood glucose, and the main hydrolytic enzymes are α-amylase and α-glucosidase. α-amylase can randomly hydrolyze the α-1,4-glycosidic bonds within starch molecules to produce dextrins, oligosaccharides, and glucose. α-glucosidase can further promote the breaking of glucosidic bonds in dextrins and oligosaccharides, releasing more glucose. Inhibiting the activity of these two hydrolytic enzymes slows down the digestion and breakdown of carbohydrates, thereby reducing the rate at which glucose enters the bloodstream, and is considered an important way to control postprandial hyperglycemia. Researching the ability of sugar-free polyphenol-flavored sugarcane water to inhibit the activity of α-amylase and α-glucosidase can provide basic data for the development and utilization of sugar-free polyphenol-flavored sugarcane water.

[0078] Reagents: PBS solution: NaCl 8 g / L, KCl 0.2 g / L, Na₂HPO₄ 1.42 g / L, KH₂PO₄ 0.27 g / L, adjust pH to 7.4, add deionized water to a final volume of 1 L, autoclave at 121ºC for 20 min, and store at room temperature. 0.5 mmol / L PNPG solution: Weigh 0.0251 g of p-nitrophenyl-α-D glucoside (molecular weight 401.38 g / mol) and dissolve in 50 ml of sterile water. Filter the PNPG solution through a 0.22 μm filter. 1 mol / L Na₂CO₃: Weigh 106 g of Na₂CO₃ and bring the volume to 1 L. 1% (w / v) starch solution: Add 1 g of starch to sterile water and bring the volume to 100 L. Boil in a water bath for 30 min. DNS solution: Weigh 800 g of potassium sodium tartrate, 2 g of anhydrous sodium sulfite, and 40 g of 3,5-dinitrosalicylic acid into a graduated cylinder, add deionized water to dissolve, and add 80 g of sodium hydroxide while stirring. Stir magnetically overnight, add 8 g of redistilled phenol, and after it is completely dissolved, filter and make up to 4 L. Store in a brown bottle protected from light for one week until the solution is stable before use.

[0079] Method for determining α-glucosidase inhibitory activity: Take 500 μL of serially diluted sample into a 2 mL EP tube, add 500 μL of 10 U / mL α-glucosidase solution (pH 6.8, prepared with 0.1 mol / L PBS), and incubate at 37 ℃ for 10 min. Then add 500 μL of 0.5 mmol / L PNPG solution, incubate at 37 ℃ for 20 min, place in an ice-water bath for 5 min to reduce enzyme activity, and finally add 500 μL of 1 mol / L Na₂CO₃ to terminate the reaction. Measure the absorbance at 405 nm. Calculate the α-glucosidase inhibition rate using the following formula:

[0080] In the formula, A a The absorbance of the sample group. A b The absorbance of the sample background group (using an equal volume of buffer solution instead of enzyme solution) A c The absorbance is for the control group (equal volume of buffer solution instead of sample solution). A d The absorbance of the background control group is used as a reference (equal volume of buffer solution is used to replace the sample and enzyme solution).

[0081] Method for determining α-amylase inhibitory activity: Take 500 μL of serially diluted sample into a centrifuge tube, add 500 μL of 10 U / mL α-amylase solution (pH 7, prepared with 0.1 mol / L PBS), and incubate at 37 ℃ for 10 min. Then add 100 μL of 1% starch solution, incubate at 37 ℃ for 20 min, incubate in an ice-water bath for 5 min, add 100 μL of DNS, incubate in a boiling water bath for 5 min, cool, and then add 5 mL of PBS to make up the volume. Measure the absorbance at 540 nm. Calculate the α-amylase activity inhibition rate using the following formula:

[0082] In the formula, A a The absorbance of the sample group. A b The absorbance of the sample background group (using an equal volume of buffer solution instead of enzyme solution) A c The absorbance is for the control group (equal volume of buffer solution instead of sample solution). A d The absorbance of the background control group is used as a reference (equal volume of buffer solution is used to replace the sample and enzyme solution).

[0083] Experimental Results and Analysis: The results of the α-glucosidase inhibitory activity experiment in this embodiment are shown in Table 6. The inhibition rate of 57.10% indicates that more than half of the enzyme activity was blocked. The results of the α-amylase inhibitory activity experiment are shown in Table 7. The inhibition rate of 34.32% indicates that approximately one-third of the enzyme activity was blocked. In conclusion, the sugar-free polyphenol sugarcane-flavored water beverage has the potential to regulate blood sugar.

[0084] Table 6 α-Glucosidase Inhibitory Activity

[0085] Table 7 α-Amylase Inhibitory Activity

[0086] Example 7 Study on the content of fructose, glucose and sucrose Weigh 10 g (accurate to 0.001 g) of the sample into a 100 mL volumetric flask, add about 50 mL of water, then slowly add 5 mL of zinc acetate solution and 5 mL of potassium ferrocyanide solution, add water to make up to the mark, sonicate for 30 min, filter with dry filter paper, discard the initial filtrate, and filter the subsequent filtrate through a 0.45 μm aqueous filter membrane into a sample vial for analysis by high performance liquid chromatography.

[0087] Chromatographic conditions: Column: amino column, length 250 mm, inner diameter 4.6 mm; Mobile phase: acetonitrile + water = 70 + 30 (v / v); Flow rate: 1.0 mL / min; Column temperature: 40 ℃; Injection volume: 20 μL. Differential refractive index detector conditions: temperature 40 ℃.

[0088] Sugar standard stock solution (20 mg / mL): Weigh 1 g each of fructose, glucose and sucrose standards that have been dried at 96℃±2℃ for 2 h, add water to make up to 50 ml, and store in a sealed container at 4℃.

[0089] Sugar standard working solution: Pipette 1.00 mL, 2.00 mL, 3.00 mL, and 5.00 mL of sugar standard stock solution into 10 mL volumetric flasks and dilute to volume with water, which are equivalent to standard solutions with concentrations of 2.0 mg / mL, 4.0 mg / mL, 6.0 mg / mL, and 10.0 mg / mL, respectively.

[0090] Preparation of the standard curve: Measure the sugar standard solutions using an instrument and record the peak areas of fructose, glucose, and sucrose. Plot the standard curve using a linear equation, with the concentration of the standard working solution on the x-axis and the peak area on the y-axis. See the fructose standard curve below. Figure 7 The glucose standard curve is shown below. Figure 8 The sucrose standard curve is shown below. Figure 9 .

[0091] Determination of sample solution: Inject the sample solution into the high-performance liquid chromatograph, record the peak area, and calculate the concentrations of fructose, glucose, and sucrose in the sample solution based on the standard curve. Blank test: Perform the above steps except without adding a sample.

[0092] The contents of fructose, glucose, and sucrose in the sample are calculated using the following formula:

[0093] In the formula: X The content of fructose, glucose, and sucrose in the sample is expressed in grams per 100 grams (g / 100g). ρ The concentrations of fructose, glucose, and sucrose in the sample solution obtained from the standard curve are expressed in milligrams per milliliter (mg / mL). ρ 0 represents the concentrations of fructose, glucose, and sucrose in the blank obtained from the standard curve, in milligrams per milliliter (mg / mL). V This is the fixed volume, expressed in milliliters (mL). f This refers to the dilution factor; m The sample weight is expressed in grams (g); 1000 is the conversion factor; 100 is the conversion factor.

[0094] The test results are shown in Table 8-10. The total sugar content of the sugarcane aroma condensate and sugarcane polyphenol condensate was 0.268 g / 100 g (of which sucrose content was 0.268 g / 100 g, and fructose and glucose content were both 0) and 0.722 g / 100 g (of which sucrose, fructose and glucose contents were 0.489 g / 100 g, 0.138 g / 100 g and 0.095 g / 100 g, respectively), which were extremely low. Sugar-free polyphenols... The total sugar content of the finished sugarcane-flavored beverage is 0.387g / 100g (of which sucrose, fructose, and glucose content are 0.315g / 100g, 0.044g / 100g, and 0.028g / 100g, respectively), which is lower than the requirement of GB28050 "General Rules for Nutrition Labelling of Prepackaged Foods" for sugar-free beverages with a content of ≤0.5g / 100g. Therefore, the finished sugar-free polyphenol sugarcane-flavored beverage is indeed a sugar-free beverage. Combined with the results of Examples 2-7, this demonstrates that the beverage obtained by this invention not only retains the sugarcane flavor but also fully preserves the polyphenols in sugarcane, achieving sugar-free status and possessing the potential to regulate blood sugar.

[0095] Table 8 Results of Fructose Content Determination

[0096] Table 9. Results of glucose content determination

[0097] Table 10 Results of sucrose content determination

[0098] Example 8 A sugar-free polyphenol sugarcane flavored water beverage production line includes a sugarcane aroma condensed raw water preparation unit, a sugarcane polyphenol raw water preparation unit, and a mixing unit. The outlet of the sugarcane aroma condensed raw water preparation unit is connected to the inlet of the mixing unit 14, and the sugarcane polyphenol raw water preparation unit is connected to the inlet of the mixing unit 14.

[0099] The sugarcane aroma condensate preparation unit includes a sugarcane juice preliminary filtration device 1, a first low-temperature high-vacuum distillation device 2, and a sugarcane aroma condensate storage tank 17. The outlet of the sugarcane juice preliminary filtration device 1 is connected to the inlet of the first low-temperature high-vacuum distillation device 2, the steam outlet of the first low-temperature high-vacuum distillation device 2 is connected to the inlet of the sugarcane aroma condensate storage tank 17, and the outlet of the sugarcane aroma condensate storage tank 17 is connected to the inlet of the mixing unit 14.

[0100] The sugarcane polyphenol raw water preparation unit includes a sugarcane juice preliminary filtration device 1, a first low-temperature high-vacuum distillation device 2, a ceramic membrane module 4, a resin adsorption module 5, a first ethanol storage tank 10, a third low-temperature high-vacuum distillation device 12, and a sugarcane polyphenol raw water storage tank 13. The outlet of the sugarcane juice preliminary filtration device 1 is connected to the inlet of the first low-temperature high-vacuum distillation device 2. The liquid phase outlet of the first low-temperature high-vacuum distillation device 2 is connected to the syrup inlet of the ceramic membrane module 4. The syrup outlet of the ceramic membrane module 4 is connected to the syrup inlet of the resin adsorption module 5. The outlet of the first ethanol storage tank 10 is connected to the eluent inlet of the resin adsorption component 5, the eluent outlet of the resin adsorption component 5 is connected to the inlet of the third low-temperature high-vacuum distillation device 12, the liquid phase outlet of the third low-temperature high-vacuum distillation device 12 is connected to the inlet of the sugarcane polyphenol raw water storage tank 13, and the outlet of the sugarcane polyphenol raw water storage tank 13 is connected to the inlet of the mixing unit 14.

[0101] It also includes a resin permeation syrup storage tank 6, a second low-temperature high-vacuum distillation apparatus 7, and a condensed sugarcane juice storage tank 9. The syrup outlet of the resin adsorption component 5 is connected to the inlet of the resin permeable syrup storage tank 6, the outlet of the resin permeable syrup storage tank 6 is connected to the syrup inlet of the second low temperature high vacuum distillation device 7, the steam outlet of the second low temperature high vacuum distillation device 7 is connected to the inlet of the condensed sugarcane water storage tank 9, and the outlet of the condensed sugarcane water storage tank 9 is connected to the inlet of the first ethanol storage tank 10.

[0102] A preliminary concentrated syrup storage tank 3 is provided between the first low-temperature high-vacuum distillation device 2 and the ceramic membrane module 4. The liquid phase outlet of the first low-temperature high-vacuum distillation device 2 is connected to the inlet of the preliminary concentrated syrup storage tank 3, and the outlet of the preliminary concentrated syrup storage tank 3 is connected to the syrup inlet of the ceramic membrane module 4. An eluent storage tank 11 is provided between the resin adsorption component 5 and the third low-temperature high-vacuum distillation device 12. The outlet of the eluent 5 of the resin adsorption component is connected to the inlet of the eluent storage tank 11, and the outlet of the eluent storage tank 11 is connected to the inlet of the third low-temperature high-vacuum distillation device 12.

[0103] Example 9 A sugar-free polyphenol sugarcane flavored water beverage production line includes a sugarcane juice preliminary filtration device 1, a first low-temperature high-vacuum distillation device 2, a preliminary concentrated syrup storage tank 3, a ceramic membrane assembly 4, a resin adsorption assembly 5, a resin permeation syrup storage tank 6, a second low-temperature high-vacuum distillation device 7, a white sugar production line 8, a condensed sugarcane water storage tank 9, a first ethanol storage tank 10, an eluent storage tank 11, a third low-temperature high-vacuum distillation device 12, a sugarcane polyphenol raw water storage tank 13, a mixing unit 14, a filling and packaging unit 15, an HPP sterilization assembly 16 or a UHT sterilization assembly 15, a filling and packaging unit 16, a sugarcane aroma condensed raw water storage tank 17, and a second ethanol storage tank 18. The sugarcane juice outlet of the sugarcane pressing workshop is connected to the inlet of the sugarcane juice primary filtration device 1, and the outlet of the sugarcane juice primary filtration device 1 is connected to the inlet of the first low-temperature high-vacuum distillation device 2. The steam outlet of the first low-temperature high-vacuum distillation apparatus 2 is connected to the inlet of the sugarcane aroma condensate storage tank 17, and the outlet of the sugarcane aroma condensate storage tank 17 is connected to the inlet of the mixing unit 14. The liquid phase outlet of the first low-temperature high-vacuum distillation device 2 is connected to the inlet of the preliminary concentrated syrup storage tank 3. The outlet of the preliminary concentrated syrup storage tank 3 is connected to the syrup inlet of the ceramic membrane module 4. The syrup outlet of the ceramic membrane module 4 is connected to the syrup inlet of the resin adsorption module 5. The syrup outlet of the resin adsorption module 5 is connected to the inlet of the resin permeation syrup storage tank 6. The outlet of the resin permeation syrup storage tank 6 is connected to the syrup inlet of the second low-temperature high-vacuum distillation device 7. The liquid phase outlet of the second low-temperature high-vacuum distillation device 7 is connected to the white sugar production line 8. The steam outlet of the second low-temperature high-vacuum distillation apparatus 7 is connected to the inlet of the condensed sugarcane water storage tank 9, and the outlet of the condensed sugarcane water storage tank 9 is connected to the inlet one of the first ethanol storage tank 10. The second ethanol storage tank 18 stores high-concentration ethanol, and the outlet of the second ethanol storage tank 18 is connected to the inlet two of the first ethanol storage tank. The outlet of the first ethanol storage tank 10 is connected to the eluent inlet of the resin adsorption component 5, the eluent outlet of the resin adsorption component 5 is connected to the inlet of the eluent storage tank 11, the outlet of the eluent storage tank 11 is connected to the inlet of the third low-temperature high-vacuum distillation device 12, the liquid phase outlet of the third low-temperature high-vacuum distillation device 12 is connected to the inlet of the sugarcane polyphenol raw water storage tank 13, and the outlet of the sugarcane polyphenol raw water storage tank 13 is connected to the inlet of the mixing unit 14.

[0104] After mixing, you can choose between sterilization before filling and packaging or filling and packaging before sterilization, depending on your needs. Filling and packaging before sterilization (e.g.) Figure 10 (As shown): The outlet of the mixing unit 14 is connected to the inlet of the filling and packaging unit 15, and the outlet of the filling and packaging unit 15 is connected to the HPP sterilization assembly 16. Sterilization before filling: The outlet of the mixing unit 14 is connected to the inlet of the UHT sterilization assembly 15, and the outlet of the UHT sterilization assembly 15 is connected to the filling and packaging unit 16.

[0105] In the condensed sugarcane juice storage tank 9, condensed sugarcane juice and high-concentration ethanol are added together in a certain proportion to the first ethanol storage tank 10. The high-concentration ethanol is diluted to 50-75% ethanol. Diluting the ethanol with condensed sugarcane juice ensures that there is no water from other sources during the entire production process, maximizing the utilization of water in the pretreated sugarcane juice. It also ensures that all the water in the finished sugar-free polyphenol sugarcane flavored beverage comes from sugarcane. The outlet of the condensed sugarcane juice storage tank 9 is also directly connected to the elution inlet. In the 7. Desorption: ① water washing and impurity removal step of Example 1, condensed sugarcane juice is used.

[0106] Example 10 A production process for a sugar-free polyphenol sugarcane flavored water beverage includes the following steps: (1) Sugarcane is pressed and filtered to obtain pretreated sugarcane juice; (2) The sugarcane juice is pretreated by low-temperature high-vacuum distillation, and the collected condensate is the sugarcane aroma condensate, while a preliminary concentrated syrup is obtained; (3) The preliminary concentrated syrup is filtered through a ceramic membrane, and the ceramic membrane filtrate is adsorbed by D101 macroporous resin to obtain resin permeated syrup and adsorbed D101 macroporous resin; (4) The adsorbed D101 macroporous resin is first washed with water to remove impurities, and then eluted with ethanol, and the eluent is collected; (5) The eluent is distilled at low temperature and high vacuum to remove ethanol, and sugarcane polyphenol raw water is obtained; (6) Sugarcane aroma condensate and sugarcane polyphenol raw water are mixed at a volume ratio of 3:1 to obtain sugar-free polyphenol sugarcane flavored water, and the sugar-free polyphenol sugarcane flavored water enters a UHT ultra-high temperature sterilization equipment with the following parameters: first stage preheating 110 ℃, second stage sterilization 125 ℃, and third stage cooling 90 ℃. ℃; enter the filling equipment for hot filling at 90 ℃, fill, cap, invert and sterilize for 15 seconds, then cool in stages: the first stage at 60 ℃, the second stage at room temperature cooling water, and after cooling, label and code to obtain the finished sugar-free polyphenol sugarcane flavored water beverage.

[0107] In step (1), the mixture is filtered through a 20-mesh sieve; in step (2), the process parameters for the low-temperature high-vacuum distillation are a temperature below 65 ℃ and a pressure below 8000 Pa; the preliminary concentrated syrup is 30 °Brix; in step (3), the average pore size of the ceramic membrane is 50 nm; in step (4), the ethanol is 50% ethanol; in step (5), the process parameters for the low-temperature high-vacuum distillation are a temperature below 65 ℃ and a pressure below 8000 Pa; in step (6), after mixing, the mixture is sterilized and packaged to obtain a sugar-free polyphenol sugarcane flavored water beverage. In step (6), the sugarcane aroma condensate and sugarcane polyphenol condensate are mixed at a weight ratio of 1:1000.

[0108] Example 11 A production process for a sugar-free polyphenol sugarcane flavored water beverage, the steps are the same as in Example 10, and the process parameters are as follows: in step (1), the water is filtered through a 300-mesh sieve; in step (2), the process parameters for the low-temperature high-vacuum distillation are a temperature below 60 ℃ and a pressure below 8000 Pa; the preliminary concentrated syrup is 50 °Brix; in step (3), the average pore size of the ceramic membrane is 500 nm; in step (4), the ethanol is 75% ethanol; in step (5), the process parameters for the low-temperature high-vacuum distillation are a temperature below 60 ℃ and a pressure below 8000 Pa; in step (6), the sugarcane aroma condensate and the sugarcane polyphenol condensate are mixed at a weight ratio of 1000:1.

[0109] Example 12 A production process for a sugar-free polyphenol sugarcane flavored water beverage, the steps are the same as in Example 10, and the process parameters are as follows: In step (1), the water is filtered through a 250-mesh sieve; In step (2), the process parameters for the low-temperature high-vacuum distillation are a temperature below 60 ℃ and a pressure below 8000 Pa; The preliminary concentrated syrup is 45°Brix; In step (3), the average pore size of the ceramic membrane is 300 nm; In step (4), the ethanol is 68% ethanol; In step (5), the process parameters for the low-temperature high-vacuum distillation are a temperature below 60 ℃ and a pressure below 8000 Pa; In step (6), the sugarcane aroma condensate and the sugarcane polyphenol condensate are mixed at a weight ratio of 1:500.

[0110] Example 13 A production process for a sugar-free polyphenol-flavored sugarcane water beverage, with the same steps as in Example 10, and the process parameters are as follows: In step (1), filter using a 50, 100, 150, 200, 250 or 300 mesh sieve; In step (2), the process parameters for the low-temperature high-vacuum distillation are: temperature of 20, 25, 30, 35, 40, 45, 50, 55, 58, 62, 65 or 60 °C, and pressure of 2000, 2500, 3000, 3500, 4000, 5000, 4500, 5500, 6000, 6500, 7000, 7500 or 8000 Pa; and the preliminary concentrated syrup is 30, 32, 35, 38, 40, 42, 45, 48 or 50 °Brix. The average pore size of the ceramic membrane in step (3) is 50, 80, 100, 120, 150, 200, 250, 300, 350, 400, 450, 500 nm; The ethanol mentioned in step (4) is 50%, 53%, 58%, 55%, 60%, 63%, 68%, 65%, 70%, 73% or 75% ethanol; In step (5), the process parameters for the low-temperature high-vacuum distillation are: temperature of 20, 25, 30, 35, 40, 45, 50, 55, 58, 62, 65 or 60 °C, and pressure of 2000, 2500, 3000, 3500, 4000, 5000, 4500, 5500, 6000, 6500, 7000, 7500 or 8000 Pa; In step (6), sugarcane aroma condensate and sugarcane polyphenol condensate are mixed in weight ratios of 1:1, 1:2, 1:3, 1:4, 1:5, 1:6, 1:7, 1:8, 1:9, 1:10, 1:20, 1:30, 1:40, 1:50, 1:60, 1:70, 1:80, 1:90, 1:100, 1:200, 1:300, 1:400, 1:500, 1:600, 1:70 ... Mixed ratios of 00, 1:900, 1:100, 2:1, 3:1, 4:1, 5:1, 6:1, 7:1, 8:1, 9:1, 10:1, 20:1, 30:1, 40:1, 50:1, 60:1, 70:1, 80:1, 90:1, 100:1, 200:1, 300:1, 400:1, 500:1, 600:1, 700:1, 800:1, 900:1, or 1000:1.

[0111] Example 14 Antioxidant Capacity Determination Free radicals are highly reactive and active, interacting with various substances in the body to remove hydrogen atoms and produce harmful oxidation products and intermediates, ultimately damaging the structure and function of living cells. Antioxidants can neutralize the effects of free radicals, reducing the cumulative impact of oxidative damage on reactive oxygen species in the human body, and providing data support for the development and utilization of sugar-free polyphenol-flavored sugarcane water beverages. DPPH free radical scavenging rate and ABTS scavenging rate are two commonly used indicators for evaluating the antioxidant capacity of substances, reflecting their antioxidant performance by measuring their ability to scavenge free radicals.

[0112] (1) DPPH free radical scavenging rate determination method: Weigh 0.002 mg of DPPH powder and dissolve it in anhydrous ethanol, mix well and make up to 50 mL to prepare a 0.1 mmol / L DPPH solution. Add 100 μL of sample (according to the concentration gradient of 20, 40, 60, 80, 100, 120 mg / mL), then add 100 μL of DPPH solution, shake well, react in the dark for 30 min, and measure the absorbance at a wavelength of 517 nm (C). Add 100 μL of sample (according to the concentration gradient of 20, 40, 60, 80, 100, 120 mg / mL), then add 100 μL of anhydrous ethanol, shake well, react in the dark for 30 min, and measure the absorbance at a wavelength of 517 nm (B). Add 100 μL of anhydrous ethanol, then add 100 μL of DPPH solution, shake well, react in the dark for 30 min, and measure the absorbance at a wavelength of 517 nm (A). The DPPH free radical scavenging rate is calculated using the following formula:

[0113] In the formula: C represents the absorbance value measured after mixing the sample solution with the DPPH solution; B represents the absorbance value after mixing anhydrous ethanol and the sample; A represents the absorbance value after mixing anhydrous ethanol and DPPH. A regression curve is plotted with sample concentration on the x-axis and DPPH free radical scavenging rate on the y-axis. The IC50 value is calculated based on the curve equation. The DPPH curve equation is as follows: DFGZZWS-1: y = 0.2964ln(x) - 0.7921, R 2 =0.9566;DFGZZWS-5:y=0.3261ln(x)-0.9223, R 2 =0.9309; DFGZZWS-4: y=0.3684ln(x)-1.02, R 2 =0.9381.

[0114] (2) ABTS free radical scavenging rate determination method: Dissolve 0.1 g ABTS and 0.029 g potassium persulfate in deionized water, mix the ABTS solution and potassium persulfate solution evenly to prepare 100 mL of ABTS free radical stock solution, and store the prepared solution in a refrigerator at 4 °C for 12 hours. Dilute the ABTS solution to an appropriate concentration using phosphate buffer (pH=7.4, prepared from disodium hydrogen phosphate and sodium dihydrogen phosphate) so that its absorbance at a specified wavelength is approximately 0.7±0.02. This is the ABTS working solution. Add 10 μL of sample (according to the concentration gradient of 10, 20, 30, 40, 50, 60 mg / mL), then add 200 μL of ABTS+· working solution, shake well, react in the dark for 10 min, and measure the absorbance value C at a wavelength of 405 nm. Add 10 μL of sample (according to concentration gradients of 10, 20, 30, 40, 50, and 60 mg / mL), then add 200 μL of phosphate buffer and mix well. Incubate in the dark for 10 min, and measure the absorbance at 405 nm (B). Add 10 μL of phosphate buffer, then add 200 μL of ABTS working solution and mix well. Incubate in the dark for 10 min, and measure the absorbance at 405 nm (A). The ABTS free radical scavenging rate is calculated using the following formula:

[0115] In the formula: C represents the absorbance value measured after mixing the sample solution with the ABTS working solution; B represents the absorbance value after mixing the phosphate buffer and the sample; A represents the absorbance value after mixing the phosphate buffer and the ABTS working solution. A regression curve is plotted with sample concentration on the x-axis and ABTS free radical scavenging rate on the y-axis. The IC50 value is calculated based on the curve equation. The ABTS curve equation is as follows: DFGZZWS-1: y = 0.4133ln(x) - 0.7681, R 2 =0.9794;DFGZZWS-5:y=0.3975ln(x)-0.75, R 2 =0.9695; DFGZZWS-4: y=0.3728ln(x)-0.5831, R 2 =0.9801.

[0116] (3) DPPH / ABTS free radical scavenging rate experimental results: Due to the high concentration and dark color of DFGZZWS_5 (sugarcane polyphenol raw water), in order to avoid its color affecting the absorbance measurement, DFGZZWS_5 (sugarcane polyphenol raw water) was diluted 5 times before the above experimental operation. The following DPPH / ABTS free radical scavenging rate experimental results and the corresponding regression curves of DFGZZWS_5 (sugarcane polyphenol raw water) are all results after dilution by 5 times; the following IC50 experimental results have been converted into the original DFGZZWS_5 (sugarcane polyphenol raw water) solution results. The experimental results of DPPH free radical scavenging rate and ABTS scavenging rate in this embodiment are shown in Tables 11 and 12. It can be seen that compared with the pretreated sugarcane juice as raw material, the antioxidant capacity of sugar-free polyphenol sugarcane flavored water beverage has been greatly improved, which is due to the contribution of sugarcane polyphenol raw water.

[0117] Table 11 Results of DPPH free radical scavenging rate determination

[0118] Table 12 Results of ABTS Free Radical Scavenging Rate Measurement

[0119] Example 15 Detection of Phenolic Components 1. Experimental Introduction: This embodiment uses ultra-high performance liquid chromatography-tandem electrostatic field orbital trap mass spectrometry (UHPLC-Q Exactive HFX) to detect metabolites in samples. By matching the metabolites' retention time, molecular mass (molecular mass error within 10 ppm), and secondary fragmentation spectra in the database, qualitative and quantitative analysis of phenolic monomers in the samples and subsequent informatics analysis are performed.

[0120] 2. Main equipment and reagents Q Exactive HFX mass spectrometer, Vanquish ultra-high pressure liquid chromatograph, chromatographic column: ACQUITY UPLC HSST3 Column (100 × 2.1 mm, 1.8 μm, Waters), low-temperature high-speed centrifuge (Eppendorf 5430R), ultrasonic cleaner, vortex mixer, methanol / acetonitrile / formic acid (HPLC, ANPEL), ultrapure water system.

[0121] 3. Experimental Methods 3.1 Sample preparation: Accurately measure an appropriate volume of sample into a centrifuge tube, add 2 times the volume of extraction buffer (methanol / acetonitrile, 1:1, v / v), vortex for 60 s, perform low-temperature ultrasonic extraction for 30 min, centrifuge at 12000 rpm for 10 min at 4℃, collect the supernatant and place it at -20℃ for 1 h to precipitate, then centrifuge at 12000 rpm for 10 min at 4℃, collect the supernatant solution and vacuum dry it, add 100 μL of 30% acetonitrile solution to reconstitute, vortex, centrifuge at 12000 rpm for 10 min at 4℃, collect the supernatant solution for instrumental analysis.

[0122] 3.2 Instrument Parameters Chromatographic column: Waters HSS T3 (100×2.1 mm, 1.8 μm); mobile phase: phase A was 0.1% formic acid-water solution, phase B was 0.1% formic acid-acetonitrile solution; flow rate: 0.3 mL / min; column temperature: 40℃; injection volume: 2 μL; elution gradient: 0 min phase A / phase B (100:0, v / v), 1 min phase A / phase B (100:0, v / v), 4 min phase A / phase B (40:60, v / v), 6.5 min phase A / phase B (5:95, v / v), 6.6 min phase A / phase B (100:0, v / v), 8.0 min phase A / phase B (100:0, v / v).

[0123] 3.3 Mass spectrometry conditions: Equipped with an electrospray ionization (ESI) source, sheath gas 40 arb, auxiliary gas 10 arb, ion spray voltage +3000 V / -2800 V, temperature 350℃, ion transmission tube temperature 320℃. Scan mode was Full-ms-ddMS2, scan mode was positive / negative ion. Primary mass spectrometry scan range (scan m / z range): 70-1050 Da, primary resolution 70000, secondary resolution 17500.

[0124] 4. Analysis of Experimental Results The results are shown in Table 13. A total of 175 phenolic substances were detected in the samples from the three stages. Among them, 175 were detected in DFGZZWS_1, 166 in DFGZZWS_5, and 166 in DFGZZWS_4. It is evident that the sugar-free polyphenol-enriched sugarcane-flavored beverage (DFGZZWS_4) largely retains the phenolic substances in sugarcane juice and can highly replicate the core functional component characteristics of the pretreated sugarcane juice (DFGZZWS_1). Combined with the results of the total polyphenol content study in Example 4, it can be seen that DFGZZWS_4, while increasing the total polyphenol content by 11.39%, almost completely replicated the compositional spectrum of its phenolic substances. This allows DFGZZWS_4 to not only retain the characteristics of the raw material in terms of antioxidant capacity but also achieve functional enhancement through a synergistic effect.

[0125] Table 13 Results of phenolic monomer determination in samples

Claims

1. A sugar-free polyphenol-flavored sugarcane water beverage, characterized in that, It is made by mixing sugarcane aroma condensate and sugarcane polyphenol condensate. The sugarcane aroma condensate is the condensate obtained by low-temperature high-vacuum distillation of sugarcane juice. The sugarcane polyphenol raw water is a liquid phase obtained by removing ethanol from the macroporous resin eluent through low-temperature high-vacuum distillation. The macroporous resin eluent is obtained by eluting and collecting the macroporous resin after adsorbing sugarcane syrup with ethanol as the eluent.

2. A production process for a sugar-free polyphenol-flavored sugarcane water beverage, characterized in that, Includes the following steps: (1) After pressing the sugarcane, the juice is filtered to obtain pretreated sugarcane juice. (2) Sugarcane juice is pretreated by low-temperature high-vacuum distillation. The collected condensate is the sugarcane aroma condensate, and a preliminary concentrated syrup is obtained at the same time. (3) The initially concentrated syrup is filtered through a ceramic membrane, and the filtrate from the ceramic membrane is adsorbed through macroporous resin to obtain resin-permeable syrup and adsorbed macroporous resin. (4) After adsorption, the macroporous resin is first washed with water to remove impurities, then eluted with ethanol, and the eluent is collected. (5) After removing ethanol from the eluent by low-temperature high-vacuum distillation, sugarcane polyphenol raw water is obtained. (6) Mix the sugarcane aroma condensed raw water and sugarcane polyphenol raw water to obtain a sugar-free polyphenol sugarcane flavored water beverage.

3. The production process of the sugar-free polyphenol sugarcane flavored water beverage as described in claim 2, characterized in that, In step (1), the material is filtered through a 20-300 mesh sieve; In step (2), the process parameters for the low-temperature high-vacuum distillation are: temperature below 65 °C and pressure below 8000 Pa; the initial concentrated syrup is 30~50 °Brix. The ceramic membrane described in step (3) has an average pore size of 50~500 nm; The ethanol mentioned in step (4) is 50-75% ethanol; In step (5), the process parameters for the low-temperature high-vacuum distillation are a temperature below 65 °C and a pressure below 25000 Pa.

4. The production process of the sugar-free polyphenol sugarcane flavored water beverage as described in claim 2 or 3, characterized in that, In step (6), sugarcane aroma condensate and sugarcane polyphenol condensate are mixed in a weight ratio of 1:1000 to 1000:

1.

5. The production process of the sugar-free polyphenol sugarcane flavored water beverage as described in claim 3, characterized in that, The 50-75% ethanol is prepared by diluting 95% or more ethanol with condensed sugarcane juice, which is collected during the process of passing the syrup through a low-temperature, high-vacuum distillation resin.

6. A sugar-free polyphenol sugarcane flavored water beverage production line, characterized in that, The unit includes a sugarcane aroma condensate preparation unit, a sugarcane polyphenol condensate preparation unit, and a mixing unit. The outlet of the sugarcane aroma condensate preparation unit is connected to the inlet of the mixing unit. The outlet of the sugarcane polyphenol raw water preparation unit is connected to the inlet of the mixing unit.

7. The sugar-free polyphenol sugarcane flavored water beverage production line as described in claim 6, characterized in that, The sugarcane aroma condensate preparation unit includes a sugarcane juice preliminary filtration device, a first low-temperature high-vacuum distillation device, and a sugarcane aroma condensate storage tank. The outlet of the sugarcane juice preliminary filtration device is connected to the inlet of the first low-temperature high-vacuum distillation device, the steam outlet of the first low-temperature high-vacuum distillation device is connected to the inlet of the sugarcane aroma condensate storage tank, and the outlet of the sugarcane aroma condensate storage tank is connected to the inlet of the mixing unit.

8. The sugar-free polyphenol sugarcane flavored water beverage production line as described in claim 6, characterized in that, The sugarcane polyphenol raw water preparation unit includes a sugarcane juice preliminary filtration device, a first low-temperature high-vacuum distillation device, a ceramic membrane module, a resin adsorption module, a first ethanol storage tank, a third low-temperature high-vacuum distillation device, and a sugarcane polyphenol raw water storage tank. The outlet of the sugarcane juice preliminary filtration device is connected to the inlet of the first low-temperature high-vacuum distillation device. The liquid phase outlet of the first low-temperature high-vacuum distillation device is connected to the syrup inlet of the ceramic membrane module. The syrup outlet of the ceramic membrane module is connected to the syrup inlet of the resin adsorption module. The outlet of the first ethanol storage tank is connected to the eluent inlet of the resin adsorption component, the eluent outlet of the resin adsorption component is connected to the inlet of the third low-temperature high-vacuum distillation unit, the liquid phase outlet of the third low-temperature high-vacuum distillation unit is connected to the inlet of the sugarcane polyphenol raw water storage tank, and the outlet of the sugarcane polyphenol raw water storage tank is connected to the inlet of the second mixing unit.

9. The sugar-free polyphenol sugarcane flavored water beverage production line as described in claim 6, characterized in that, It also includes a resin permeation syrup storage tank, a second low-temperature high-vacuum distillation apparatus, and a condensed sugarcane juice storage tank. The syrup outlet of the resin adsorption component is connected to the inlet of the resin-through-syrup storage tank, the outlet of the resin-through-syrup storage tank is connected to the syrup inlet of the second low-temperature high-vacuum distillation device, the steam outlet of the second low-temperature high-vacuum distillation device is connected to the inlet of the condensed sugarcane water storage tank, and the outlet of the condensed sugarcane water storage tank is connected to the inlet of the first ethanol storage tank.

10. The sugar-free polyphenol sugarcane flavored water beverage production line as described in claim 6, characterized in that, A preliminary concentrated syrup storage tank is provided between the first low-temperature high-vacuum distillation device and the ceramic membrane module. The liquid phase outlet of the first low-temperature high-vacuum distillation device is connected to the inlet of the preliminary concentrated syrup storage tank, and the outlet of the preliminary concentrated syrup storage tank is connected to the syrup inlet of the ceramic membrane module. An eluent storage tank is provided between the resin adsorption component and the third low-temperature high-vacuum distillation device. The eluent outlet of the resin adsorption component is connected to the inlet of the eluent storage tank, and the eluent storage tank outlet is connected to the inlet of the third low-temperature high-vacuum distillation device.

11. The sugar-free polyphenol sugarcane flavored water beverage production line according to any one of claims 6 to 10, characterized in that, It also includes filling and packaging units and sterilization components; The mixing unit's liquid outlet is connected to the filling and packaging unit's inlet, and the filling and packaging unit's outlet is connected to the sterilization component. Alternatively, the mixing unit's liquid outlet is connected to the sterilization component's inlet, and the sterilization component's outlet is connected to the filling and packaging unit.

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