Ferrous glycinate and EDTA (Ethylene Diamine Tetraacetic Acid) ferric sodium compound product and preparation method thereof

Abstract

The invention discloses a ferrous glycinate and EDTA ferric sodium compound product and a preparation method thereof. The compound product comprises a core material and a double-layer wall material, the core material is prepared from ferrous glycinate and EDTA (Ethylene Diamine Tetraacetic Acid) ferric sodium; the inner-layer wall material is cyclodextrin and Arabic gum; the outer-layer wall material is pectin and hydroxypropyl methyl cellulose; in the compound product, the mass percentage content of the ferrous glycinate is 20%-25%; the mass percentage content of the EDTA ferric sodium is 8%-10%; the mass percentage content of the inner-layer wall material is 60%-70%; and the mass percentage of the outer layer wall material is 2-5%. The EDTA ferric sodium and the ferrous glycinate are compounded to serve as the core material, and the double-layer embedding wall material is adopted, so that the iron fishy smell of the ferrous glycinate can be effectively covered on the basis of relatively high iron absorption and utilization rate, and relatively good stability can be achieved when the iron-iron composite material is applied to a liquid preparation product.

Description

Technical Field

[0001] The invention belongs to the technical field of food processing, and particularly relates to a compound product of ferrous glycinate and sodium ferric EDTA and a preparation method thereof. Background Art

[0002] Iron is a trace element essential for the growth and development of animals and humans. It participates in energy metabolism, carrier composition, nutrient transport and storage, and immune function. It is a key component and activating factor for many enzymes in biochemical reactions.

[0003] Amino acid chelated iron has a high bioavailability in animals, equivalent to 125% to 185% of the same level of ferrous sulfate. Glycine is the smallest amino acid, making ferrous glycine more easily absorbed and utilized in the body. Sodium EDTA, as an iron supplement, is widely used in food, health products, dairy products, pharmaceuticals, and other fields. Its high absorption rate can avoid the obstruction of iron absorption by substances such as phytic acid. Sodium EDTA also promotes the absorption of other iron sources in the diet or endogenous iron sources. However, the ferrous glycine commonly available on the market has a noticeable iron smell and a poor taste, which limits its application. Currently, several papers have introduced the preparation of ferrous glycine microcapsule powder, but there is no research on solving the iron smell, which has prevented ferrous glycine from being widely used.

[0004] Therefore, it is an urgent problem to prepare a compound product of ferrous glycinate and sodium ferrous EDTA that has no obvious iron smell and is used in liquid preparation products, and it can meet market demand. Summary of the Invention

[0005] The purpose of the present invention is to provide a compound product of ferrous glycinate and sodium ferric EDTA and a preparation method thereof in order to solve the deficiencies of the prior art.

[0006] The purpose of the present invention is achieved by the following technical solutions:

[0007] A compound product of ferrous glycinate and sodium ferric EDTA, comprising a core material and a double-wall material;

[0008] The core material is ferrous glycinate and sodium ferric EDTA;

[0009] The inner wall material is cyclodextrin and gum arabic;

[0010] The outer wall material is pectin and hydroxypropyl methylcellulose;

[0011] In the compound product, the mass percentage of the ferrous glycinate is 20% to 25%; the mass percentage of the sodium ferric EDTA is 8% to 10%; the mass percentage of the inner wall material is 60% to 70%; and the mass percentage of the outer wall material is 2% to 5%.

[0012] The mass ratio of the cyclodextrin and the gum arabic in the inner wall material is (2-4):1;

[0013] The mass ratio of the pectin and the hydroxypropyl methylcellulose in the outer wall material is (1.5-2.5):1.

[0014] Preferably, the pectin is high-ester pectin with an esterification degree ≥50%.

[0015] Preferably, the gum arabic is gum arabic with an AGP content of not less than 17%.

[0016] The preparation method of the composite product of ferrous glycinate and sodium ferric EDTA as described above comprises the following steps:

[0017] S1. Add cyclodextrin and gum arabic to water and allow to fully swell to obtain Solution I;

[0018] S2. While stirring, slowly add the ferrous glycine and EDTA-sodium iron mixture to Solution I to obtain Solution II;

[0019] S3. Using water as the solvent, first fully swell the pectin and hydroxypropyl methylcellulose, then add solution II and stir until completely dissolved and dispersed;

[0020] S4. Then perform high pressure homogenization;

[0021] S5. Finally, spray drying is performed to obtain a compound product.

[0022] Preferably, step S3 uses hot water at 60°C to 80°C.

[0023] Preferably, the mass percentage of solid content of the solution II is 30% to 35%.

[0024] Preferably, the first-level homogenization pressure in step S4 is 8 MPa to 12 MPa, and the second-level pressure is 45 MPa to 55 MPa. Under this homogenization condition, homogenization is performed for 3 to 7 minutes.

[0025] Preferably, the spray drying air inlet temperature in step S5 is 165°C to 175°C, and the air outlet temperature is 90°C to 100°C.

[0026] Preferably, step S5 further includes a sieving step after spray drying, and the sieving mesh size is 60-100 mesh.

[0027] This application uses a compound of sodium ferric EDTA and ferrous glycinate as the core material, and adopts a double-layer embedding wall material. On the basis of having a high iron absorption and utilization rate, the iron smell of ferrous glycinate can be effectively masked. Moreover, the wall materials used in this application are all soluble materials. After homogenization, they have a good embedding effect on sodium ferric EDTA and ferrous glycinate. When used in liquid preparation products, no precipitation will occur, and the embedding effect on the iron smell will not be weakened, and it has good stability. DETAILED DESCRIPTION

[0028] The invention discloses a compound product of ferrous glycinate and sodium ferric EDTA, comprising a core material and a double-layer wall material.

[0029] The core material is ferrous glycinate and sodium ferric EDTA;

[0030] The inner wall material is cyclodextrin and gum arabic;

[0031] The outer wall material is pectin and hydroxypropyl methylcellulose;

[0032] The mass percentage of ferrous glycinate is 20% to 25%; the mass percentage of sodium ferric EDTA is 8% to 10%; the mass percentage of the inner wall material is 60% to 70%; and the mass percentage of the outer wall material is 2% to 5%.

[0033] This application uses a compound of ferrous glycine and sodium iron EDTA, and the total iron content is maintained between 5.8% and 6.5%. Among them, sodium iron EDTA has no obvious iron smell, and can avoid the obstruction of phytic acid and other substances on the absorption of ferrous glycine, thereby promoting the absorption of ferrous glycine by the human body. After ferrous glycine and sodium iron EDTA are compounded, they can cooperate with each other during the absorption process, further improving the overall absorption rate of iron.

[0034] A double-layer encapsulation technique is then employed. First, macromolecular cyclodextrin and gum arabic are used as the inner wall materials. The most notable characteristic of cyclodextrin is that, as a host, it can form inclusion compounds with a wide variety of guest substances. The iron complex can enter the cyclodextrin cavity, forming inclusion compounds that mask the iron odor. Gum arabic is a typical natural plant hydrophilic colloid with excellent emulsification and film-forming properties. Once the iron complex and cyclodextrin are encapsulated, a first encapsulation layer forms on the outside. Gum arabic also enhances the cyclodextrin's encapsulation capacity. Pectin and hydroxypropyl methylcellulose are then used as the second encapsulation layer to further mask the iron odor. Pectin, especially high-ester pectin (DE ≥ 50%), has high film-forming and ductile properties. During the spray drying process, it quickly solidifies on the surface to form a dense film. This soft, elastic film increases the toughness of the capsule wall. Pectin also offers a better taste than other film-forming products. Its presence as the outermost layer effectively mitigates the unpleasant flavor of ferrous glycinate. Hydroxypropyl methylcellulose (HPMC) has thermogel properties. When heated, its aqueous solution forms a gel that precipitates, then dissolves upon cooling. After spray drying, it forms a thin film that adheres to the surface of the iron salt mixture, further masking the iron smell. Therefore, pectin and hydroxypropyl methylcellulose are placed in the outer layer to combine and form a dense film, fully masking the iron smell.

[0035] Therefore, the present application adopts sodium ferric EDTA and ferrous glycine for compounding as core material, and adopts double-layer embedding wall material, on the basis of having higher iron absorption utilization rate, can effectively mask the iron smell of ferrous glycine. Moreover, the wall materials adopted in the present application are all soluble materials. After homogenization treatment, they have good embedding effect on sodium ferric EDTA and ferrous glycine, and no precipitation will occur when applied to liquid preparation products. The compounded iron will not be released when embedded in the cyclodextrin cavity. At the same time, gum arabic, pectin, and hydroxypropyl methylcellulose have a certain viscosity after being dissolved in water, and still have film-forming properties, so the embedding effect on the iron smell will not deteriorate, and has good stability.

[0036] The amount of core material and wall material should be appropriate. If the amount of core material is too low, the iron loading rate is low, and if the amount is too high, the embedding effect is affected. If the amount of wall material is too low, the embedding effect is not achieved. However, the amount should not be too high, otherwise it will not only reduce the iron loading rate but also affect the product yield.

[0037] Experiments were conducted using different ratios of cyclodextrin and gum arabic (other conditions being the same), and the results are shown in Table 1.

[0038] Table 1

[0039]

[0040] As shown in Table 1, the ratio of the two raw materials in the inner wall material significantly affects the encapsulation effect. When the mass ratio of cyclodextrin to gum arabic is (2-4):1, the iron odor masking effect is better and the product yield is higher. This indicates that the inner wall material, which is primarily composed of cyclodextrin, can better encapsulate the complex iron and effectively utilize the gum arabic's promoting effect on cyclodextrin inclusion.

[0041] Experiments were conducted using pectin and hydroxypropyl methylcellulose at different ratios (other conditions being the same), and the results are shown in Table 2.

[0042] Table 2

[0043]

[0044] As can be seen in Table 2, the ratio of the two raw materials in the outer wall material also has a significant impact on the embedding effect solution. When the mass ratio of pectin to hydroxypropyl methylcellulose in the outer wall material is (1.5-2.5):1, the masking effect of the iron odor is better. A more preferred ratio is 2.5:1, which not only has a good masking effect on the iron odor, but also has a higher product yield.

[0045] Preferably, the gum arabic is gum arabic with an AGP content of not less than 17%. The emulsification effect and film-forming property of the gum arabic rich in AGP are better than those of ordinary gum arabic.

[0046] The present application also provides a method for preparing the composite product of ferrous glycinate and sodium ferric EDTA, comprising the following steps:

[0047] S1. Add cyclodextrin and gum arabic to water and allow to fully swell to obtain Solution I;

[0048] S2. While stirring, slowly add the ferrous glycine and EDTA-sodium iron mixture to Solution I to obtain Solution II;

[0049] S3. Using water as a solvent, pectin and hydroxypropyl methylcellulose are first fully swollen, and then solution II is added and stirred until completely dissolved and dispersed; preferably, hot water at 60 ℃ to 80 ℃ is used to promote the swelling of pectin and hydroxypropyl methylcellulose; preferably, the mass percentage of solids in solution II is 30% to 35%;

[0050] S4. High-pressure homogenization is then performed; preferably, the first-level homogenization pressure is 8Mpa to 12Mpa, and the second-level pressure is 45Mpa to 55Mpa. Under these homogenization conditions, homogenization is performed for 3 to 7 minutes; the high-pressure homogenization process is used to make the particles finer, further promote the embedding effect of the composite iron, thereby reducing the iron smell; the homogenization pressure should not be too large, otherwise it will cause excessive shear stress, destroy the product structure, and affect the product yield.

[0051] S5. Finally, spray drying is performed to obtain a composite product; preferably, the spray drying air inlet temperature is 165°C to 175°C, and the air outlet temperature is 90°C to 100°C.

[0052] In order to ensure the uniformity of the product particles, a sieving step is also included after spray drying, and the sieving mesh number is 60 mesh to 100 mesh.

[0053] Example 1

[0054] This embodiment provides a compound product of ferrous glycinate and sodium ferric EDTA, including a core material and a double-wall material.

[0055] The core material is ferrous glycinate and sodium ferric EDTA;

[0056] The inner wall material is cyclodextrin and gum arabic, wherein the mass ratio of cyclodextrin to gum arabic is 3:1;

[0057] The outer wall material is pectin and hydroxypropyl methylcellulose; the mass ratio of pectin to hydroxypropyl methylcellulose is 5:2;

[0058] The contents of ferrous glycinate, sodium ferric EDTA, inner wall material and outer wall material in the product are shown in Table 1.

[0059] The compound product was prepared by following the steps below using the above formula:

[0060] S1. Add cyclodextrin and gum arabic to water and allow to fully swell to obtain Solution I;

[0061] S2. While stirring, slowly add the ferrous glycine and EDTA-sodium iron mixture to Solution I to obtain Solution II;

[0062] S3. Using 70°C water as the solvent, pectin and hydroxypropyl methylcellulose were first fully swollen, and then solution II was added and stirred until completely dissolved and dispersed; the mass percentage of solids in solution II was 33%;

[0063] S4. Perform high-pressure homogenization; the first-level homogenization pressure is 10 MPa and the second-level pressure is 50 MPa. Under these homogenization conditions, homogenize for 5 minutes;

[0064] S5. Spray drying is performed with an inlet air temperature of 170°C and an outlet air temperature of 95°C;

[0065] S6. Pass through an 80-mesh sieve to obtain a compound product.

[0066] Different compound products were produced by selecting different formulas and process parameters. The formulas and process parameters are shown in Table 3. The obtained compound products were then tested, and the results are shown in Table 3.

[0067] Table 3

[0068]

[0069] As can be seen from Table 3, when different amounts of core material, inner wall material and outer wall material are used, as well as when different process parameters are used, there is a significant impact on the iron smell masking effect and product yield of the product. When the amount of EDTA sodium iron and ferrous glycine is too large (reference comparative examples 1-2), the amount of inner wall material is too low (reference comparative example 5), and the amount of outer wall material is too low (reference comparative example 3), it is easy to cause incomplete embedding of the composite iron core material, and the masking effect of the iron smell is relatively poor. When normal pressure homogenization is used (reference comparative example 4), it will also significantly affect the embedding effect of the iron smell. When the amount of outer wall material is too much (reference comparative example 6) and the homogenization pressure is too large (reference comparative example 7), it will significantly affect the product yield. The main reason is that the outer wall material is mainly pectin. Although the embedding effect is relatively good when too much gum is added, it will increase the viscosity of the system. Due to the increased viscosity of the liquid, sticking to the wall will occur during the spraying process, resulting in a reduced yield. When the homogenization pressure is too high, the shear force is too large, causing the system to be over-crushed and producing more fine particles, which will be discharged with the hot air during the spraying process, thereby reducing the yield.

[0070] In Examples 1 to 3 using the technical solution of the present application, not only are the product yields relatively high, but the product particles and the stability in the liquid state (change in iron smell) are also relatively high.

[0071] Although preferred embodiments of the present invention have been described, those skilled in the art may make additional changes and modifications to these embodiments once they are aware of the basic inventive concepts. Therefore, the appended claims are intended to be interpreted as including the preferred embodiments and all changes and modifications that fall within the scope of the invention. Obviously, those skilled in the art may make various changes and modifications to the present invention without departing from the spirit and scope of the invention. Thus, the present invention is intended to include such changes and modifications as fall within the scope of the claims and their equivalents.

Claims

1. A compound product of ferrous glycinate and sodium ferric EDTA, characterized in that: Including core material and double wall material; The core material is ferrous glycinate and sodium ferric EDTA; The inner wall material is cyclodextrin and gum arabic; The outer wall material is pectin and hydroxypropyl methylcellulose; In the compound product, the mass percentage of the ferrous glycinate is 20% to 25%; the mass percentage of the sodium ferric EDTA is 8% to 10%; the mass percentage of the inner wall material is 60% to 70%; and the mass percentage of the outer wall material is 2% to 5%. The mass ratio of the cyclodextrin and the gum arabic in the inner wall material is (2-4):1; The mass ratio of the pectin and the hydroxypropyl methylcellulose in the outer wall material is (1.5-2.5):

1.

2. The composite product of ferrous glycinate and sodium iron EDTA according to claim 1, wherein The pectin is high-ester pectin with an esterification degree of ≥50%.

3. The composite product of ferrous glycinate and sodium iron EDTA according to claim 1, wherein The gum arabic is gum arabic with an AGP content of not less than 17%.

4. The method for preparing the composite product of ferrous glycinate and sodium ferric EDTA according to any one of claims 1 to 3, characterized in that: The following steps are involved: S1. Add cyclodextrin and gum arabic to water and allow to fully swell to obtain Solution I; S2. While stirring, slowly add the ferrous glycine and EDTA-sodium iron mixture to Solution I to obtain Solution II; S3. Using water as the solvent, first fully swell the pectin and hydroxypropyl methylcellulose, then add solution II and stir until completely dissolved and dispersed; S4. Then perform high pressure homogenization; S5. Finally, spray drying is performed to obtain a compound product.

5. The preparation method of the composite product of ferrous glycinate and sodium iron EDTA according to claim 4, wherein Step S3 uses hot water at 60°C to 80°C.

6. The preparation method of the composite product of ferrous glycinate and sodium iron EDTA according to claim 4, wherein The mass percentage of solid content of the solution II is 30% to 35%.

7. The preparation method of the composite product of ferrous glycinate and sodium iron EDTA according to claim 4, wherein The first-level homogenization pressure in step S4 is 8 MPa to 12 MPa, and the second-level pressure is 45 MPa to 55 MPa. Under this homogenization condition, homogenization is performed for 3 to 7 minutes.

8. The preparation method of the composite product of ferrous glycinate and sodium iron EDTA according to claim 4, wherein In step S5, the spray drying air inlet temperature is 165°C to 175°C, and the air outlet temperature is 90°C to 100°C.

9. The preparation method of the composite product of ferrous glycinate and sodium iron EDTA according to claim 4, wherein After the spray drying step S5, a screening step is also included, and the screening mesh number is 60 mesh to 100 mesh.

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