Process for the preparation of ferrous glycinate without significant iron taste in liquid dosage products

Abstract

The application discloses a preparation method of glycine ferrous without obvious iron smell in a liquid agent product, and relates to the technical field of food or health product processing. The method comprises the following steps: preparing a first solution by hot water swelling of gamma-cyclodextrin; preparing a second solution by adding glycine ferrous and vitamin C or citric acid into the first solution after cooling; preparing a third solution by dissolving soluble soybean polysaccharide or pectin in water and then adding malt dextrin; and then slowly adding the second solution into the third solution, and then performing high-pressure homogenization and spray drying. Through the synergistic effect of gamma-cyclodextrin inclusion, acidic auxiliary protection and double embedding of a film forming agent, the prepared glycine ferrous is clear and free of precipitation in hot water, has no obvious iron smell, and has a significantly improved absorption rate, and is particularly suitable for liquid dosage forms such as oral liquids.

Description

Technical Field

[0001] This invention relates to the field of food or health product processing technology, and more specifically to a method for preparing ferrous glycinate without a noticeable metallic taste in a liquid product. Background Technology

[0002] Iron is one of the essential trace elements for the growth and development of animals and humans. It participates in energy metabolism, carrier composition, transport and storage of nutrients, and immune function in the body. It is also an important component and activator of many enzymes in the body's biochemical reactions.

[0003] Amino acid chelated iron has a high bioavailability in animals, equivalent to 125-185% of the same level of ferrous sulfate. Glycine is the smallest amino acid in terms of molecular weight, so ferrous glycinate should be more easily absorbed and utilized in the body. However, commercially available ferrous glycinate often produces a flocculent precipitate when added to hot water, and has a noticeable irony taste, resulting in a poor palatability, which limits its application.

[0004] Among the currently disclosed technologies, patent CN120678225A mainly masks the metallic taste through encapsulation technology, without addressing improvements in solubility or absorption rate. Patents CN112544976A and CN107320487A both employ grinding followed by granulation, primarily masking the metallic taste through the addition of flavoring agents. However, this involves excessive additives, a fixed formula, and is suitable for single-product output, not for use as raw materials. Furthermore, the process is complex and time-consuming.

[0005] Therefore, it is necessary to propose a method for preparing ferrous glycinate without a noticeable iron smell in liquid products to solve the above problems. Summary of the Invention

[0006] The purpose of this invention is to solve the problems of existing ferrous glycinate products, such as easy formation of flocculent precipitate, obvious iron smell, and poor absorption rate after high-temperature heating when applied to liquid dosage forms.

[0007] To achieve the above objectives, the present invention specifically adopts the following technical solution:

[0008] A method for preparing ferrous glycinate in liquid form without a noticeable metallic odor, comprising the following raw materials by weight percentage: 22-25% ferrous glycinate, 5-10% acidic excipients, 30-40% γ-cyclodextrin, 1-3% film-forming agent, and the balance being maltodextrin, including the following steps:

[0009] a. Add γ-cyclodextrin to hot water and allow it to swell to obtain the first solution;

[0010] b. Dry mix ferrous glycinate with an acidic excipient, add the first solution after it has cooled down, mix well to obtain a second solution, wherein the acidic excipient is vitamin C or citric acid;

[0011] c. Dissolve the film-forming agent in water, then add maltodextrin to dissolve it, to obtain a third solution, wherein the film-forming agent is soluble soybean polysaccharide or pectin;

[0012] d. Slowly add the second solution to the third solution, stir until homogeneous, and then perform high-pressure homogenization to obtain a homogeneous liquid;

[0013] e. Spray dry the homogenized liquid and collect the dried product to obtain ferrous glycinate in the liquid product without a distinct iron smell.

[0014] The above-mentioned technical solution of the present invention utilizes the macromolecular cavity of γ-cyclodextrin to initially encapsulate ferrous glycine, leveraging its molecular capsule properties to isolate the metallic odor and improve stability. Simultaneously, vitamin C or citric acid is introduced to provide an acidic microenvironment, promoting the dissolution of ferrous glycine and inhibiting the oxidation of ferrous ions. Furthermore, soluble soybean polysaccharides or pectin are used as outer film-forming agents to form a dense protective film on the microcapsule surface, achieving double encapsulation. Finally, high-pressure homogenization ensures uniform nanoscale dispersion of all components, followed by rapid spray drying for molding. This synergistic effect achieves the following: clarity without precipitation in a liquid environment, especially after heating; effective masking of the metallic odor; and significantly improved bioavailability of iron.

[0015] Preferred solution

[0016] Furthermore, in step a, the temperature of the hot water is above 75°C.

[0017] Furthermore, in step b, the first solution is cooled to 50-60°C.

[0018] Furthermore, the weight percentages of each raw material are as follows: ferrous glycine 23-24%, the acidic excipients 6-8%, γ-cyclodextrin 33-37%, and the film-forming agent 1.5-2.5%.

[0019] Furthermore, the ferrous glycine content is 24%, the acidic excipient content is 6%, the γ-cyclodextrin content is 35%, and the film-forming agent content is 2%.

[0020] Furthermore, in step d, the pressure of the high-pressure homogenization is 40-60 MPa, and the time is 3-8 minutes.

[0021] Furthermore, in step e, the inlet air temperature of the spray dryer is 160-180℃, and the outlet air temperature is 90-100℃.

[0022] Furthermore, after step e, the process also includes passing the dried product through an 80-mesh sieve.

[0023] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0024] 1. The ferrous glycinate prepared by this invention becomes clear and transparent after dissolving in hot water at 60-90℃, without any flocculent precipitate. After 3 months of accelerated testing, its sensory score for the iron-smelling odor is significantly lower than that of the control sample. In vitro absorption rate evaluation shows that its iron absorption rate is much higher than that of untreated ferrous glycinate raw material and the control sample with improper formulation. This invention achieves simultaneous improvement in water solubility, taste masking effect, and absorption rate through the synergistic effect of specific components and processes, and is especially suitable for dosage forms such as liquid oral liquids with stringent requirements for sensory and stability.

[0025] 2. This invention achieves a synergistic effect through the molecular inclusion of γ-cyclodextrin, the acidic protection and solubilization of vitamin C / citric acid, and the physical barrier of the outer film-forming agent. The absence of any one of these three components or an improper ratio will lead to a sharp decline in the masking and stabilizing effects. Attached Figure Description

[0026] Figure 1 This is a diagram showing the dissolution effect of the glycine ferrous microcapsule powder prepared in Example 2 of the present invention compared with that of untreated glycine ferrous raw material.

[0027] Figure 2 This is a schematic diagram showing the absorption rate of glycine ferrous microcapsule powder prepared in Example 2 of the present invention and untreated raw materials at different concentrations. Detailed Implementation

[0028] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. 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 of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0029] Example 1

[0030] This embodiment provides a method for preparing ferrous glycinate without obvious iron smell in a liquid product. The raw material ratio is: ferrous glycinate 22%, vitamin C 5%, γ-cyclodextrin 30%, soluble soybean polysaccharide 1%, and maltodextrin 42%.

[0031] Preparation steps:

[0032] 1. Add γ-cyclodextrin to hot water at 80℃ and stir until completely swollen to obtain solution 1.

[0033] 2. Mix ferrous glycinate and vitamin C thoroughly. Once the temperature of solution 1 has dropped to 50°C, add the dry mixture to it, stir to dissolve, and obtain solution 2.

[0034] 3. Dissolve soluble soybean polysaccharide in water, then add maltodextrin to dissolve, to obtain solution 3.

[0035] 4. While stirring, slowly add solution 2 to solution 3. After mixing evenly, homogenize under high pressure at 50 MPa for 5 minutes to obtain a homogenized solution.

[0036] 5. Set the spray dryer's inlet air temperature to 170℃, outlet air temperature to 95℃, and atomizer frequency to 330Hz. After the temperature stabilizes, pump in the homogenized liquid for spray drying. Collect the outlet material and pass it through an 80-mesh sieve to obtain the final product.

[0037] Example 2

[0038] The difference between this embodiment and Example 1 lies in the ratio of raw materials: 24% ferrous glycine, 6% vitamin C, 35% γ-cyclodextrin, 2% pectin, and 33% maltodextrin. Other steps and parameters are the same as in Example 1.

[0039] Example 3

[0040] The difference between this embodiment and Example 1 lies in the ratio of raw materials: 25% ferrous glycine, 10% citric acid, 40% γ-cyclodextrin, 3% pectin, and 22% maltodextrin. Other steps and parameters are the same as in Example 1.

[0041] Comparative Examples 1-8

[0042] The raw material ratios of Comparative Examples 1-8 were performed according to the table below, deviating from the ratio range required by this invention. For example, the proportion of ferrous glycine was 20% or 26%, the proportion of vitamin C / citric acid was 4% or 11%, and the proportion of γ-cyclodextrin was 40%. The preparation process was the same as that of Example 1. Comparative Examples 1-4 used pectin, and Comparative Examples 5-8 used soluble soybean polysaccharides.

[0043]

[0044] Performance Testing and Evaluation

[0045] Evaluation of the metallic odor of the liquid: 10g of the microcapsule powder prepared in each example and comparative example was added to 100mL of water at 60℃ and stirred until evenly dispersed. The solution was then stored in an accelerated testing chamber for 3 months at 40℃ and 75% humidity. Each month, 10 sensory evaluators scored the metallic odor of the solution from 0 to 10 points, with higher scores indicating a stronger metallic odor. The average score was taken. The results are shown in Table 1.

[0046] Solubility observation: Take the sample from Example 2 and the untreated ferrous glycine raw material, prepare an aqueous solution of 1 mg / mL, heat and sterilize at 90°C for 20 minutes, and observe the state of the solution.

[0047] Absorption rate evaluation: The iron absorption rate of the sample from Example 2 and the untreated raw material at different concentrations was evaluated using the Caco-2 cell model. Results are shown in Table 2 or... Figure 2 .

[0048] Result comparison:

[0049] Table 1. Accelerated test scores for metallic taste of samples with different ratios

[0050]

[0051] Solubility observation: such as Figure 1 As shown, the sample in Example 2 was clear and transparent after dissolution; the untreated raw material solution had obvious flocculent precipitate.

[0052] Absorption rate evaluation: as shown in Table 2 or Figure 2 As shown, the iron absorption rate of the sample in Example 2 was significantly higher than that of the untreated ferrous glycine group at all test concentrations.

[0053] Table 2. Iron absorption rate (%) for each group at different concentrations

[0054]

[0055] in conclusion

[0056] As shown in Table 1, the formulations of Examples 1-3 fall within the scope of protection claimed by this invention, and their iron odor scores remained below 2 points after 3 months of accelerated testing, demonstrating excellent stability. In contrast, the formulations of Comparative Examples 1-8 exceeded the range, resulting in a rapid increase in iron odor scores, especially a noticeable fishy smell appearing after 2-3 months. Combined with the absorption rate data, this demonstrates that only under the specific components and formulations defined by this invention, and through a specific preparation process, can a synergistic effect of masking odor, dissolving, and promoting absorption be achieved.

[0057] The above are merely preferred embodiments of the present invention and are not intended to limit the present invention. The scope of patent protection of the present invention shall be determined by the claims. Similarly, any equivalent structural changes made based on the content of the present invention's specification shall also be included within the scope of protection of the present invention.

Claims

1. A method for preparing ferrous glycinate in liquid products without a noticeable iron odor, wherein the raw materials used, by weight percentage, include: The product comprises 22-25% ferrous glycine, 5-10% acidic excipients, 30-40% γ-cyclodextrin, 1-3% film-forming agent, and the balance being maltodextrin. Its characteristic feature is that it includes the following steps: a. Add γ-cyclodextrin to hot water and allow it to swell to obtain the first solution; b. Dry mix ferrous glycinate with an acidic excipient, add the first solution after it has cooled down, mix well to obtain a second solution, wherein the acidic excipient is vitamin C or citric acid; c. Dissolve the film-forming agent in water, then add maltodextrin to dissolve it, to obtain a third solution, wherein the film-forming agent is soluble soybean polysaccharide or pectin; d. Slowly add the second solution to the third solution, stir until homogeneous, and then perform high-pressure homogenization to obtain a homogeneous liquid; e. Spray dry the homogenized liquid and collect the dried product to obtain ferrous glycinate in the liquid product without a distinct iron smell.

2. The method for preparing ferrous glycinate without a distinct iron odor in the liquid product according to claim 1, characterized in that, In step a, the temperature of the hot water is above 75°C.

3. The method for preparing ferrous glycinate without a distinct iron odor in the liquid product according to claim 1 or 2, characterized in that, In step b, the first solution is cooled to 50-60°C.

4. The method for preparing ferrous glycinate without a distinct iron odor in the liquid product according to claim 3, characterized in that, The weight percentages of each raw material are as follows: ferrous glycine 23-24%, the acidic excipients 6-8%, γ-cyclodextrin 33-37%, and the film-forming agent 1.5-2.5%.

5. The method for preparing ferrous glycinate without a distinct iron odor in the liquid product according to claim 4, characterized in that, The content of ferrous glycine is 24%, the content of acidic excipients is 6%, the content of γ-cyclodextrin is 35%, and the content of film-forming agent is 2%.

6. The method for preparing ferrous glycinate without a distinct iron odor in the liquid product according to claim 1, characterized in that, In step d, the pressure of the high-pressure homogenization is 40-60 MPa, and the time is 3-8 minutes.

7. The method for preparing ferrous glycinate without a distinct iron odor in the liquid product according to claim 1, characterized in that, In step e, the inlet air temperature of the spray dryer is 160-180℃, and the outlet air temperature is 90-100℃.

8. The method for preparing ferrous glycinate without a distinct iron odor in the liquid product according to claim 1, characterized in that, After step e, the process also includes passing the dried product through an 80-mesh sieve.

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