Preparation method of chelating type antioxidant iron supplementing agent

Abstract

The invention discloses a preparation method of a chelating antioxidant iron supplement agent, and belongs to the technical field of iron supplement agents. The preparation method comprises the following steps: a, separating pulp and seeds of lemon fruits; extracting the lemon pulp by adopting an extraction process to obtain a lemon pulp extract containing citric acid; extracting lemon seeds by adopting an extraction process to obtain lemon seed oil; and b, dissolving the lemon pulp extract in water, under the protection of nitrogen, adding ferrite, adjusting the pH value to 4.5-5, then carrying out a heating reaction, then adjusting the pH value to 5-5.5, then continuing the heating reaction, after the reaction is finished, adding lemon seed oil, and carrying out emulsification, pasteurization and spray drying to obtain the chelating antioxidant iron supplementing agent. The chelation stability, the oxidation resistance and the bioavailability of the iron supplementing agent are remarkably improved.

Description

Technical Field

[0001] The present invention relates to the technical field of iron supplements, and more specifically, to a preparation method of a chelated antioxidant iron supplement. Background Art

[0002] Iron deficiency anemia refers to a microcytic, hypochromic anemia caused by insufficient iron stores in the body, which affects hemoglobin synthesis. It is the most common type of anemia worldwide and one of the important global nutritional deficiency diseases. The prevention and treatment of iron deficiency anemia are mainly achieved by taking iron supplements. Currently, most iron supplements on the market are simple inorganic salts and organic salts, such as ferrous sulfate, ferrous lactate, ferrous gluconate, etc. These products have disadvantages such as poor stability, irritation to the gastrointestinal tract, and low iron absorption and utilization rate. Summary of the Invention

[0003] The purpose of the present invention is to overcome the above-mentioned deficiencies of the prior art and provide a preparation method of a chelated antioxidant iron supplement, which significantly improves the chelation stability, antioxidant property and bioavailability of the iron supplement.

[0004] To achieve the above purpose, the present invention adopts the following technical solutions:

[0005] A preparation method of a chelated antioxidant iron supplement, comprising the following steps:

[0006] a. Separate the pulp and seeds of lemon fruits; use an extraction process to extract the lemon pulp to obtain a lemon pulp extract containing citric acid; use an extraction process to extract the lemon seeds to obtain lemon seed oil;

[0007] b. Dissolve the lemon pulp extract in water, add ferrous salt under nitrogen protection, adjust the pH value to 4.5 - 5 and then heat and react, then adjust the pH value to 5 - 5.5 and continue to heat and react. After the reaction is completed, add lemon seed oil for emulsification, pasteurize, and spray dry to obtain the chelated antioxidant iron supplement.

[0008] The present invention is further configured such that in step a, the specific preparation steps of the lemon pulp extract are: crush the lemon pulp and add it to a solvent for extraction, then centrifuge and filter, and rotary evaporate the filtrate to remove the solvent to obtain the lemon pulp extract.

[0009] In the preparation of the lemon pulp extract, the material-liquid ratio of the lemon pulp powder to the solvent is 1:10, the solvent is ethanol, the extraction temperature is 50 - 55 °C, and the extraction time is 3 - 4 h.

[0010] The present invention is further configured such that in step a, the specific preparation steps of lemon seed oil are as follows: Wash and dry lemon seeds, then crush them. Add the obtained lemon seed powder to a solvent for ultrasonic extraction, and then perform liquid-solid separation. Rotate evaporate the filtrate to remove the solvent to obtain lemon seed oil.

[0011] The present invention is further configured such that in the preparation of lemon seed oil, the liquid-solid ratio of lemon seed powder to the solvent is 1:10, the solvent is n-hexane, the ultrasonic extraction temperature is 45 - 50 °C, the ultrasonic power is 200 W, and the extraction time is 25 - 35 min.

[0012] The present invention is further configured such that in step b, the mass ratio of ferrous salt to citric acid and lemon seed oil in the lemon pulp extract is 18 - 40:1 - 8:1 - 5.

[0013] The present invention is further configured such that in step b, the ferrous salt is ferrous sulfate.

[0014] The present invention is further configured such that in step b, adjust the pH value to 4.5 - 5 and react at 50 - 60 °C for 45 - 60 min, then adjust the pH value to 5 - 5.5 and react at 60 - 70 °C for 20 - 30 min.

[0015] The present invention is further configured such that in step b, the pH value is adjusted using a citric acid - sodium citrate buffer system.

[0016] The present invention is further configured such that in step b, the emulsification temperature is 60 - 65 °C and the emulsification time is 30 - 40 min.

[0017] In summary, the present invention has the following beneficial effects:

[0018] Using the lemon pulp extract containing citric acid as a chelating agent and lemon seed oil as an emulsifier to prepare an iron supplement, realizing ferrous chelation by substances such as citric acid, polysaccharides, and amino acids in lemon, realizing antioxidant effects through flavonoids and polyphenolic substances in lemon, and adopting a step-by-step pH adjustment and chelation method to ensure the full chelation of ferrous salt and citric acid, avoiding the interference of trace elements in lemon on chelation, and significantly improving the chelation stability, antioxidant property, and bioavailability of the iron supplement. Specific Embodiments

[0019] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0020] The preparation method of the chelating antioxidant iron supplement of the present invention includes the following steps:

[0021] a. Separate the pulp and seeds of lemon fruits; extract the lemon pulp using an extraction process (i.e., crush the lemon pulp and add it to ethanol for extraction for 3 - 4 h, the material - liquid ratio of lemon pulp powder to solvent is 1:10, and the extraction temperature is 50 - 55°C; then centrifuge and filter, and rotary - evaporate the filtrate to remove the solvent) to obtain a lemon pulp extract containing citric acid; extract the lemon seeds using an extraction process (i.e., wash, dry, and crush the lemon seeds, add the obtained lemon seed powder to n - hexane for ultrasonic extraction for 25 - 35 min, the material - liquid ratio of lemon seed powder to solvent is 1:10, the ultrasonic extraction temperature is 45 - 50°C, and the ultrasonic power is 200 W; then separate the solid and liquid, and rotary - evaporate the filtrate to remove the solvent) to obtain lemon seed oil;

[0022] b. Dissolve the lemon pulp extract in water, under nitrogen protection, add a ferrous salt (preferably ferrous sulfate), adjust the pH value to 4.5 - 5 using a citric acid - sodium citrate buffer system and react at 50 - 60°C for 45 - 60 min, then adjust the pH value to 5 - 5.5 using a citric acid - sodium citrate buffer system and react at 60 - 70°C for 20 - 30 min. After the reaction, add lemon seed oil and emulsify at 60 - 65°C for 30 - 40 min, then perform pasteurization and spray - drying to obtain a chelated antioxidant iron - supplementing agent; the mass ratio of water, ferrous salt, citric acid in the lemon pulp extract, and lemon seed oil is 800:(18 - 40):(1 - 8):(1 - 5).

[0023] Example 1

[0024] a. Separate the pulp and seeds of lemon fruits; extract the lemon pulp using an extraction process (i.e., crush the lemon pulp and add it to ethanol for extraction for 4 h, the material - liquid ratio of lemon pulp powder to solvent is 1:10, and the extraction temperature is 50 - 55°C; then centrifuge and filter, and rotary - evaporate the filtrate to remove the solvent) to obtain a lemon pulp extract containing citric acid; extract the lemon seeds using an extraction process (i.e., wash, dry, and crush the lemon seeds, add the obtained lemon seed powder to n - hexane for ultrasonic extraction for 30 min, the material - liquid ratio of lemon seed powder to solvent is 1:10, the ultrasonic extraction temperature is 45 - 50°C, and the ultrasonic power is 200 W; then separate the solid and liquid, and rotary - evaporate the filtrate to remove the solvent) to obtain lemon seed oil;

[0025] b. Dissolve the lemon pulp extract in water. Under nitrogen protection, add ferrous sulfate, and use the citric acid - sodium citrate buffer system to adjust the pH value to 4.5, then react at 50 - 60 °C for 50 min. After that, use the citric acid - sodium citrate buffer system to adjust the pH value to 5.5, and then react at 60 - 70 °C for 20 min. After the reaction is completed, add lemon seed oil and emulsify at 60 °C for 40 min, then perform pasteurization and spray drying to obtain the chelated antioxidant iron supplement. The mass ratio of water, ferrous sulfate, citric acid in the lemon pulp extract, and lemon seed oil is 800:20:4.1:2.

[0026] Comparative Example 1

[0027] Prepare the iron supplement according to Example 1, but step b is: Dissolve the lemon pulp extract in water. Under nitrogen protection, add ferrous sulfate, and use the citric acid - sodium citrate buffer system to adjust the pH value to 5.5, then react at 60 - 70 °C for 70 min. After the reaction is completed, add lemon seed oil and emulsify at 60 °C for 40 min, then perform pasteurization and spray drying to obtain the chelated antioxidant iron supplement. The mass ratio of water, ferrous sulfate, citric acid in the lemon pulp extract, and lemon seed oil is 800:20:4.1:2.

[0028] Comparative Example 2

[0029] Under nitrogen protection, add citric acid to water, control the citric acid concentration in the solution to be [concentration value], under nitrogen protection, add ferrous sulfate, and use the citric acid - sodium citrate buffer system to adjust the pH value to 4.5, then react at 50 - 60 °C for 50 min. After that, use the citric acid - sodium citrate buffer system to adjust the pH value to 5.5, and then react at 60 - 70 °C for 20 min. After the reaction is completed, add lecithin and emulsify at 60 °C for 40 min, then perform pasteurization and spray drying to obtain the chelated antioxidant iron supplement. The mass ratio of water, ferrous sulfate, citric acid, and lecithin is 800:20:4.1:2.

[0030] Comparative Example 3

[0031] Prepare the lemon pulp extract according to step a of Example 1. Dissolve the lemon pulp extract in water. Under nitrogen protection, add ferrous sulfate, and use the citric acid - sodium citrate buffer system to adjust the pH value to 4.5, then react at 50 - 60 °C for 50 min. After that, use the citric acid - sodium citrate buffer system to adjust the pH value to 5.5, and then react at 60 - 70 °C for 20 min. After the reaction is completed, add lecithin and emulsify at 60 °C for 40 min, then perform pasteurization and spray drying to obtain the chelated antioxidant iron supplement. The mass ratio of water, ferrous sulfate, citric acid in the lemon pulp extract, and lecithin is 800:20:4.1:2.

[0032] Comparative Example 4

[0033] Under nitrogen protection, citric acid was added to water, and the concentration of citric acid in the solution was controlled. Under nitrogen protection, ferrous sulfate was added, and the pH value was adjusted to 4.5 using a citric acid-sodium citrate buffer system. Then, the reaction was carried out at 50 - 60 °C for 50 min. After that, the pH value was adjusted to 5.5 using a citric acid-sodium citrate buffer system, and the reaction was carried out at 60 - 70 °C for 20 min. After the reaction was completed, lemon seed oil was added and emulsified at 60 °C for 40 min, followed by pasteurization and spray drying to obtain a chelated antioxidant iron supplement; the mass ratio of water, ferrous sulfate, citric acid, and lemon seed oil was 800:20:4.1:2.

[0034] The blood-enriching effects of the iron supplements in Test Example 1 and Comparative Examples 1 - 4 were tested (according to the verification method in the preparation method of a protein iron iron supplement, CN105998059A). The results showed that the Hb of the rats taking the iron supplement in Example 1 reached 146.7 g / L on the 18th day of iron supplementation (the Hb of the rats was 81.6 g / L at 0 day of iron supplementation, and the Hb of the rats in the normal control group was 145.89 on the 18th day); the Hb of the rats taking the iron supplement in Comparative Example 1 was 136.7 g / L on the 18th day of iron supplementation (the Hb of the rats was 81.1 g / L at 0 day of iron supplementation) and 144.6 g / L on the 20th day of iron supplementation; the Hb of the rats taking the iron supplement in Comparative Example 2 was 117.5 g / L on the 18th day of iron supplementation (the Hb of the rats was 80.8 g / L at 0 day of iron supplementation) and 129.3 g / L on the 20th day of iron supplementation; the Hb of the rats taking the iron supplement in Comparative Example 3 was 127.2 g / L on the 18th day of iron supplementation (the Hb of the rats was 82.4 g / L at 0 day of iron supplementation) and 139.4 g / L on the 20th day of iron supplementation; the Hb of the rats taking the iron supplement in Comparative Example 3 was 123.9 g / L on the 18th day of iron supplementation (the Hb of the rats was 82.0 g / L at 0 day of iron supplementation) and 135.2 g / L on the 20th day of iron supplementation.

[0035] The antioxidant activities of the iron supplements in Test Example 1 and Comparative Examples 1 - 4 were tested. The results showed that the DPPH radical scavenging rates of the iron supplements in Example 1 and Comparative Examples 1 - 4 were 95.2%, 90.6%, 64.1%, 78.4%, and 83.7% in sequence.

[0036] From the above results, it can be seen that chelation under segmented pH conditions, chelation with lemon pulp extract, and emulsification with lemon seed oil to prepare iron supplements can improve the bioavailability and antioxidant activity performance of iron supplements.

[0037] In addition, the stabilities of the chelation products obtained in the preparation of Test Example 1 and Comparative Examples 1 - 4 were tested, that is, the reaction solutions of the examples and each comparative example after emulsification but before sterilization and spray drying were stored at 40 °C and 75% humidity for 90 days, and it was found that only the reaction solution of Example 1 did not show precipitation.

[0038] The above are only the preferred embodiments of the present invention. The protection scope of the present invention is not limited to the above embodiments. Any technical solutions falling within the concept of the present invention belong to the protection scope of the present invention. It should be noted that for those of ordinary skill in the art, without departing from the principle of the present invention, several improvements and refinements should also be regarded as within the protection scope of the present invention.

Claims

1. A preparation method of a chelated antioxidant iron supplement, characterized in that, It includes the following steps: a. Separate the pulp and seeds of lemon fruits; use an extraction process to extract the lemon pulp to obtain a lemon pulp extract containing citric acid; use an extraction process to extract the lemon seeds to obtain lemon seed oil; b. Dissolve the lemon pulp extract in water, add ferrous salt under nitrogen protection, adjust the pH value to 4.5 - 5 and then heat for reaction, then adjust the pH value to 5 - 5.5 and continue heating for reaction. After the reaction ends, add lemon seed oil for emulsification, pasteurize, and spray dry to obtain a chelated antioxidant iron supplement.

2. The preparation method of a chelated antioxidant iron supplement according to claim 1, wherein In step a, the specific preparation steps of the lemon pulp extract are: crush the lemon pulp and add it to a solvent for extraction, then centrifuge and filter, and rotary evaporate the filtrate to remove the solvent to obtain the lemon pulp extract.

3. The preparation method of a chelated antioxidant iron supplement according to claim 2, characterized in that, In the preparation of the lemon pulp extract, the ratio of the lemon pulp powder to the solvent is 1:10, the solvent is ethanol, the extraction temperature is 50 - 55 °C, and the extraction time is 3 - 4 h.

4. The preparation method of a chelated antioxidant iron supplement according to claim 1, characterized in that, In step a, the specific preparation steps of the lemon seed oil are: wash and dry the lemon seeds and then crush them, add the obtained lemon seed powder to a solvent for ultrasonic extraction, then separate the solid and liquid, and rotary evaporate the filtrate to remove the solvent to obtain the lemon seed oil.

5. The preparation method of a chelated antioxidant iron supplement according to claim 4, characterized in that, In the preparation of the lemon seed oil, the ratio of the lemon seed powder to the solvent is 1:10, the solvent is n - hexane, the ultrasonic extraction temperature is 45 - 50 °C, the ultrasonic power is 200 W, and the extraction time is 25 - 35 min.

6. The preparation method of a chelated antioxidant iron supplement according to claim 1, characterized in that, In step b, the mass ratio of the ferrous salt to citric acid and lemon seed oil in the lemon pulp extract is 18 - 40:1 - 8:1 - 5.

7. The preparation method of a chelated antioxidant iron supplement according to claim 1, wherein In step b, the ferrous salt is ferrous sulfate.

8. The preparation method of a chelated antioxidant iron supplement according to claim 1, characterized in that, In step b, adjust the pH value to 4.5 - 5 and react at 50 - 60 °C for 45 - 60 min, adjust the pH value to 5 - 5.5 and react at 60 - 70 °C for 20 - 30 min.

9. The preparation method of a chelated antioxidant iron supplement according to claim 1, wherein In step b, use a citric acid - sodium citrate buffer system to adjust the pH value.

10. The preparation method of a chelated antioxidant iron supplement according to claim 1, characterized in that, In step b, the emulsification temperature is 60 - 65 °C, and the emulsification time is 30 - 40 min.