Preparation method of odor-reducing glycine chelated magnesium

By adding a flavor-reducing agent at the upstream of glycine magnesium synthesis and optimizing process parameters, the bitterness problem of glycine magnesium was solved, achieving the preparation of glycine magnesium with high bioavailability and good taste, which is suitable for a variety of foods and nutritional supplements.

CN121318752APending Publication Date: 2026-01-13NANTONG LICHENG BIOLOGICAL ENG CO LTD +1
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Patent Information

Application Number
CN202511540000.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-10-27
Publication Date
2026-01-13

AI Technical Summary

Technical Problem

Existing magnesium glycinate has an unpleasant taste and a noticeable bitterness. Current masking methods are limited in effectiveness and costly, which affects bioavailability.

Method used

By optimizing reaction conditions and raw material ratios, flavor-reducing agents such as citric acid, ascorbic acid, or gluconic acid are added at the upstream of glycine magnesium synthesis. Combined with specific spray drying parameters, the bitterness of glycine magnesium is reduced, thus preparing flavor-reduced glycine chelated magnesium.

Benefits of technology

The prepared flavor-reduced magnesium glycine maintains high bioavailability and solubility without relying on additional flavor masking agents, simplifies the production process, reduces costs, and improves taste. It is suitable for use in food products such as tablets, capsules, beverages, and solid drinks.

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Abstract

The invention belongs to the technical field of amino acid salts, and particularly relates to a preparation method of odor-reducing glycine chelated magnesium. According to the invention, the raw material ratio and the preparation process are improved, the high bioavailability of magnesium glycinate is ensured, and meanwhile, the preparation method is different from the existing technology depending on rear-end taste masking, and the bitter taste of magnesium glycinate is reduced from the source by optimizing the reaction conditions and the raw material ratio at the front end of synthesis.
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Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of amino acid salts, and particularly relates to a preparation method of taste-reduced glycine chelated magnesium. BACKGROUND

[0002] Glycine magnesium is a common organic magnesium salt formed by the complexation of magnesium ions and glycine. Compared with inorganic magnesium salts such as magnesium oxide and magnesium sulfate, glycine magnesium has higher solubility and bioavailability, can be better absorbed and utilized by the human body, and is therefore widely used in the fields of drugs, health foods and nutritional supplements. Magnesium, as an essential constant mineral substance for the human body, plays an important role in maintaining the stability of the nervous system, muscle contraction, bone health and various enzyme reaction processes, and has a broad application market.

[0003] Existing glycine magnesium is usually obtained in the form of powder or granules through the complexation reaction of a magnesium salt and a glycine solution, followed by concentration and drying processes. Although such products are superior to most inorganic magnesium salts in terms of absorption efficiency, they have certain defects in terms of taste. Specifically, the bitterness of the metal in glycine magnesium directly leads to a poor experience when taken orally, and the flavor of other components is easily masked in beverage or solid drink formulations, thereby limiting the popularization and application of glycine magnesium in functional foods.

[0004] In order to improve the taste, the existing technology usually adopts the method of adding sweeteners, flavors, embedding or complexing auxiliary materials to mask the bitterness. However, these methods have certain limitations. For example, sweeteners and flavors can only mask the unpleasant flavor to a certain extent and are difficult to completely improve the taste; embedding and complexing techniques can partially isolate the bitter substances, but the process is complex, the cost is high, and the solubility and absorption rate of glycine magnesium may be affected. Therefore, the existing technology still lacks a glycine magnesium preparation method that can balance high bioavailability and good taste. SUMMARY

[0005] Therefore, the purpose of the present application is to provide a taste-reduced glycine magnesium and a preparation method thereof, so as to solve the problems of poor taste and obvious bitterness of existing glycine magnesium, and the limited effect, high cost or affected absorption rate of existing taste-masking methods. By improving the raw material ratio and preparation process, the present application ensures the high bioavailability of glycine magnesium, and unlike the existing technology which relies on post-end taste masking, the present application optimizes the reaction conditions and raw material ratio at the front end of synthesis to reduce the bitterness of glycine magnesium from the source.

[0006] The present application provides a preparation method of taste-reduced glycine chelated magnesium, which comprises the following steps: (1) mixing glycine, a magnesium salt, a taste-reducing agent and water, and stirring and reacting at 70-85°C for 1-3 hours to obtain a reaction solution; The taste-reducing agent is one or more of citric acid, ascorbic acid and gluconic acid; In the present application, the taste-reducing agent is preferably citric acid. (2) filtering the reaction solution obtained in step (1) to obtain a transparent filtrate, and spray drying the filtrate to obtain the taste-reduced glycine magnesium chelate.

[0007] In the present application, the molar ratio of the glycine, the magnesium salt and the taste-reducing agent in step (1) is 1: (0.5-0.6): (0.05-0.1).

[0008] In the present application, the magnesium salt in step (1) includes one or more of magnesium oxide, magnesium hydroxide or magnesium carbonate.

[0009] In the present application, the amount of water used in step (1) is 200-300 liters per kilomole of glycine.

[0010] In the present application, the pore size of the filter used in step (2) is 1 μm.

[0011] In the present application, the spray drying in step (2) is performed at an inlet temperature of 200-220°C, an outlet temperature of 110-120°C and an atomizer speed of 10,000-20,000 r / min.

[0012] In the specific operation of the present application, the spray drying is preferably performed at an inlet temperature of 210-215°C, an outlet temperature of 110-115°C and an atomizer speed of 16,000-18,000 r / min.

[0013] The present application also provides a taste-reduced glycine magnesium chelate, which is prepared by the preparation method described in any one of the above embodiments.

[0014] Compared with the prior art, the present application provides a taste-reduced glycine magnesium chelate with the following advantages: The present application regulates the reaction conditions and the ratio of raw materials at the front end of synthesis, so that the bitter taste of glycine magnesium is reduced during the formation process, and the taste is improved without relying on additional essences, sweeteners or embedding aids. Since no embedding or complexing aids affecting solubility are introduced, the glycine magnesium prepared by the present application has high solubility and bioavailability. At the same time, the process is simple and the cost is low, and the complex taste-masking treatment process at the rear end is effectively avoided, the production process is simplified, the preparation cost is reduced, and industrial application is facilitated. The taste-reduced glycine magnesium has a mild taste and is more suitable for use in tablets, capsules, beverages, solid drinks and other nutritionally fortified foods, thereby improving consumer acceptance and product competitiveness. BRIEF DESCRIPTION OF DRAWINGS

[0015] Figure 1 SEM image of the taste-reduced magnesium glycinate prepared in Example 1; Figure 2 Infrared spectrum of the taste-reduced magnesium glycinate prepared in Example 1; Figure 3 Radar chart for human sensory evaluation; Figure 4 Radar chart for electronic tongue determination. DETAILED DESCRIPTION

[0017] The specific embodiments of the present application will be described below in conjunction with the drawings and examples, but the following examples are only used to illustrate the present application in detail, and do not limit the scope of the present application in any way.

[0018] It should be noted that for the numerical range in the present application, it is understood that each intermediate value between the upper limit and the lower limit of the range is also specifically disclosed. Each smaller range between any stated value or stated range and any other stated value or intermediate value within the stated range is also included in the present application. The upper limit and the lower limit of these smaller ranges can be independently included or excluded from the range.

[0019] In the following examples, the instrument equipment involved, if not specified, is conventional instrument equipment; the reagents involved, if not specified, are conventional commercial reagents; the test methods involved, if not specified, are conventional methods.

[0020] Unless otherwise indicated, all technical and scientific terms used in this specification have the same meaning as commonly understood by one of ordinary skill in the art to which the application pertains. Although methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present application, preferred methods and materials are described. All documents mentioned in this specification are incorporated by reference to disclose and describe in full the methods and / or materials which are described in the cited documents. In the case of conflict between the present specification and any document incorporated by reference, the present specification controls.

[0021] Example 1 Synthesis reaction: Put glycine 150 kg, magnesium oxide 42 kg, citric acid 29 kg and 400 L water into the reaction kettle, start stirring and heat to 75℃, react for 1.5 h; Spray drying: After the solution is transparent, filter it through a 1 μm filter, then spray dry the reaction solution, the inlet air temperature of spray drying is 210℃, the outlet air temperature is 110℃, and the rotation speed is 16000 r / min, to obtain the taste-reduced magnesium glycinate product 240.8 kg.

[0022] The yield is 98.8%, and the magnesium content is 10.34%.

[0023] The SEM of the prepared taste-reduced magnesium glycinate is shown in Figure 1 The SEM image shows that the taste-reduced magnesium glycinate exists in a regular form, is uniformly dispersed, has few impurities, and has high purity.

[0024] The infrared spectrum of the prepared taste-reduced magnesium glycinate is shown in Figure 2 The infrared spectrum shows that the strong wide absorption peak of glycine between 2500 cm -1 and 3100 cm -1 disappears, i.e., the characteristic absorption peak of NH 3+ disappears, and the amino group has undergone a coordination reaction, and the magnesium glycinate is a chelate.

[0025] Example 2

[0026] (1) Synthesis reaction: glycine 150 kg, magnesium hydroxide 60 kg, taste-reducing agent citric acid 29 kg, and 400 L of water were added to a reaction kettle, stirring was started, and the temperature was raised to 75°C, and the reaction was carried out for 1.5 h; (2) Spray drying: after the solution became transparent, filtration was carried out with a 1 μm filter, and then the reaction solution was spray dried, the inlet air temperature of the spray drying was 215°C, the outlet air temperature was 115°C, and the rotation speed was 17000 r / min, to obtain 233.6 kg of the taste-reduced magnesium glycinate product.

[0027] The yield was 96.9%, and the magnesium content was 10.30%.

[0028] Example 3

[0029] (1) Synthesis reaction: glycine 150 kg, magnesium oxide 44 kg, taste-reducing agent ascorbic acid 34 kg, and 450 L of water were added to a reaction kettle, stirring was started, and the temperature was raised to 80°C, and the reaction was carried out for 2 h; (2) Spray drying: after the solution became transparent, filtration was carried out with a 1 μm filter, and then the reaction solution was spray dried, the inlet air temperature of the spray drying was 215°C, the outlet air temperature was 115°C, and the rotation speed was 18000 r / min, to obtain 249.2 kg of the taste-reduced magnesium glycinate product.

[0030] The yield was 98.27%, and the magnesium content was 10.41%.

[0031] Example 4

[0032] (1) Synthesis reaction: glycine 150 kg, magnesium carbonate 92.4 kg, taste-reducing agent gluconic acid 39 kg, and 600 L of water were added to a reaction kettle, stirring was started, and the temperature was raised to 85°C, and the reaction was carried out for 2.5 h; (2) Spray drying: After the solution is transparent, filter it with a 1 μm filter, then spray dry the reaction solution, with an inlet temperature of 220°C, an outlet temperature of 115°C, and a rotation speed of 17000 r / min, to obtain 252.3 kg of the reduced-taste magnesium glycinate product.

[0033] The yield was 98.15%, and the magnesium content was 10.27%.

[0034] Comparative Example 1 Reduced-taste effect in aqueous solution 1. Materials: Sample A: reduced-taste magnesium glycinate prepared in Example 1 of the present application Control B: conventional magnesium glycinate commercially available Solvent: pure water 2. Instruments Electronic tongue system (ASTREE: with bitter, astringent, umami, sweet, and salty sensors) 3. Sample preparation Dissolve the reduced-taste magnesium glycinate and the control magnesium glycinate in water to prepare aqueous solutions with a Mg concentration of 0.01%, 0.03%, and 0.05%, and shake well for use.

[0035] 4. Sensory evaluation 4-1 Human sensory evaluation (1) Recruit 10-15 healthy adult volunteers for random blind testing.

[0036] (2) Before tasting each sample, the volunteers rinse their mouths with water.

[0037] (3) Use a 5-point scale to rate the taste of bitterness, astringency, umami, sweetness, and irritation: 0—no taste; 1—slight; 2—moderate; 3—obvious; 4—very obvious Calculate the average score for each sample and compare the taste differences between the reduced-taste magnesium glycinate and the control magnesium glycinate.

[0038] 4-2 Electronic tongue test method (1) Calibrate the electronic tongue, and use standard solutions for sensor rinsing and baseline setting.

[0039] (2) Measure each sample three times, with each measurement lasting 120 seconds, and take the average value of the stable interval signals.

[0040] (3) Record the response signals of various taste sensors.

[0041] Example 1

[0042] (1) The human sensory evaluation data are shown in Table 1 and Figure 3 .

[0043] Table 1 Human sensory evaluation data

[0044] (2) Electronic tongue determination data as shown in Table 2 and Figure 4

[0045] Table 2 Electronic tongue determination data

[0046] Conclusion: Human sensory evaluation shows that the bitterness, astringency and irritation of the taste-reduced magnesium glycinate of the present application at various concentrations are significantly lower than those of the control magnesium glycinate. The electronic tongue determination results are consistent with the sensory evaluation, quantitatively proving that the present application has a significant taste-reducing effect in aqueous solution. This experiment fully supports the feasibility and superiority of the application in the food, beverage and pharmaceutical fields.

[0047] Example 2 Taste reduction in solid drinks 1. Materials: Sample A: taste-reduced magnesium glycinate prepared in Example 2 of the present application; Control B: conventional commercially available magnesium glycinate, white granulated sugar, soluble starch.

[0048] 2. Sample preparation According to the formula, mix the magnesium glycinate or taste-reduced magnesium glycinate with other solid raw materials (such as white granulated sugar, soluble starch, etc.) uniformly.

[0049] 3-1 Human sensory evaluation (1) Recruit 10-15 healthy adult volunteers for random blind test.

[0050] (2) Before tasting the sample each time, the volunteers rinse their mouths with water.

[0051] (3) Use a 5-point scale to rate the taste bitterness, astringency, aftertaste, and overall taste: 1—very obvious; 2—obvious; 3—moderate; 4—mild; 5—no taste.

[0052] 3-2 Electronic tongue test method Use a multi-channel electronic tongue system to determine the bitterness, astringency and saltiness response of the sample, with consistent concentration, and repeat the determination three times to take the average value. The electronic tongue test data are shown in Table 3.

[0053] Table 3 Electronic tongue test data

[0054] ​Compared with the control group, the solid drink prepared using the taste-reduced magnesium glycinate has significantly reduced bitter taste and astringent taste, and the overall mouthfeel is significantly improved. The electronic tongue results are consistent with the sensory scores, verifying the taste-reducing effect. The comparative example shows that the taste-reduced magnesium glycinate can be directly applied in the solid drink, realizing front-end taste reduction, without the need for additional taste-masking agents, and significantly improving the mouthfeel of the product.

[0055] The above describes the present application and its embodiments, which are not restrictive, and the specific embodiments shown are only some of the embodiments of the present application, not all the embodiments, and the actual structure is not limited thereto. In general, if a person skilled in the art is inspired thereby, without departing from the purpose of the present application, without creative design, similar structure and embodiments of the technical solutions can be designed, which should belong to the protection scope of the present application.

Claims

1. A method for preparing glycine-chelated magnesium with reduced flavor, characterized in that, The preparation method includes the following steps: (1) Mix glycine, magnesium salt, flavor reducer and water, and stir at 70℃~85℃ for 1~3 hours to obtain reaction solution; The flavor-reducing agent is one or more of citric acid, ascorbic acid, and gluconic acid; (2) Filtration step (1) The reaction solution obtained in step (1) is filtered to obtain a transparent filtrate. The filtrate is spray-dried to obtain glycine chelated magnesium with reduced flavor.

2. The preparation method according to claim 1, characterized in that, The molar ratio of glycine, magnesium salt and flavor reducer in step (1) is 1:(0.5~0.6):(0.05~0.1).

3. The preparation method according to claim 1, characterized in that, The magnesium salt mentioned in step (1) includes one or more of magnesium oxide, magnesium hydroxide, or magnesium carbonate.

4. The preparation method according to claim 1, characterized in that, The amount of water used in step (1) is 200-300 liters of water per kilomoles of glycine.

5. The preparation method according to claim 1, characterized in that, The pore size of the filter described in step (2) is 1 μm.

6. The preparation method according to claim 1, characterized in that, In step (2), the inlet air temperature of the spray dryer is 200℃~220℃, the outlet air temperature is 110℃~120℃, and the atomizer speed is 10000~20000 r / min.

7. A flavor-reducing glycine chelated magnesium, characterized in that, The flavor-reduced glycine chelated magnesium is prepared by the preparation method described in any one of claims 1 to 6.