5-hydroxytryptophan microcapsule powder and a method for preparing the same

Abstract

The present application relates to the technical field of microcapsule powder, and discloses 5-hydroxytryptophan microcapsule powder and a preparation method thereof.The microcapsule powder comprises 5-hydroxytryptophan and wall material, and the wall material comprises sodium octenyl succinate starch and maltodextrin.The preparation method mainly comprises the following steps: sodium octenyl succinate starch and maltodextrin are added into water, stirred uniformly and dissolved; 5-hydroxytryptophan is continuously added, sheared by a high-pressure homogenizer to form a coarse emulsion; the coarse emulsion is ground by a sander to obtain an emulsion; and the emulsion is subjected to a spray drying powder preparation process to obtain the microcapsule powder.The 5-hydroxytryptophan microcapsule powder prepared by the method has good water dispersibility, the water dispersion liquid is stable, the retention rate of 5-hydroxytryptophan is high, the microcapsule particle size is not greater than 0.5 microns, the bioavailability can be effectively improved, and the medicinal activity is improved.The preparation method is simple in operation, low in energy consumption, does not use organic solvents, and is suitable for industrial production.

Description

Technical Field

[0001] This invention relates to the field of microencapsulation powder technology, specifically to a 5-hydroxytryptophan microencapsulation powder and its preparation method. Background Technology

[0002] 5-Hydroxytryptophan is a natural amino acid with the compound name 5-Hydroxy-L-tryptophan and the chemical name 5-hydroxy-3-indolyl-A-aminopropionic acid. Its molecular formula is C6H5O7. 11 H 12 N₂O₃ is the precursor to serotonin. 5-Hydroxytryptophan is converted to serotonin by decarboxylase. Like dopamine and norepinephrine, serotonin is an important neurotransmitter and autoregulatory substance in the central nervous system, playing a vital role in nerve tissue. Currently, in addition to its traditional medicinal functions and antidepressant and sedative effects, serotonin is known to have functions such as weight loss, addiction treatment, sleep improvement, premenstrual syndrome (PMS) relief, and migraine treatment.

[0003] To facilitate storage and use, 5-hydroxytryptophan supplements are mostly sold in powder and capsule form. However, 5-hydroxytryptophan is almost insoluble in water, directly affecting its bioavailability and limiting its application in oral formulations. Therefore, new technologies are urgently needed to effectively improve the solubility and bioavailability of 5-hydroxytryptophan. Microencapsulation refers to the encapsulation of solid or liquid drugs in natural or synthetic polymer materials, forming microcapsules with diameters ranging from 1 to 1000 nm. Immobilized microcapsules are water-soluble and can improve the stability of the encapsulated drug. Microencapsulation technology can solve the application problems of 5-hydroxytryptophan in solid foods and health supplements.

[0004] The main source of 5-hydroxytryptophan is extracted and isolated from the seeds of the plant Ghana. As a major producer of plant extracts, my country's research focuses on the isolation and preparation processes of 5-hydroxytryptophan, with less research on its in-depth development and pharmaceutical applications. Currently, there are no reports on the microencapsulation of 5-hydroxytryptophan. Microencapsulation techniques for other active substances often use emulsifiers; however, each active substance has its own unique properties, and different microencapsulation materials will exhibit different expected effects. Applying existing microencapsulation techniques to 5-hydroxytryptophan may not effectively promote its bioavailability and may also present problems in terms of water solubility, dispersibility, and stability. Summary of the Invention

[0005] To address the aforementioned problems, the present invention aims to provide a 5-hydroxytryptophan microcapsule powder. This microcapsule powder exhibits good dispersibility, effectively improving the bioavailability of 5-hydroxytryptophan and thus increasing its activity. Another objective of the present invention is to provide a method for preparing 5-hydroxytryptophan microcapsule powder. The 5-hydroxytryptophan microcapsules obtained by this method have small particle size, high bioavailability, are easily dispersed in water, and the process is simple, which is beneficial for industrial production.

[0006] The objective of this invention is achieved through the following technical solution:

[0007] A 5-hydroxytryptophan microcapsule powder, wherein the microcapsule particle size is no greater than 0.6 μm, the water dispersion time of the microcapsule powder is no greater than 85 s, and the content of 5-hydroxytryptophan in the microcapsule powder is 10% to 20%.

[0008] A 5-hydroxytryptophan microcapsule powder includes a wall material and 5-hydroxytryptophan, wherein the wall material comprises sodium octenyl succinate starch and maltodextrin, the mass ratio of 5-hydroxytryptophan to wall material is 1:(4-9), and the mass ratio of sodium octenyl succinate starch to maltodextrin is 1:(1-4).

[0009] Furthermore, in the 5-hydroxytryptophan microcapsule powder, the mass ratio of 5-hydroxytryptophan to the wall material is 1:4, 1:6, 1:7 or 1:9, and the mass ratio of sodium octenyl succinate starch to maltodextrin is 1:1, 1:3 or 1:4.

[0010] A method for preparing 5-hydroxytryptophan microcapsule powder as described above, characterized by comprising the following steps:

[0011] (1) Add sodium octenyl succinate starch and maltodextrin to water, stir until dissolved;

[0012] (2) Continue to add 5-hydroxytryptophan and shear it with a high-pressure homogenizer to form a crude emulsion;

[0013] (3) The crude emulsion was obtained by grinding with a grinding mill.

[0014] (4) The emulsion is prepared by spray drying to obtain microcapsule powder.

[0015] In the further preparation method of 5-hydroxytryptophan microcapsule powder, in step (1), the weight ratio of sodium octenyl succinate starch to maltodextrin is 1:(1-4), and the mass-volume percentage of the wall material in the aqueous solution is 25%-35%.

[0016] In the further preparation method of 5-hydroxytryptophan microcapsule powder, in step (1), the weight ratio of sodium octenyl succinate starch to maltodextrin is 1:3, and the mass-volume percentage of the wall material in the aqueous solution is 30%.

[0017] In the further preparation method of 5-hydroxytryptophan microcapsule powder, in step (2), the mass-volume percentage of 5-hydroxytryptophan in the aqueous solution is 2% to 7%, and the high-pressure homogenizer is used to shear at a speed of 10,000 to 12,000 rpm for 10 to 15 minutes.

[0018] In the further preparation method of 5-hydroxytryptophan microcapsule powder, in step (2), the mass-volume percentage of 5-hydroxytryptophan in the aqueous solution is 5%, and the high-pressure homogenizer is sheared at a speed of 10,000 rpm.

[0019] In the further preparation method of 5-hydroxytryptophan microcapsule powder, in step (3), the grinding time of the sand mill is 60-120 min and the rotation speed is 1800-2600 rpm.

[0020] In the further preparation method of 5-hydroxytryptophan microcapsule powder, step (3) involves grinding in a sand mill for 90 minutes at a speed of 2200 rpm.

[0021] In the further preparation method of 5-hydroxytryptophan microcapsule powder, in step (4), the inlet air temperature during spray drying is 170-180℃ and the outlet air temperature is 80-95℃.

[0022] Currently, nanoencapsulation technology has been widely used in food, pharmaceuticals, cosmetics, pesticides, and other fields. However, there are currently no reports on methods for preparing 5-hydroxytryptophan microcapsule powder using nanoencapsulation technology. This invention uses a combination of sodium octenyl succinate starch and maltodextrin as the wall material, and employs a horizontal sand mill nano-grinding process. The resulting microcapsule powder is fully dispersed in water, effectively improving the solubility and bioavailability of 5-hydroxytryptophan. Attached Figure Description

[0023] Figure 1 The dispersion of 5-hydroxytryptophan microcapsule powder prepared by process 1 in water in Example 1;

[0024] Figure 2 The dispersion of 5-hydroxytryptophan in water. Detailed Implementation

[0025] Unless otherwise specified, the experimental methods used in the following examples are conventional methods.

[0026] Unless otherwise specified, the materials and reagents used in the following examples are all commercially available products that can be purchased on the market.

[0027] The present invention will be further described below through embodiments, but these descriptions are not intended to further limit the scope of the invention. Those skilled in the art should understand that equivalent substitutions or corresponding improvements made to the present invention still fall within the protection scope of the present invention.

[0028] The materials and instruments involved in the specific implementation method are as follows:

[0029] NT-V0.6L grinding mill, Dongguan Langling Machinery Co., Ltd.; ATS high-pressure homogenizer AH-BASIC, Antos Nanotechnology (Suzhou) Co., Ltd.; Bettersize 2600 laser particle size analyzer, Dandong Better Instruments Co., Ltd.; Sodium octenyl succinate (SSOS) Hi-cap 100, Ingredion Incorporated; Maltodextrin DE20, Anhui Shanhe Pharmaceutical Excipients Co., Ltd.; 5-Hydroxytryptophan 98% purity, Hubei Dixing Chemical Manufacturing Co., Ltd.

[0030] Example 15: Preparation and Process Optimization of 5-Hydroxytryptophan Microcapsule Powder

[0031] Sodium octenyl succinate starch and maltodextrin were added to purified water as wall materials, stirred until dissolved, and then 5-hydroxytryptophan was added. The mixture was then sheared using a high-pressure homogenizer to form a crude emulsion. The crude emulsion was then nano-ground using a horizontal mill (bead size 0.3-0.4 mm). The resulting material was spray-dried at an inlet air temperature of 180℃, an atomization pressure of 0.15 MPa, and an outlet air temperature of 85-90℃ to obtain microcapsule powder.

[0032] The following table shows the following parameters for the preparation processes of 5-hydroxytryptophan microcapsules (processes 1 to 7 and comparative processes 1 to 5): the dosage of 5-hydroxytryptophan, sodium octenyl succinate starch, and maltodextrin (percentages are by mass and volume); the shearing rate and time of the high-pressure homogenizer; and the grinding speed and time of the grinder.

[0033] Table 1. Preparation process of 5-hydroxytryptophan microcapsule powder

[0034]

[0035]

[0036] Example 25: Detection of 5-hydroxytryptophan microcapsule powder

[0037] 1. Test item: Dispersibility of 5-hydroxytryptophan microcapsule powder

[0038] Add 1g of sample to 100mL of water and stir magnetically at 300rpm. Observe the dispersion of the powder in the water. Complete dispersion means that no particles are visible in the water. Record the time it takes for the powder to be completely dispersed in the water.

[0039] 2. Test items: 5-hydroxytryptophan content and retention rate

[0040] Content detection method: The content of 5-hydroxytryptophan in the aqueous dispersion of the final product microcapsule powder was detected by high performance liquid chromatography. The chromatographic column was Sphersorb C18 (250×4.6mm), the detection wavelength was 278nm, the mobile phase was acetonitrile:water (1% triethanolamine, pH3.0) (0.05:0.95, v / v), isocratic elution was performed, and the flow rate was 1mL / min.

[0041] Content retention rate: The percentage of actual detected content to theoretical content.

[0042] 3. Test item: Microcapsule particle size in the aqueous dispersion of 5-hydroxytryptophan microcapsule powder

[0043] Take the aqueous dispersion of 5-hydroxytryptophan microcapsule powder from test item 1 and use a laser particle size analyzer to detect the particle size distribution of 5-hydroxytryptophan microcapsules.

[0044] 4. Test item: Stability of 5-hydroxytryptophan microcapsule powder aqueous dispersion

[0045] Take 50 ml of the aqueous dispersion of 5-hydroxytryptophan microcapsule powder from test item 1, add it to a 50 ml stoppered graduated cylinder, let it stand at room temperature for 24 h, and observe whether there is any sediment at the bottom of the stoppered graduated cylinder and whether the aqueous dispersion is separated into layers.

[0046] The 5-hydroxytryptophan microcapsule powder prepared in Example 1 was tested according to the above detection method. The test results are shown in Table 2.

[0047] Table 2. Detection results of 5-hydroxytryptophan microcapsule powder

[0048]

[0049]

[0050] The microcapsule powder of the present invention disperses rapidly in water (52-83s, completely dispersed in water), retains 91.2-98.7% of 5-hydroxytryptophan content during the preparation process, has a particle size D90 of 0.332-0.589μm in the aqueous dispersion, and remains stable after 24h without precipitation or stratification.

[0051] The microcapsule powder of the present invention contains 10-20% 5-hydroxytryptophan. Increasing the amount of maltodextrin in the wall material is beneficial to improving the water dispersibility of the microcapsule powder to a certain extent. However, if the amount added is too much, the emulsification effect is poor and the stability of the microcapsule powder water dispersion is affected.

[0052] During the preparation process, the 5-hydroxytryptophan microcapsule powder prepared using a grinder showed significantly improved water dispersibility, particle size, and stability of the aqueous dispersion compared to that prepared using a high-pressure homogenizer. Furthermore, the grinding speed and time of the grinder significantly affected the content and performance of the 5-hydroxytryptophan microcapsule powder. High grinding speeds caused a rapid rise in the temperature of the grinding chamber, potentially leading to 5-hydroxytryptophan degradation; conversely, low grinding speeds resulted in larger particle sizes and poorer water dispersibility in the aqueous dispersion of 5-hydroxytryptophan microcapsules, which may reduce the bioavailability of 5-hydroxytryptophan in the body.

Claims

1. A 5-hydroxytryptophan microcapsule powder, characterized in that, The microcapsule particle size is no greater than 0.6 μm.

2. The microencapsulated powder as described in claim 1, characterized in that, The water dispersion time of the microcapsule powder is no more than 85 seconds.

3. The microencapsulated powder as described in claim 1, characterized in that, The microcapsule powder contains 10% to 20% 5-hydroxytryptophan.

4. The microencapsulated powder according to any one of claims 1 to 3, characterized in that, The microcapsule powder includes a wall material and 5-hydroxytryptophan, wherein the wall material comprises sodium octenyl succinate starch and maltodextrin.

5. The microencapsulated powder as described in claim 4, characterized in that, The mass ratio of 5-hydroxytryptophan to the wall material is 1:(4-9), and the mass ratio of sodium octenyl succinate starch to maltodextrin is 1:(1-4).

6. The microencapsulated powder as described in claim 5, characterized in that, The mass ratio of 5-hydroxytryptophan to the wall material is 1:4, 1:6, 1:7 or 1:9, and the mass ratio of sodium octenyl succinate starch to maltodextrin is 1:1, 1:3 or 1:

4.

7. A method for preparing 5-hydroxytryptophan microcapsule powder as described in any one of claims 1 to 6, characterized in that, Includes the following steps: (1) Add sodium octenyl succinate starch and maltodextrin to water, stir until dissolved; (2) Continue to add 5-hydroxytryptophan and shear it with a high-pressure homogenizer to form a crude emulsion; (3) The crude emulsion was obtained by grinding with a grinding mill. (4) The emulsion is prepared by spray drying to obtain microcapsule powder.

8. The preparation method according to claim 7, characterized in that, In step (1), the weight ratio of sodium octenyl succinate starch to maltodextrin is 1:(1-4), and the mass-volume percentage of the wall material in the aqueous solution is 25%-35%.

9. The preparation method according to claim 8, characterized in that, In step (1), the weight ratio of sodium octenyl succinate starch to maltodextrin is 1:3, and the mass-volume percentage of the wall material in the aqueous solution is 30%.

10. The preparation method according to claim 7, characterized in that, In step (2), the mass-volume percentage of 5-hydroxytryptophan in the aqueous solution is 2% to 7%, and the high-pressure homogenizer is used to shear the sample at a speed of 10,000 to 12,000 rpm for 10 to 15 minutes.

11. The preparation method according to claim 10, characterized in that, In step (2), the mass-volume percentage of 5-hydroxytryptophan in the aqueous solution is 5%, and the high-pressure homogenizer is used to shear at a speed of 10,000 rpm.

12. The preparation method according to claim 7, characterized in that, In step (3), the grinding time of the sand mill is 60-120 min and the rotation speed is 1800-2600 rpm.

13. The preparation method according to claim 12, characterized in that, In step (3), the grinding time of the sand mill is 90 minutes and the rotation speed is 2200 rpm.

14. The preparation method according to claim 7, characterized in that, In step (4), the inlet air temperature during spray drying is 170-180℃ and the outlet air temperature is 80-95℃.

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