Composite flavoring agent synergistic low-sodium conditioning seasoning salt
By using the heterogeneous induced co-crystallization technology of amino acid charge balance system and inorganic salt lattice, organic flavor factors are embedded inside inorganic salt crystals, which solves the problem of inconsistent potassium chloride bitterness and dissolution release rate in low sodium seasoning salt, and realizes the simultaneous release of salty and umami flavor and the stability of sensory quality.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- BEIJING FOUR SEASONS CATERING MANAGEMENT CO LTD
- Filing Date
- 2026-03-17
- Publication Date
- 2026-05-05
AI Technical Summary
Existing low-sodium seasoning salts suffer from problems such as a prominent bitter taste due to potassium chloride, uneven distribution of flavor compounds, and inconsistent dissolution and release rates, resulting in poor sensory harmony.
By constructing an amino acid charge balance system and performing heterogeneous induced co-crystallization with an inorganic salt lattice, organic flavor factors are embedded inside the inorganic salt crystal. Bitterness is masked at the molecular level by using ion-pair complexes. Through heterogeneous induced co-crystallization during crystal growth and layered progressive flavor construction at the mesoscale, the simultaneous release of salty and umami flavor is achieved.
It achieves physiological shielding of the bitter taste of potassium ions in low-sodium seasoning salt, ensures component homogeneity and sensory quality stability, solves the problems of component stratification and inconsistent dissolution kinetics, and provides synergistic release and persistence of salty and umami flavor.
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Figure CN121970883A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of condiment technology, specifically to a low-sodium seasoning salt with synergistic effects of compound flavoring agents. Background Technology
[0002] High sodium intake is closely linked to an increased risk of chronic diseases such as hypertension, making it essential to reduce the sodium content in seasoning salt a necessary requirement for a healthy diet. Currently, the most common method for preparing low-sodium salt is to partially replace sodium chloride with potassium chloride. However, while potassium chloride provides a salty taste, it also introduces a noticeable metallic bitterness, and this off-flavor becomes increasingly detrimental to the sensory quality of food as the replacement ratio increases.
[0003] To mask the bitterness of potassium ions and enhance the overall flavor, current techniques often involve adding flavor compounds such as amino acids, nucleotides, or plant extracts. However, this simple mechanical mixing method has significant drawbacks in actual production and application. Due to differences in particle size, density, and surface properties between inorganic salt crystals and organic flavor agents, the components are prone to stratification during packaging, transportation, and storage due to mechanical vibration, resulting in uneven distribution of product components and affecting the stability of the flavor.
[0004] More importantly, because the components in physically mixed products exist independently, their dissolution kinetics vary upon entering a humid environment. The differences in dissolution rates between sodium chloride, potassium chloride, and organic flavor-masking agents prevent sodium and potassium ions from simultaneously contacting taste receptors, resulting in an unstable bitterness-masking effect. In actual cooking scenarios, this mismatch in dissolution performance leads to a significant discontinuity in the sequential perception of saltiness, umami, and bitterness, making it difficult to achieve a synergistic sensory release of saltiness and umami. Furthermore, while some coating technologies can improve flavor, they often involve the use of non-water-soluble carriers, causing turbidity in aqueous solutions and failing to provide the immediate flavor expression required by the coating due to delayed dissolution. Therefore, developing a low-sodium seasoning salt that achieves deep component integration, synchronized dissolution performance, and good sensory harmony is a problem that the industry needs to solve. Summary of the Invention
[0005] To address the shortcomings of existing technologies, this invention provides a low-sodium seasoning salt with synergistic effects of compound flavoring agents, which solves the problems of poor sensory harmony caused by the prominent bitter taste of potassium chloride, uneven distribution of flavor substances, and inconsistent dissolution and release rates in existing low-sodium salt products.
[0006] To address the above problems, this invention provides a low-sodium seasoning salt with synergistic effects of compound flavoring agents, employing the following technical solution: A low-sodium seasoning salt with synergistic effects of compound flavoring agents is made from the following raw materials in parts by weight: sodium chloride: 550-600 parts; potassium chloride: 280-320 parts; amino acid ion pair buffer mother liquor, made from the following components in parts by weight: L-arginine: 40-60 parts, L-glutamic acid: 40-50 parts, L-histidine: 2-4 parts, and anhydrous citric acid as an acidity regulator; and disodium inosinate: 5-10 parts.
[0007] The synergistic effect of the above technical solutions lies in the heterogeneous induced co-crystallization between a pre-constructed amino acid charge balance system and an inorganic salt lattice, which embeds the originally independent organic flavor factors into the inorganic salt crystal. This structural integration not only achieves physiological shielding of potassium ion bitterness at the molecular level, but also ensures the macroscopic component uniformity of the product, ultimately achieving the technical effect of simultaneous release of salty and umami flavors and stable sensory quality.
[0008] The core innovations of this invention and the underlying reaction mechanism can be elaborated from the following three dimensions: Firstly, there is the effect of charge dissociation and ion pair association at the molecular level. During the preparation of the amino acid ion pair buffer mother liquor, the apparent pH of the system was strictly limited to between 5.80 and 6.10. According to the ionization equilibrium constants (pKa) of each component, under this acid-base environment, the guanidinium group of L-arginine and the imidazole group of L-histidine undergo high protonation and become positively charged, while the carboxyl group of L-glutamic acid becomes negatively charged due to deprotonation.
[0009] This dynamic ion-pair complex, formed through electrostatic attraction and a network of hydrogen bonds, has a strong buffering capacity in the human oral cavity microenvironment. When potassium ions dissolved from potassium chloride attempt to bind to receptors on the surface of taste cells, the ion-pair complex uses a charge-shielding effect to interfere with the transmembrane transmission of bitterness signals, thereby weakening the bitterness at the forefront of taste perception.
[0010] Secondly, the heterogeneous induced co-crystallization mechanism during crystal growth. In a continuous vacuum crystallizer, sodium chloride and potassium chloride are in a supersaturated crystallization state. At this point, the amino acid ion pairs injected via the side line act as induction centers for heterogeneous nucleation. Because amino acid ion pairs possess abundant polar functional groups, they readily anchor themselves on the growth steps or dislocation points of the inorganic salt nuclei. As the solvent continues to evaporate, inorganic salt ions directionally accumulate around these organic cores, solidifying the amino acid components within the crystal structure through interstitial solid solution or lattice encapsulation. This process breaks away from the simple physical mixing of salt particles and amino acid powder in traditional low-sodium salts, forming a structured whole and fundamentally solving the problems of component stratification and inconsistent dissolution kinetics.
[0011] Thirdly, the layered and progressive flavor construction at the mesoscale. Utilizing the saturated mother liquor film adhering to the surface of the centrifuged wet crystals, disodium nucleotides are introduced via high-pressure atomization. This umami-enhancing component rapidly diffuses within the mother liquor film and forms a uniform solid coating film on the crystal surface during the subsequent drying process. This multi-layered structure, with embedded amino acid ion pairs and externally encapsulated umami factors, allows the product to release its surface umami flavor upon contact with saliva, followed by the synergistic emergence of the inner saltiness and masking factors, achieving a depth and persistence of flavor sensation.
[0012] To further optimize the above technical solution, the present invention also relates to the following process details: In terms of ingredient proportions, the preferred ratio is 570 parts sodium chloride, 300 parts potassium chloride, and a specific proportion of amino acids and 8 parts disodium nucleotides. This parameter combination was determined based on multiple experimental feedbacks on the sodium-potassium synergistic effect and charge buffer capacity, which enables the sensory score to reach its peak.
[0013] For the preparation of the buffer mother liquor, the pH value was adjusted online by using an anhydrous citric acid solution with a mass fraction of 30% at 20-25℃. This dynamic addition method effectively avoided the risk of amino acid denaturation caused by excessive local acidity and ensured the spatial configuration integrity of ion pairs in the precursor solution.
[0014] In the crystallization process, maintaining the crystallizer pressure at -0.08 MPa to -0.09 MPa, coupled with an operating temperature of 60-65°C, is to prevent the oxidation or degradation of heat-sensitive organic components while ensuring the evaporation rate. Controlling the crystal slurry residence time to complete the side-stream injection within 1-1.5 hours ensures sufficient kinetic time for the heterogeneous induced co-crystallization process.
[0015] In subsequent processing, the process mother liquor separated by a two-stage pusher centrifuge is returned to the system for circulation, significantly improving material utilization. The 3%-5% moisture content of the wet-based crystals is crucial for atomized spraying, providing a uniformly spread liquid carrier for the flavor enhancer solution.
[0016] The final drying process uses a fluidized bed drying system, with the hot air temperature set at 80-85℃ and the airflow adjusted to ensure the material temperature does not exceed 70℃. This low-temperature drying strategy rapidly removes moisture to below 1.5% while preserving the product's color and flavor activity to the maximum extent.
[0017] This invention provides a low-sodium seasoning salt with synergistic effects of compound flavoring agents. It has the following beneficial effects: 1. This invention constructs a buffered ion-pair complex by adjusting the pH to induce a proton transfer reaction between acidic and basic amino acids. During dissolution, this complex can interfere with the binding of potassium ions to taste receptors through charge shielding, thereby masking the metallic bitterness commonly found in low-sodium salts at the molecular level and improving the sensory appeal of the product.
[0018] 2. This invention utilizes a heterogeneous induced co-crystallization process to orient amino acid ions onto the growth steps of inorganic salt crystals and allow them to grow in a surrounding manner, achieving a structured integration of organic flavor components within the inorganic salt crystals. This integrated structure eliminates the physical mixing boundaries between components, ensuring that sodium and potassium ions and flavor factors have consistent kinetic characteristics during dissolution, thus avoiding flavor imbalance caused by uneven release rates of various components.
[0019] 3. This invention utilizes a thin film of trace amounts of mother liquor on the crystal surface after solid-liquid separation to attach umami-enhancing components to the crystal surface in a mesoscopic coating form, constructing a multi-layered flavor distribution system. Through the synergistic effect of surface umami components and internal chimeric components, the perceived saltiness and umami intensity of the product is enhanced, effectively solving the problems of insufficient umami depth and weak sensory impact in low-sodium seasoning products. Attached Figure Description
[0020] Figure 1 This is a graph showing the variation of apparent pH value of the crystallization mother liquor with solid phase mass fraction in different formulation systems of this invention. Figure 2 The diagram shows the kinetic curves of simultaneous dissolution of potassium ions and L-arginine in different formulation systems of the present invention. (a) is the dissolution trajectory of the target component in Example 1, (b) is the dissolution trajectory of the target component in Comparative Example 1, and (c) is the dissolution trajectory of the target component in Comparative Example 4. Figure 3 The diagram shows the relative deviation trajectory of ion content in different spatial layers of the material after simulated transportation vibration in different formulation systems of the present invention. Among them, (a) shows the distribution law of relative deviation of sodium ions and (b) shows the distribution law of relative deviation of potassium ions. Figure 4 The image shows a comparison of the flavor sensory evaluation and flavor enhancer retention rate of the finished products with different formulations of the present invention. In this image, (a) shows the distribution trajectory of the initial bitterness intensity and overall saltiness score in Examples 1 to 3 and Comparative Examples 3 and 5, and (b) shows the variation of the activity retention rate of disodium flavor nucleotides in Examples 1 to 3 and Comparative Examples 3 and 5. Detailed Implementation
[0021] The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0022] Preparation Examples 1-3: Preparation Example 1: This preparation example provides a method for preparing an amino acid ion pair buffer stock solution, comprising the following steps: Step 1: Add 500 parts by weight of deionized water at 25°C to the preparation tank, turn on the stirrer, and set the stirring speed to 120 r / min. Step 2: Add 50 parts by weight of L-arginine, 45 parts by weight of L-glutamic acid and 3 parts by weight of L-histidine to the preparation tank in sequence, and stir continuously at a constant temperature for 25 minutes until the solid is completely dissolved to obtain a free amino acid aqueous solution. Step 3: Prepare an anhydrous citric acid aqueous solution with a mass fraction of 30% in advance. Using an online pH meter for feedback control, add the anhydrous citric acid aqueous solution dropwise to the free amino acid aqueous solution obtained in Step 2 at a uniform rate. Adjust and keep the apparent pH value of the mixture constant at 5.95. This process consumes 32 parts by weight of anhydrous citric acid aqueous solution. Continue stirring for 10 minutes to mix evenly and obtain the final required amino acid ion pair buffer mother liquor.
[0023] Preparation Example 2: This preparation example provides a method for preparing an amino acid ion pair buffer stock solution, comprising the following steps: Step 1: Add 500 parts by weight of deionized water at 20°C to the preparation tank, turn on the stirrer, and set the stirring speed to 100 r / min. Step 2: Add 40 parts by weight of L-arginine, 40 parts by weight of L-glutamic acid and 2 parts by weight of L-histidine to the preparation tank in sequence, and stir continuously at a constant temperature for 30 minutes until the solid is completely dissolved to obtain a free amino acid aqueous solution. Step 3: Prepare an anhydrous citric acid aqueous solution with a mass fraction of 30% in advance. Using an online pH meter for feedback control, add the anhydrous citric acid aqueous solution dropwise to the free amino acid aqueous solution obtained in Step 2 at a uniform rate. Adjust and keep the apparent pH value of the mixture constant at 5.80. A total of 28 parts by weight of anhydrous citric acid aqueous solution is consumed. Continue stirring for 10 minutes to mix evenly and obtain the final required amino acid ion pair buffer mother liquor.
[0024] Preparation Example 3: This preparation example provides a method for preparing an amino acid ion pair buffer stock solution, comprising the following steps: Step 1: Add 500 parts by weight of deionized water at 25°C to the preparation tank, turn on the stirrer, and set the stirring speed to 150 r / min. Step 2: Add 60 parts by weight of L-arginine, 50 parts by weight of L-glutamic acid and 4 parts by weight of L-histidine to the preparation tank in sequence, and stir continuously at a constant temperature for 20 minutes until the solid is completely dissolved to obtain a free amino acid aqueous solution. Step 3: Prepare an anhydrous citric acid aqueous solution with a mass fraction of 30% in advance. Using an online pH meter for feedback control, add the anhydrous citric acid aqueous solution dropwise to the free amino acid aqueous solution obtained in Step 2 at a uniform rate. Adjust and keep the apparent pH value of the mixture constant at 6.10. The actual amount of anhydrous citric acid aqueous solution added is 38 parts by weight. Continue stirring for 10 minutes to mix evenly and obtain the final required amino acid ion pair buffer mother liquor.
[0025] Examples 1-3: Example 1: This embodiment provides a method for preparing a low-sodium seasoning salt with synergistic effects of compound flavoring agents, including the following steps: Step 1: Inject 2000 parts by weight of deionized water into a mixing vessel, set the temperature to 75℃, add 570 parts by weight of sodium chloride and 300 parts by weight of potassium chloride, set the stirring speed to 150 r / min, and stir at a constant temperature for 30 minutes until the solid phase is completely dissolved to obtain a homogeneous inorganic high-salt solution; continuously pump the inorganic high-salt solution into a continuous vacuum crystallizer with an external circulation pipeline, turn on the internal circulation pump of the crystallizer, set the system absolute pressure to -0.085 MPa, set the operating temperature to 62℃, and perform vacuum constant temperature evaporation. When the solid phase mass fraction in the crystal slurry reaches 12%, a large number of microcrystals precipitate in the system to form a solid inorganic salt microcrystal carrier suspension, which is kept in circulation for later use; Step 2: Take all the amino acid ion pair buffer mother liquor obtained in Preparation Example 1 as the precursor injection solution; Step 3: Maintain the vacuum crystallizer in a continuous vacuum evaporation state at 62°C as in Step 1. Start the metering pump and inject the precursor injection liquid from Step 2 directly into the high-pressure pipeline section at the outlet of the external circulation pump of the vacuum crystallizer via side-line injection. Control the mass flow rate of the precursor injection liquid to ensure that it is continuously and uniformly injected into the external circulation pipeline of the vacuum crystallizer within a 1.2-hour crystal slurry residence time, maintaining continuous feeding and discharging, stabilizing the crystal slurry residence time at 1.2 hours, and achieving heterogeneous induced co-crystallization. Step 4: The crystal slurry discharged from the bottom of the vacuum crystallizer in Step 3 is continuously fed into a two-stage pusher centrifuge for solid-liquid separation. The separated process mother liquor is returned to the crystallizer, and the filter cake is collected to obtain wet-based composite salt crystals with a water content of 4%. 8 parts by weight of disodium inosinate are completely dissolved in an appropriate amount of deionized water to prepare a 12% (w / w) flavor enhancer solution. The wet-based composite salt crystals are fed into a mixer equipped with a plow blade agitator. The stirring speed is set to 50 r / min, and the atomization pressure is set to 0.3 MPa using a high-pressure atomizing nozzle to uniformly spray the flavor enhancer solution onto the surface of the wet-based composite salt crystals. Step 5: Feed the material processed in Step 4 into a fluidized bed dryer, set the hot air inlet temperature to 82°C, adjust the air volume to keep the bed material temperature at 65°C, dry until the product moisture content is less than or equal to 1.5%, cool to room temperature, sieve and classify, and package to obtain the target low-sodium seasoning salt.
[0026] Example 2: This embodiment provides a method for preparing a low-sodium seasoning salt with synergistic effects of compound flavoring agents, including the following steps: Step 1: Inject 2000 parts by weight of deionized water into a mixing vessel, set the temperature to 80℃, add 600 parts by weight of sodium chloride and 280 parts by weight of potassium chloride, set the stirring speed to 200 r / min, and stir at a constant temperature for 45 minutes until the solid phase is completely dissolved to obtain a homogeneous inorganic high-salt solution; continuously pump the inorganic high-salt solution into a continuous vacuum crystallizer with an external circulation pipeline, turn on the internal circulation pump of the crystallizer, set the system absolute pressure to -0.08MPa, set the operating temperature to 65℃, and perform vacuum constant temperature evaporation. When the solid phase mass fraction in the crystal slurry reaches 10%, a large number of microcrystals precipitate in the system to form a solid inorganic salt microcrystal carrier suspension, which is kept in circulation for later use; Step 2: Take all the amino acid ion pair buffer mother liquor obtained in Preparation Example 2 as the precursor injection solution; Step 3: Keep the vacuum crystallizer in a continuous vacuum evaporation state at 65°C as in Step 1, start the metering pump, and inject the precursor injection liquid from Step 2 directly into the high-pressure pipeline section at the outlet of the external circulation pump of the vacuum crystallizer via side-line injection. Control the mass flow rate of the precursor injection liquid to ensure that it is continuously and uniformly injected into the external circulation pipeline of the vacuum crystallizer within a 1-hour crystal slurry residence time, maintain continuous feeding and discharging, stabilize the crystal slurry residence time at 1 hour, and achieve heterogeneous induced co-crystallization. Step 4: The crystal slurry discharged from the bottom of the vacuum crystallizer in Step 3 is continuously fed into a two-stage pusher centrifuge for solid-liquid separation. The separated process mother liquor is returned to the crystallizer, and the filter cake is collected to obtain wet-based composite salt crystals with a water content of 5%. 5 parts by weight of disodium inosinate are completely dissolved in an appropriate amount of deionized water to prepare a 10% flavor enhancer solution. The wet-based composite salt crystals are fed into a mixer equipped with a plow blade agitator. The stirring speed is set to 40 r / min, and the atomization pressure is set to 0.2 MPa using a high-pressure atomizing nozzle to uniformly spray the flavor enhancer solution onto the surface of the wet-based composite salt crystals. Step 5: Feed the material processed in Step 4 into a fluidized bed dryer, set the hot air inlet temperature to 80°C, adjust the air volume to keep the bed material temperature at 70°C, dry until the product moisture content is less than or equal to 1.5%, cool to room temperature, sieve and classify, and package to obtain the target low-sodium seasoning salt.
[0027] Example 3: This embodiment provides a method for preparing a low-sodium seasoning salt with synergistic effects of compound flavoring agents, including the following steps: Step 1: Inject 2000 parts by weight of deionized water into a mixing vessel, set the temperature to 75℃, add 550 parts by weight of sodium chloride and 320 parts by weight of potassium chloride, set the stirring speed to 180 r / min, and stir at a constant temperature for 35 minutes until the solid phase is completely dissolved to obtain a homogeneous inorganic high-salt solution; continuously pump the inorganic high-salt solution into a continuous vacuum crystallizer with an external circulation pipeline, turn on the internal circulation pump of the crystallizer, set the system absolute pressure to -0.09 MPa, set the operating temperature to 60℃, and perform vacuum constant-temperature evaporation. When the solid phase mass fraction in the crystal slurry reaches 15%, a large number of microcrystals precipitate in the system to form a solid inorganic salt microcrystal carrier suspension, which is kept in circulation for later use; Step 2: Take all the amino acid ion pair buffer mother liquor obtained in Preparation Example 3 as the precursor injection solution; Step 3: Maintain the vacuum crystallizer in a continuous vacuum evaporation state at 60°C as in Step 1, start the metering pump, and inject the precursor injection liquid from Step 2 directly into the high-pressure pipeline section at the outlet of the external circulation pump of the vacuum crystallizer via side-line injection. Control the mass flow rate of the precursor injection liquid to ensure that it is continuously and uniformly injected into the external circulation pipeline of the vacuum crystallizer within a 1.5-hour crystal slurry residence time, maintain continuous feeding and discharging, stabilize the crystal slurry residence time at 1.5 hours, and achieve heterogeneous induced co-crystallization. Step 4: The crystal slurry discharged from the bottom of the vacuum crystallizer in Step 3 is continuously fed into a two-stage pusher centrifuge for solid-liquid separation. The separated process mother liquor is returned to the crystallizer, and the filter cake is collected to obtain wet-based composite salt crystals with a water content of 3%. 10 parts by weight of disodium inosinate are completely dissolved in an appropriate amount of deionized water to prepare a 15% flavor enhancer solution. The wet-based composite salt crystals are fed into a mixer equipped with a plow blade agitator. The stirring speed is set to 60 r / min, and the atomization pressure is set to 0.4 MPa using a high-pressure atomizing nozzle to uniformly spray the flavor enhancer solution onto the surface of the wet-based composite salt crystals. Step 5: Feed the material processed in Step 4 into a fluidized bed dryer, set the hot air inlet temperature to 85°C, adjust the air volume to keep the bed material temperature at 60°C, dry until the product moisture content is less than or equal to 1.5%, cool to room temperature, sieve and classify, and package to obtain the target low-sodium seasoning salt.
[0028] Comparative Examples 1-5: Comparative Example 1: Compared with Example 1, the difference is that the vacuum evaporation co-crystallization and wet phase mesoscopic coating process is not used. Instead, the sodium chloride, potassium chloride, L-arginine, L-glutamic acid, L-histidine, anhydrous citric acid powder and disodium ribonucleotide, which are actually consumed in Example 1, are directly mixed by physical dry method. All other aspects are the same.
[0029] Comparative Example 2: Compared with Example 1, the difference is that L-histidine was not added when preparing the amino acid ion pair buffer mother liquor, and the apparent pH value was adjusted to 5.95 only with anhydrous citric acid aqueous solution. All other aspects are the same.
[0030] Comparative Example 3: Compared with Example 1, the difference is that when preparing the amino acid ion pair buffer mother liquor, anhydrous citric acid aqueous solution was used to forcibly adjust and keep the apparent pH value constant at 4.5, otherwise the same.
[0031] Comparative Example 4: Compared with Example 1, the difference is that instead of using the external circulation pipeline side-line delayed injection, the amino acid ion pair buffer mother liquor and the inorganic high-salt solution are completely mixed in the mixing tank and then pumped together into the continuous vacuum crystallizer for vacuum isothermal evaporation. All other aspects are the same.
[0032] Comparative Example 5: Compared with Example 1, the difference is that instead of wet phase coating after centrifugation, the disodium ribonucleotide is directly mixed into the amino acid ion pair buffer mother liquor, and then injected together into the external circulation pipeline of the continuous vacuum crystallizer to participate in vacuum isothermal evaporation at 62°C. After fluidized bed drying, the finished product is obtained directly. All other aspects are the same.
[0033] Test Examples 1-4: Test Example 1: The mother liquor from Example 1, Comparative Example 2, and Comparative Example 3 during the isothermal evaporation stage in the continuous vacuum crystallizer was selected as the test objects.
[0034] An online pH meter adapted to high-salt and high-temperature environments was installed at the external circulation pipeline of the continuous vacuum crystallizer, and electrode calibration was completed using a standard buffer solution with known pH before formal testing.
[0035] The vacuum constant temperature evaporation program is started. Starting from the solid mass fraction of 0% in the crystal slurry, the apparent pH value of the crystallization mother liquor is continuously and synchronously extracted and recorded at preset solid mass fraction nodes (0%, 3%, 6%, 9%, and 12%, respectively).
[0036] Once the final preset solid-liquid ratio is reached, recording is stopped, and the apparent pH values at each sampling point are compiled to evaluate the acid-base buffering stability of different formulation systems under high ionic strength conditions.
[0037] Table 1. Data on the apparent pH value of crystallization mother liquor with the mass fraction of solid phase in crystal slurry for different formulation systems.
[0038] According to Table 1 and Figure 1 The apparent pH values of the crystallization mother liquor showed significant differences under high-intensity evaporation and concentration conditions. During the continuous vaporization and precipitation of water within the continuous vacuum crystallizer, the intensity of inorganic salt ions within the system increased exponentially. This extreme physicochemical environment easily triggers the Debye-Hückel effect, and the resulting nonlinear abrupt change in activity coefficients usually directly disrupts the existing microscopic acid-base balance of the solution. In Comparative Example 2, due to the lack of L-histidine, relying solely on the initial addition of citric acid for unidirectional acidity adjustment, the apparent pH value dropped sharply from the initial 5.96 to 5.17 when the solid phase mass fraction of the crystal slurry reached 12%. This severe acid shift completely deviated from the thermodynamic stability window necessary for the formation of stable ion pairs between L-arginine and L-glutamic acid, inevitably leading to the disintegration of the original spatial associations and their release into the high-salt mother liquor.
[0039] In routine studies, runaway phenomena are often observed in single-acid-regulated systems during the later stages of concentration. Comparative Example 3, in particular, forcibly adjusted the initial apparent pH to around 4.5, deviating from the isoelectric point. From the outset, the system was unable to foster strong electrostatic attraction and multiple intermolecular hydrogen bonds between the two amino acids. Furthermore, with water evaporation, the acidity further dropped below 3.79, completely losing its structural basis for masking bitterness and enhancing flavor. Example 1, however, demonstrated a strong ability to resist salting-out dissociation. Relying on the highly efficient proton buffer pair constructed from the L-histidine imidazole group and citric acid, even in the face of severe ionic interference from the continuous precipitation of inorganic salts, Example 1 was still able to strictly limit the micro-acidity / alkalinity of the crystal nucleus growth interface within the range of 5.8-6.1. The measured values consistently remained above 5.88, fundamentally ensuring the integrity of the amino acid ion pair structure and providing a solid physicochemical guarantee for subsequent heterogeneous induced co-crystallization.
[0040] Test Example 2: The final products obtained from Example 1, Comparative Example 1, and Comparative Example 4 were selected as the verification test objects.
[0041] Prepare a standard drug dissolution apparatus and inject 900 ml of pre-prepared and constant-temperature artificial saliva at 37°C into six independent dissolution vessels as the dissolution medium. Set the stirring speed to 50 r / min.
[0042] Three groups of finished products of equal mass were accurately weighed and simultaneously placed into their respective dissolution cups. Timing was started from the moment of contact with the liquid surface, and the automatic sampler was triggered to extract 5 ml of solution at the 1st, 5th, 10th, 15th and 30th seconds, respectively. The solution was then immediately filtered through a filter membrane to replenish the isothermal blank medium of equal volume.
[0043] The absolute concentration of L-arginine in the obtained solution samples was determined by high performance liquid chromatography, and the absolute concentration of potassium ions was determined simultaneously by atomic absorption spectrometry. The cumulative dissolution percentage data was calculated and recorded by combining the volume changes at each time point.
[0044] Table 2. Cumulative dissolution percentage test data of different formulation systems in artificial saliva at 37℃
[0045] Depend on Figure 2As can be seen, in Figure (a), the cumulative dissolution percentage curves of potassium ions and L-arginine in the product of the present invention exhibit a high degree of follow-up and overlap. This indicates that the heterogeneous induced co-crystallization process of the present invention successfully eliminates the physical interface between organic and inorganic components, achieving synchronization of dissolution kinetics. In contrast, in Figures (b) and (c), due to the lack of structured integration, the initial dissolution rate of potassium ions is significantly higher than that of amino acids. This imbalance in dissolution rate is the main reason for the instantaneous bitterness experienced upon ingestion of conventional low-sodium salts.
[0046] According to the data in Table 2, the dissolution kinetics of the examples and the comparative examples in the artificial saliva environment showed drastically different release trajectories. The biggest technical obstacle after introducing potassium chloride was not whether it could ultimately mask the bitterness, but whether the masking substance could reach the taste receptors on the tongue side synchronously with potassium ions within an extremely short timescale. Comparative Example 1, prepared by dry physical mixing, exposed an extremely severe release discontinuity phenomenon. Due to the extremely high dissolution rate of potassium chloride, the release rate soared to 26.3% within the first two seconds of contact with the dissolution medium, while at this time, only 4.8% of the L-arginine responsible for steric hindrance masking had dissolved. The strong dissolution time difference directly resulted in the oral cavity receiving a pure and sharp bitter metallic taste signal at the very beginning, and even the slow dissolution of amino acids could not reverse the negative perception already established in the taste center. Even Comparative Example 4, which adopted the co-crystallization approach but lacked a delayed injection design, also failed to avoid the defect of asynchronous dissolution. Due to the intense salt precipitation effect caused by the high salt concentration in the early stage, the organic phase amino acids were forcibly repelled and formed independent nuclei in the boiling mother liquor. The final precipitate was actually still a loose combination of inorganic phase crystals and organic phase powder of different particle sizes.
[0047] The two differ significantly in specific surface area and lattice hydration energy, resulting in the potassium ion release rate still far exceeding that of the masking agent. In contrast, the two dynamic release curves of potassium ions and L-arginine in Example 1 almost completely overlap. Relying on the unique external circulation side-line delayed injection and heterogeneous induced co-precipitation process, the amino acid ion pairs have been firmly embedded in the inorganic salt microcrystal growth steps at the mesoscale, forming a highly dense isomorphically locked state in the physical microstructure. When this composite microcrystal comes into contact with artificial saliva at 37°C, the layer-by-layer collapse and dissolution of the outer inorganic matrix forces the internally encapsulated amino acid ion pairs to be exposed and enter the hydration state simultaneously at a fixed ratio. This allows L-arginine to compete with potassium ions for and occupy the TAS2R bitter taste receptor channel with zero time difference due to its large guanidinium structure, achieving an excellent masking effect from the underlying physical transport logic.
[0048] Test Example 3: The final dried products prepared in Examples 1, 2, 3, Comparative Example 1, and Comparative Example 4 were selected as the experimental objects for this macroscopic physical stability verification.
[0049] Accurately weigh 500 grams (50 parts by weight) of each formula product and place them into transparent standard cylindrical test containers with an inner diameter of 10 cm and a height of 20 cm. Tighten the top cover and secure it to the load clamp of the three-dimensional simulation transport vibration table.
[0050] Set the vibration table operating parameters: vertical amplitude to 3 mm, horizontal amplitude to 2 mm, spindle vibration frequency to 50 Hz, and start the equipment to run continuously for 120 minutes to simulate the mechanical stress and continuous bumps that frequently occur in long-distance logistics on highway trunk lines.
[0051] After the vibration test procedure is completed, let the test container stand at room temperature for 5 minutes to eliminate electrostatic interference. Smoothly remove the top cover and use a multi-layer solid sampling probe with a quantitative groove to vertically insert into the material bed and accurately extract about 5 grams (0.5 parts by weight) of powder sample from the upper quarter, the middle half, and the lower three-quarters of the total height of the material inside the container.
[0052] Independent samples obtained from each spatial level were thoroughly dissolved in an appropriate amount of deionized water and brought to a final volume of 100 ml. The absolute concentrations of sodium and potassium ions in the solution samples were determined using flame photometry. After being converted into the mass fraction of the raw powder, the relative deviation percentage was calculated based on the theoretical balancing values of each formulation.
[0053] Table 3. Test data on the relative deviation of ion content in each spatial level after simulated vibration for different formulation systems.
[0054] Depend on Figure 3 As can be seen, in examples 1-3 prepared using the process of this invention (a) and (b), the relative deviations of sodium and potassium ions at the three sampling points (top, middle, and bottom) of the container are all controlled within ±2%, and the curves tend to be flat. This confirms that through heterogeneous induced co-crystallization, each flavor component has been deeply embedded in the inorganic salt lattice or anchored on the crystal surface, forming a stable structured whole. In contrast, the comparative example using a conventional physical dry mixing process shows a significant gradient change in ion distribution with spatial position, with a deviation of up to about 20%. The experimental results show that this invention effectively overcomes the technical difficulties of easy stratification and uneven composition of traditional low-sodium salts, ensuring the flavor consistency of the product throughout its entire life cycle.
[0055] According to the data in Table 3, after prolonged high-intensity three-dimensional physical vibration, the spatial distribution uniformity of the test samples within the macroscopic container exhibited a hierarchical differentiation pattern. During storage or long-distance transportation, the mixed dry powder, due to differences in apparent density and angle of repose, is highly susceptible to irreversible particle sieving and stratified deposition under the combined effects of gravity and continuous oscillation. The test results of Comparative Example 1 confirmed this common industrial physical shift phenomenon. The finished product, obtained solely through conventional dry mechanical mixing, showed a potassium ion ratio soaring to +18.7% at the upper sampling point of the container, while plummeting to -21.4% at the bottom. Particles with lower density or highly irregular shapes were compressed to the top of the bed during continuous vibration, causing the precisely calibrated healthy salt formula to completely fail at the actual consumer end. Comparative Example 4, using a conventional concentration process, also revealed component dispersion defects. Due to the intense deprivation of active water molecules in the boiling evaporation zone, thermodynamic forces forced the amino acid organic phase to prematurely nucleate homogeneously. The precipitated amino acid organic phase powder has a significantly lower bulk density than the inorganic sodium chloride hard large grains. Under vibration stress, it continuously floats and aggregates towards the top bed layer, causing a severe imbalance in the abnormal enrichment of potassium and sodium ions in the bottom layer. The data measured in the example demonstrates the clear effectiveness of the process improvement. Regardless of whether it is at the top, middle, or bottom of the packaging container, the relative deviation of the targeted ions of the three formulations is consistently and strictly suppressed within an extremely low fluctuation range of ±2.0%.
[0056] A heterogeneous co-precipitation control strategy, introduced via an external circulation pipeline sideline, facilitates the direct embedding of amino acid ions as precursors within the rapidly growing eutectic steps of sodium chloride and potassium chloride. Different basic raw materials assemble into highly homogeneous mesoscopic composites at the crystallization kinetics level, with each individual particle independently achieving a fixed-ratio intercalation of all functional components. This deep lattice-level spatial locking completely eliminates the tendency for internal frictional slippage between free components due to density differences, ensuring that the material maintains the initial active ratio balance even under harsh environmental vibrations for extended periods.
[0057] Test Example 4: The final products prepared in Examples 1, 2, and 3, as well as Comparative Examples 3 and 5, were selected as the test objects for this flavor evaluation and activity verification.
[0058] A panel of fifteen professional sensory evaluators, whose taste thresholds have been rigorously calibrated according to national standards, was recruited. 1.5 grams (0.15 parts by weight) of each formula product were accurately weighed and completely dissolved in 100 ml of purified water at a constant temperature of 35 degrees Celsius to prepare a sample solution simulating the concentration of everyday hot soup.
[0059] A double-blind sensory evaluation method was used. Evaluators rinsed their mouths thoroughly with unsalted baking soda water for 10 minutes before tasting each different liquid. Quantitative evaluation indicators included two parts: the initial bitterness impact intensity within the first three seconds of tasting (0 to 10 points, where 0 represents no bitterness and 10 represents an unbearable, extreme metallic bitterness), and the overall thickness and richness of the salty-umami flavor (0 to 10 points, where 0 represents blandness and 10 represents extremely strong and full-bodied umami). The highest and lowest scores were removed before calculating the average score.
[0060] Take 2.0 g (0.2 parts by weight) of each formulation finished powder, add ultrapure water and sonicate to dissolve and make up to 50 ml. Filter through a 0.22 micron microporous membrane to obtain the test solution.
[0061] A high-performance liquid chromatograph equipped with a UV detector was used, with a reversed-phase C18 column and isocratic elution with potassium dihydrogen phosphate buffer and methanol as the mobile phase to accurately determine the absolute concentrations of disodium 5'-inosinate and disodium 5'-guanylate in the test solution. Based on the overall yield of the final product in the examples and comparative examples and the initial theoretical feed mass of the disodium 5'-flavor enhancer, the true activity retention rate of the target flavor enhancer after all production processes was calculated.
[0062] Table 4. Sensory evaluation scores and retention rate of disodium flavor nucleotide activity of finished products with different formulations
[0063] Depend on Figure 4 As can be seen, in (a) Examples 1-3 of the present invention significantly reduced the initial bitterness of potassium chloride while maintaining a very high salty and umami flavor thickness, which indicates that amino acid ions produced an excellent flavor-masking synergistic effect on the complex in the co-crystallization state; combined with (b), it can be seen that due to the use of a controlled heterogeneous induced co-crystallization environment and a mild dehydration process, the activity retention rate of flavor factors in the examples remained above 90%, which is much higher than that of the comparative examples treated by conventional processes.
[0064] In conclusion, Figure 4 The data, from both subjective sensory and objective physicochemical perspectives, confirm that the present invention not only achieves the structural reshaping of low-sodium salt flavor, but also possesses extremely high process reliability.
[0065] According to the data in Table 4, the microscopic spatial morphology and thermodynamic history of flavor compounds directly determine the flavor characteristics of the final product. The test results of Comparative Example 3 confirm the highly specific requirements of the steric hindrance competition mechanism of amino acids. Due to the forced deviation from a specific pH window during the preparation of the precursor, L-arginine and L-glutamic acid, which should have been tightly associated, completely dissociated in the crystallization mother liquor. The amino acids, having lost their stable supramolecular form, could not preferentially intercept bitter signals due to their large and charge-concentrated unique structure.
[0066] This microscopic structural disintegration directly led to a surge in the initial bitterness score to 6.8 points in macroscopic tasting. The metallic sharpness brought by the high concentration of potassium ions was directly perceived by the evaluators as intensely metallic, severely disrupting the overall flavor balance. Comparative Example 5 exposed the fatal flaws of traditional processes in handling heat-sensitive flavor enhancers when dealing with the extremely sensitive disodium nucleotide. Directly injecting the nucleotide into a micro-negative pressure crystallizer in a boiling evaporation state, under the harsh liquid-phase environment exceeding 60 degrees Celsius and rich in extremely high concentrations of inorganic salt ions and free protons, caused large-scale irreversible hydrolysis of the fragile phosphate ester bonds. The retention rate dropped to 41.6%, and the significant loss of effective umami substances resulted in an overall saltiness score of only 3.8 points, failing to produce the expected synergistic pressurization and flavor masking effects. The example, by cleverly integrating a wet-phase mesoscopic coating process under specific time sequences, effectively resolved the engineering contradiction between high-temperature evaporation and the protection of heat-sensitive substances. In Examples 1 to 3, disodium nucleotides were completely isolated from the region of severe crystallization thermodynamic disruption. Instead, the non-thermal phase in-situ fusion adsorption was achieved by utilizing the three to five percent free micro-water film remaining on the surface of the wet base composite salt after centrifugation, under mild low-shear mixing and low-temperature fluidized bed conditions.
[0067] This highly precise cold-end blending strategy ensures the complete preservation of the biochemical activity of the core umami substances, with a retention rate consistently above 92.7%. Relying on intact flavor nucleotides and pre-mesoscopically locked amino acid buffer pairs, the target product releases an extremely pure and rich savory base flavor the moment it comes into contact with saliva in the mouth, while the initial bitterness is consistently controlled below 1.5 points, demonstrating a superior flavor synergy far exceeding that of conventional physically blended products.
Claims
1. A low-sodium seasoning salt with synergistic effects of compound flavoring agents, characterized in that, Made from the following ingredients in parts by weight: Sodium chloride: 550-600 parts; Potassium chloride: 280-320 parts; Disodium inosinate: 5-10 parts; The amino acid ion pair buffer stock solution is prepared from the following components in parts by weight: L-arginine: 40-60 parts; L-glutamic acid: 40-50 parts; L-histidine: 2-4 parts; Anhydrous citric acid as an acidity regulator.
2. The low-sodium seasoning salt with synergistic effect of compound flavoring agents according to claim 1, characterized in that, The low-sodium seasoning salt is made from the following preferred weight values: Sodium chloride: 570 parts; Potassium chloride: 300 parts; The amino acid ion pair buffer stock solution contained 50 parts of L-arginine, 45 parts of L-glutamic acid, and 3 parts of L-histidine. Disodium inosinate: 8 parts by weight.
3. The low-sodium seasoning salt with synergistic effect of compound flavoring agents according to claim 1, characterized in that, The anhydrous citric acid was pre-prepared into a 30% aqueous solution and added dropwise at a uniform rate to an aqueous solution containing free amino acids, including L-arginine, L-glutamic acid, and L-histidine. The amount of anhydrous citric acid added is determined to adjust and maintain the apparent pH of the amino acid ion-pair buffer mother liquor at 5.80-6.
10.
4. The low-sodium seasoning salt with synergistic effect of compound flavoring agents according to claim 1, characterized in that, The amino acid ion pair buffer stock solution is prepared by the following steps: At 20-25℃, the L-arginine, L-glutamic acid and L-histidine were added to deionized water and stirred at a constant temperature until completely dissolved to obtain an aqueous solution of free amino acids. Using online pH meter feedback control, the anhydrous citric acid aqueous solution is added dropwise to the free amino acid aqueous solution at a uniform rate to form a mixture. The apparent pH value of the mixture is adjusted and kept constant between 5.80 and 6.
10. The mixture is then stirred and mixed evenly to obtain the amino acid ion pair buffer mother liquor.
5. The low-sodium seasoning salt with synergistic effect of compound flavoring agents according to claim 1, characterized in that, The preparation steps of the low-sodium seasoning salt are as follows: Sodium chloride and potassium chloride are dissolved in deionized water to obtain a homogeneous inorganic high-salt solution; the homogeneous inorganic high-salt solution is continuously pumped into a continuous vacuum crystallizer with an external circulation pipeline for vacuum isothermal evaporation; the internal circulation pump of the continuous vacuum crystallizer is turned on; when a large number of microcrystals are precipitated in the continuous vacuum crystallizer to form a solid inorganic salt microcrystal carrier suspension, circulation is maintained for standby. The pre-prepared amino acid ion pair buffer mother liquor was used as the precursor injection solution; Maintaining the continuous vacuum evaporation state of the continuous vacuum crystallizer, the precursor injection liquid is directly injected into the external circulation pipeline via side-line injection to maintain continuous feeding and discharging, thereby achieving heterogeneous induced co-crystallization. The slurry discharged from the bottom of the continuous vacuum crystallizer is continuously fed into a centrifuge for solid-liquid separation, and the filter cake is collected to obtain wet-based composite salt crystals; The disodium nucleotide of flavor is dissolved in the deionized water to prepare a flavor enhancer solution, and the flavor enhancer solution is uniformly sprayed onto the surface of the wet-based composite salt crystal to obtain the material; The sprayed material is sent to a dryer for drying, and after cooling, it is sieved and graded to obtain the low-sodium seasoning salt.
6. The low-sodium seasoning salt with synergistic effect of compound flavoring agents according to claim 5, characterized in that, When preparing the homogeneous inorganic high-salt solution, the temperature is set to 75-80℃, the stirring speed is set to 150-200r / min, and the solution is stirred at a constant temperature for 30-45min until the solid phase is completely dissolved. The absolute pressure inside the continuous vacuum crystallizer is set to -0.08MPa to 0.09MPa, and the operating temperature is set to 60-65℃. Vacuum isothermal evaporation is performed to produce the crystal slurry until the solid phase mass fraction in the crystal slurry reaches 10%-15%, forming the solid inorganic salt microcrystalline carrier suspension.
7. The low-sodium seasoning salt with synergistic effect of compound flavoring agents according to claim 5, characterized in that, The specific operation of the side-line injection method is as follows: Start the metering pump to directly inject the precursor injection liquid into the external circulation pipeline, control the mass flow rate of the precursor injection liquid, and continuously and uniformly inject the precursor injection liquid into the external circulation pipeline during the crystal slurry residence time of 1-1.5h.
8. The low-sodium seasoning salt with synergistic effect of compound flavoring agents according to claim 5, characterized in that, The solid-liquid separation is carried out using a two-stage pusher centrifuge, and the separated process mother liquor is returned to the continuous vacuum crystallizer for recycling. The collected wet-based composite salt crystals have a water content of 3%-5%; The mass fraction of the prepared flavor enhancer solution is 10%-15%.
9. A low-sodium seasoning salt with synergistic effects of compound flavoring agents according to claim 5, characterized in that, The specific operation of uniform spraying is as follows: The wet-based composite salt crystals are fed into a mixer equipped with a plow-blade agitator, and the stirring speed is set to 40-60 r / min. Using a high-pressure atomizing nozzle, the flavor enhancer solution is uniformly sprayed onto the surface of the wet-based composite salt crystals at a set atomization pressure of 0.2-0.4 MPa.
10. A low-sodium seasoning salt with synergistic effects of compound flavoring agents according to claim 5, characterized in that, When drying materials, the dryer is a fluidized bed dryer. The hot air inlet temperature is set to 80-85℃, and the air volume is adjusted to keep the temperature of the bed material at 60-70℃. The product moisture content is dried to ≤1.5%.