Stable spherical phosphatidylserine particles and preparation method thereof

Abstract

The invention discloses stable spherical phosphatidylserine particles and a preparation method thereof.The preparation method comprises the steps that phosphatidylserine generated through an enzymolysis reaction is filtered and then put into an organic solvent to be dissolved, meanwhile, an antioxidant is added, vacuum concentration is conducted till the concentration is 40%-60%, then the obtained concentrated solution passes through a porous membrane to form spherical liquid drops, and the spherical liquid drops are dried to obtain the stable spherical phosphatidylserine particles. Dispersing into an acetone solution in stirring, filtering and drying to obtain the phosphatidylserine spherical particles. According to the preparation technology, the risk that the PS is oxidized is reduced in the preparation process compared with conventional crushing, meanwhile, the prepared particles are uniform in particle size, good in fluidity, large in bulk specific gravity and not prone to oxidation and moisture absorption, and the applicability of the PS is greatly improved.

Description

Technical Field

[0001] The invention relates to the technical field of food and health products, and more particularly to a stable spherical phosphatidylserine particle and a preparation method thereof. Background Art

[0002] Phosphatidylserine (PS) is a naturally occurring nutritional phospholipid, also known as compound neuraminic acid. It is mainly present in the cell membrane and constitutes the basic structure of the cell membrane with other phospholipids, playing an important role in intercellular communication and the transmission of biochemical information to cells. Especially in the human nervous system, it is one of the important components of the brain cell membrane. Its function is mainly to improve the function of nerve cells, regulate the conduction of nerve impulses, and play an important regulatory role in various functions of the brain.

[0003] Phosphatidylserine (PS) can be synthesized by human or animal conditions, extracted from plants, or produced from soybean lecithin using biocatalytic technology. The head group of phospholipids can be easily modified by using the transphosphatidylation reaction of phospholipase D (PLDS). Therefore, phosphatidylserine can be produced from phosphatidylcholine or any other phospholipid mixture with serine by PLD catalysis.

[0004] At present, the method of preparing solid granule preparations in the production of PS is mainly to filter and dry the flake PS generated by the enzyme reaction, and then crush it with a pulverizer to granulate it. The high heat generated during the crushing process and repeated contact with air will easily increase the peroxide value. At the same time, the surface of the particles produced by this process is rough and needle-like, with a small bulk density and poor fluidity. Due to the large specific surface area, it is also more susceptible to moisture absorption and oxidation. Summary of the invention

[0005] In view of this, the present invention provides a method for preparing a spherical PS particle product with simple operation. Compared with conventional PS particle products, the PS particle product prepared by the method has a higher bulk density, better fluidity, is not easy to absorb moisture and oxidize, has a lower increase in peroxide value during the processing, and is suitable for large-scale production.

[0006] To achieve the above object, the present invention adopts the following technical solution:

[0007] First, the present invention provides a method for preparing stable spherical phosphatidylserine particles, comprising the following steps:

[0008] (1) filtering the phosphatidylserine generated by the enzymatic hydrolysis reaction, dissolving it in an organic solvent, adding an antioxidant, and concentrating it in vacuum until the mass concentration of the phosphatidylserine is 40%-60%;

[0009] (2) The concentrated solution obtained in step (1) is formed into spherical droplets through a porous membrane, dispersed into a stirring acetone solution, filtered and dried to obtain phosphatidylserine spherical particles.

[0010] Preferably, the organic solvent in step (1) is one of n-hexane, chloroform and cyclohexane.

[0011] Preferably, the antioxidant described in step (1) is a fat-soluble antioxidant.

[0012] Furthermore, the antioxidant is one or more of BHA, BHT, TBHQ, PG, and AP.

[0013] Preferably, the antioxidant is added in an amount of 0.02% of the mass of phosphatidylserine.

[0014] Preferably, the vacuum concentration temperature in step (1) is 30-35°C.

[0015] Preferably, the porous membrane in step (2) comprises one or more of a silica sand porous glass membrane, a ceramic membrane, a silica-alumina porous membrane, a zeolite-based porous membrane, and a metal oxide-based porous membrane.

[0016] Preferably, in step (2), the volume ratio of the concentrated solution to acetone is (0-15):100, and the temperature of the acetone solution is 10-15°C.

[0017] Preferably, in step (2), the stirring speed is 50-150 r / min and the time is 80-120 min.

[0018] Preferably, in step (2), the drying temperature is 40° C. and the drying time is 60-100 min.

[0019] In addition, the present invention also provides spherical phosphatidylserine particles prepared by the method described in the above technical solution, with a particle size of 30-200 meshes.

[0020] It can be seen from the above technical solutions that, compared with the prior art, the present invention discloses a stable spherical phosphatidylserine particle and a preparation method thereof, which has the following beneficial effects:

[0021] The invention presses a PS organic solvent concentrated liquid into an acetone solution in which PS is not dissolved through a porous membrane, and the PS concentrated liquid forms spherical particles under the action of stirring shear force. Meanwhile, the organic solvent diffuses into the acetone solution due to its mutual dissolution with acetone, and the PS concentrated liquid droplets form PS spherical solid particles as the organic solvent is reduced. The PS particles obtained by filtration are further vacuum dried to obtain a final PS spherical particle product. Compared with the pulverized PS, the processed product has a reduced chance of contact between PS and air during the processing, and reduces the increase of the peroxide value during the processing. The particle size distribution of the PS particles processed by the method is narrow, and the particle size of the finished product is highly controllable (by replacing membranes with different apertures and controlling the stirring shear speed). The PS particles processed by the method are dense spherical bodies, have good fluidity, high bulk density, and are not easy to absorb moisture and oxidize. DETAILED DESCRIPTION

[0022] The technical solution of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0023] Example 1

[0024] (1) Filter the PS generated by the enzymatic hydrolysis reaction and dissolve it in n-hexane, add 0.02% TBHQ, and concentrate it in vacuum at 30-35° C. to a 60% PS n-hexane solution;

[0025] (2) 100 ml of 60% PS n-hexane solution (temperature controlled at 30° C.) was pressed into 900 ml of acetone solution at 10° C. under stirring through a silica sand porous glass membrane with a pore size of 60 μm. The stirring speed was 60 r / min and the stirring was continued for 120 min. Then, the PS acetone suspension was filtered to obtain PS spherical particles, which were then dried in a vacuum oven at 40° C. for 100 min to obtain PS spherical particle products.

[0026] Example 2

[0027] (1) Filter the PS generated by the enzymatic hydrolysis reaction and dissolve it in n-hexane, add 0.02% AP, and concentrate it in vacuum at 32°C to a 50% PS n-hexane solution;

[0028] (2) 100 ml of 60% PS n-hexane solution (temperature controlled at 32°C) was pressed into 1200 ml of acetone solution at 10°C under stirring through a silica sand porous glass membrane with a pore size of 50 μm. The stirring speed was 100 r / min and the mixture was stirred for 100 min. Then, the PS acetone suspension was filtered to obtain PS spherical particles, which were then dried in a vacuum oven at 40°C for 80 min to obtain PS spherical particle products.

[0029] Example 3

[0030] (1) Filter the PS generated by the enzymatic hydrolysis reaction and dissolve it in n-hexane, add 0.02% TBHQ, and concentrate it in vacuum at 35°C to a 60% PS n-hexane solution (the temperature is controlled at 35°C);

[0031] (2) 100 ml of 60% PS n-hexane solution (temperature controlled at 35°C) was pressed into 900 ml of acetone solution at 10°C under stirring through a silica sand porous glass membrane with a pore size of 40 μm. The stirring speed was 140 r / min and the stirring was continued for 80 min. Then, the PS acetone suspension was filtered to obtain PS spherical particles, which were then dried in a vacuum oven at 40°C for 60 min to obtain PS spherical particle products.

[0032] Experimental example

[0033] The products prepared in the above examples 1-3 were tested, and the specific results are as follows:

[0034] 1. Comparison of repose angle (adding 0.5% micro powder silica gel)

[0035] Group Example 1 Example 2 Example 3 Crushed particles 46.1 47.5 48.3 Spherical particles 38.3 38.9 39.3

[0036] 2. Particle size distribution

[0037] Example 1

[0038]

[0039]

[0040] Example 2

[0041] factor 30-50 mesh 50-70 mesh 70-90 mesh 90-110 mesh 110-130 mesh Crushed particles 19.5％ 23.6％ 31.1％ 18.3％ 7.5％ Spherical particles 6.5％ 11.2％ 62.8％ 15.2％ 4.3％

[0042] Example 3

[0043] factor 30-50 mesh 50-70 mesh 70-90 mesh 90-110 mesh 110-130 mesh Crushed particles 9.5％ 13.6％ 21.1％ 38.3％ 17.5％ Spherical particles 3.5％ 7.2％ 16.8％ 58.2％ 14.3％

[0044] 3. Bulk density (adding 0.5% micro powder silica gel)

[0045] Group Example 1 Example 2 Example 3 Crushed particles 0.423g / ml 0.456g / ml 0.489g / ml Spherical particles 0.545g / ml 0.567g / ml 0.586g / ml

[0046] 4. Hygroscopicity (75% humidity, weight gain percentage at 25°C for 24 hours)

[0047] factor Example 1 Example 2 Example 3 Crushed particles 2.12％ 2.64％ 3.32％ Spherical particles 1.14％ 1.37％ 1.63％

[0048] 5. Antioxidant property (peroxide value increase after being placed at 25°C for 10 days)

[0049] factor Example 1 Example 2 Example 3 Crushed particles 4.23meq / kg 4.56meq / kg 4.71meq / kg Spherical particles 2.15meq / kg 2.31meq / kg 2.42meq / kg

[0050] In this specification, each embodiment is described in a progressive manner, and each embodiment focuses on the differences from other embodiments, and the same and similar parts between the embodiments can be referred to each other. The above description of the disclosed embodiments enables professionals and technicians in this field to implement or use the present invention. Various modifications to these embodiments will be obvious to professionals and technicians in this field, and the general principles defined herein can be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to these embodiments shown in this article, but will comply with the widest range consistent with the principles and novel features disclosed herein.

Claims

1. A method for preparing stable spherical phosphatidylserine particles, characterized in that: The following steps are involved: (1) filtering the phosphatidylserine generated by the enzymatic hydrolysis reaction, dissolving it in an organic solvent, adding an antioxidant, and concentrating it in vacuum until the mass concentration of the phosphatidylserine is 40%-60%; (2) The concentrated solution obtained in step (1) is formed into spherical droplets through a porous membrane, dispersed into a stirring acetone solution, filtered and dried to obtain phosphatidylserine spherical particles.

2. The method for preparing a stable spherical phosphatidylserine particle according to claim 1, characterized in that: The organic solvent described in step (1) is one of n-hexane, chloroform and cyclohexane.

3. The method for preparing a stable spherical phosphatidylserine particle according to claim 1, characterized in that: The antioxidant described in step (1) is a fat-soluble antioxidant.

4. The method for preparing a stable spherical phosphatidylserine particle according to claim 1 or 3, characterized in that: The antioxidant is one or more of BHA, BHT, TBHQ, PG and AP.

5. The method for preparing a stable spherical phosphatidylserine particle according to claim 1, characterized in that: The amount of the antioxidant added is 0.02% of the mass of phosphatidylserine.

6. The method for preparing a stable spherical phosphatidylserine particle according to claim 1, characterized in that: The vacuum concentration temperature in step (1) is 30-35°C.

7. The method for preparing a stable spherical phosphatidylserine particle according to claim 1, characterized in that: The porous membrane in step (2) includes one or more of silica sand porous glass membrane, ceramic membrane, silica-alumina porous membrane, zeolite-based porous membrane, and metal oxide-based porous membrane.

8. The method for preparing a stable spherical phosphatidylserine particle according to claim 1, characterized in that: In step (2), the volume ratio of the concentrated solution to acetone is (0-15):100, the temperature of the acetone solution is 10-15° C., the stirring speed is 50-150 r / min, and the stirring time is 80-120 min.

9. The method for preparing a stable spherical phosphatidylserine particle according to claim 1, characterized in that: In step (2), the drying temperature is 40° C. and the drying time is 60-100 min.

10. Spherical phosphatidylserine particles prepared by the method according to any one of claims 1 to 9.

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