Preparation method of lycopene phospholipid complex

Abstract

The invention discloses a preparation method of a lycopene phospholipid complex, which comprises the following steps: S1, dissolving phospholipid in an ester agent to obtain a phospholipid solution; s2, dissolving povidone K30 in an alcohol agent to obtain a povidone solution; s3, adding lycopene and the povidone solution into the phospholipid solution, and performing reflux mixing to obtain a composite solution; and S4, removing the solvent from the composite solution to obtain the lycopene phospholipid complex. The lycopene phospholipid composite composition which is thick and can be easily scraped off from a vessel is obtained.

Description

Technical Field

[0001] The present invention relates to the fields of health care products and functional foods, and particularly to a preparation method of a lycopene phospholipid complex. Background Art

[0002] Lycopene is a fat-soluble natural carotenoid, mainly present in the ripe fruits of Solanaceae plants such as tomatoes, and is also a strong antioxidant in natural plants. Lycopene contains a highly unsaturated structure and has biological activities such as quenching singlet oxygen, scavenging free radicals, anti-inflammatory, preventing atherosclerosis, enhancing immunity, improving cardiovascular diseases, and anti-tumor. Lycopene and its products are widely used in the food industry as nutritional fortifiers, health foods, etc. However, lycopene has poor water solubility. Although its phospholipid complex can be prepared to improve its water solubility, the lycopene phospholipid complex is viscous and difficult to scrape off and solidify, resulting in low overall utilization rate and affecting the preparation of downstream preparations. If the solvent is not completely removed, it will affect the quality and safety of downstream preparations and result in low overall solid content. Therefore, the field has been struggling to find a method to solve the problem that the complex is viscous and difficult to scrape off from the vessel after the solvent is completely removed, and is eager to obtain a lycopene phospholipid complex that is easy to scrape off from the vessel after the solvent is completely removed. Summary of the Invention

[0003] The purpose of the present invention is to provide a lycopene complex to improve the technique that the lycopene phospholipid complex is viscous and difficult to scrape off from the vessel. Another purpose of the present invention is to provide a lycopene phospholipid composite composition that is relatively viscous and easier to scrape off from the vessel.

[0004] To solve the above technical problems, the present invention adopts the following technical solutions:

[0005] A preparation method of a lycopene phospholipid complex, comprising the following steps:

[0006] S1. Dissolve phospholipids in an ester agent to obtain a phospholipid solution;

[0007] S2. Dissolve polyvinylpyrrolidone K30 in an alcohol agent to obtain a polyvinylpyrrolidone solution;

[0008] S3. Add lycopene and the polyvinylpyrrolidone solution to the phospholipid solution, and reflux and mix to obtain a composite solution;

[0009] S4. Remove the solvent from the composite solution to obtain a lycopene phospholipid complex.

[0010] Preferably, the mass ratio of the lycopene, the phospholipids, and the polyvinylpyrrolidone K30 is 1:2:2 - 10.

[0011] Preferably, the volume ratio of the ester agent to the alcohol agent is 6:1.

[0012] Preferably, the phospholipid includes egg yolk lecithin; the ester agent includes ethyl acetate; the alcohol agent includes ethanol and methanol.

[0013] Preferably, the alcohol agent includes 95% ethanol by volume.

[0014] Povidone k30 can be completely dissolved in 95% ethanol, while egg yolk lecithin is easily soluble in ethyl acetate. When these two solvents are selected, povidone solution and phospholipid solution can be obtained better, which helps subsequent synergistic compounding.

[0015] Preferably, in step S1, the mass-to-volume ratio of the phospholipid to the ester agent is 1 g:30 ml; in step S2, the mass-to-volume ratio of povidone K30 to the alcohol agent is 2 - 10 g:10 - 30 ml.

[0016] Preferably, in step S1, the way of dissolving the phospholipid in the ester agent includes reflux stirring; in step S3, the way of reflux mixing includes reflux stirring; in step S4, the way of removing the solvent includes one or more of suction filtration, evaporation to dryness, rotary evaporation, and vacuum drying.

[0017] Preferably, in step S1, the temperature of the reflux stirring is 50°C; in step S3, the temperature of the reflux mixing is 50°C, and the time is 2 - 4 h.

[0018] A lycopene phospholipid complex obtained by the preparation method of the above lycopene phospholipid complex.

[0019] An application of the above lycopene phospholipid complex, which is used in one or more of foods and health products.

[0020] Compared with the prior art, implementing the present invention has the following beneficial effects:

[0021] The present invention obtains a lycopene phospholipid composite composition that is relatively viscous and easy to scrape off from the vessel. Through the synergistic effect of povidone k30 and phospholipid, it solves the problem that has been plaguing the field, that is, after the solvent is completely removed, the complex is viscous and difficult to scrape off from the vessel. It meets the pain point of eager to obtain a lycopene phospholipid complex that is easy to scrape off from the vessel after the solvent is removed, obtains a lycopene phospholipid composite composition that is relatively viscous and easy to scrape off from the vessel, and at the same time realizes high utilization rate and high solid content, which helps the preparation of downstream preparations. Specific Embodiments

[0022] To make the objectives, technical solutions and advantages of the present invention clearer, the present invention will be further described in detail below in conjunction with specific embodiments.

[0023] Example 1

[0024] (1) Add 60 ml of ethyl acetate to 2.0 g of egg yolk lecithin, and reflux and stir at 50 °C until the egg yolk lecithin is completely dissolved to obtain an egg yolk lecithin ethyl acetate solution.

[0025] (2) Add 10 ml of 95% ethanol to 2.0 g of polyvinylpyrrolidone K30 until the polyvinylpyrrolidone K30 is completely dissolved to obtain a polyvinylpyrrolidone K30 ethanol solution.

[0026] (3) Add 1.0 g of lycopene and the polyvinylpyrrolidone K30 ethanol solution to the egg yolk lecithin ethyl acetate solution, and reflux and stir at 50 °C for 4 h to obtain a lycopene polyvinylpyrrolidone egg yolk lecithin ethyl acetate composite solution.

[0027] (4) Stop heating and stirring, filter the lycopene polyvinylpyrrolidone egg yolk lecithin ethyl acetate composite solution by suction, and rotary evaporate to remove its solvent to obtain a lycopene polyvinylpyrrolidone phospholipid complex. Place it in a vacuum drying oven at -0.1 MPa and 50 °C for drying for 5 h to obtain 1.80 g of a viscous complex. The complex is relatively viscous in the evaporating dish and is relatively easy to scrape off. The total weight of the product that can be scraped off is 1.56 g, and the scraping rate reaches over 86%.

[0028] Example 2

[0029] (1) Add 60 ml of ethyl acetate to 2.0 g of egg yolk lecithin, and reflux and stir at 50 °C until the egg yolk lecithin is completely dissolved to obtain an egg yolk lecithin ethyl acetate solution.

[0030] (2) Add 30 ml of 95% ethanol to 10.0 g of polyvinylpyrrolidone K30 until the polyvinylpyrrolidone K30 is completely dissolved to obtain a polyvinylpyrrolidone K30 ethanol solution.

[0031] (3) Add 1.0 g of lycopene and the polyvinylpyrrolidone K30 ethanol solution to the egg yolk lecithin ethyl acetate solution, and reflux and stir at 50 °C for 2 h to obtain a lycopene polyvinylpyrrolidone egg yolk lecithin ethyl acetate composite solution.

[0032] (4) Stop heating and stirring, filter the lycopene polyvinylpyrrolidone egg yolk lecithin ethyl acetate composite solution by suction and evaporate to dryness its solvent to obtain 7.20 g of a viscous lycopene polyvinylpyrrolidone phospholipid complex. The complex is relatively viscous in the evaporating dish and is relatively easy to scrape off. The total weight of the product that can be scraped off is 6.15 g, and the scraping rate reaches over 85%.

[0033] Example 3

[0034] (1) Add 60 ml of ethyl acetate to 2.0 g of egg yolk lecithin, and reflux and stir at 50 °C until the egg yolk lecithin is completely dissolved to obtain an egg yolk lecithin ethyl acetate solution.

[0035] (2) Add 10 ml of methanol to 2.0 g of polyvinylpyrrolidone K30 until the polyvinylpyrrolidone K30 is completely dissolved to obtain a polyvinylpyrrolidone K30 methanol solution.

[0036] (3) Add 1.0 g of lycopene and a polyvinylpyrrolidone K30 methanol solution to an egg yolk lecithin ethyl acetate solution, reflux and stir at 50 °C for 2 h to obtain a lycopene-polyvinylpyrrolidone-egg yolk lecithin ethyl acetate composite solution.

[0037] (4) Stop heating and stirring, filter the lycopene-polyvinylpyrrolidone-egg yolk lecithin ethyl acetate composite solution by suction filtration, and rotary evaporate to remove its solvent to obtain a lycopene-polyvinylpyrrolidone phospholipid complex. Place it in a vacuum drying oven at -0.1 MPa and 60 °C for drying for 4 h to obtain 2.72 g of a viscous complex. The complex is relatively viscous in the evaporating dish and is relatively easy to scrape off. The total weight of the product that can be scraped off is 2.4 g, and the scraping-off rate reaches over 88%.

[0038] Comparative Example 1

[0039] (1) Add 60 ml of ethyl acetate to 2.0 g of egg yolk lecithin, reflux and stir at 50 °C until the egg yolk lecithin is completely dissolved to obtain an egg yolk lecithin ethyl acetate solution.

[0040] (2) Add 1.0 g of lycopene to the egg yolk lecithin ethyl acetate solution, reflux and stir at 50 °C for 4 h to obtain a lycopene-egg yolk lecithin ethyl acetate composite solution.

[0041] (3) Stop heating and stirring, filter the lycopene-egg yolk lecithin ethyl acetate composite solution by suction filtration and evaporate to dryness its solvent to obtain a lycopene phospholipid complex. Place it in a vacuum drying oven at -0.1 MPa and 60 °C for drying for 4 h to obtain 2.06 g of a complex. The complex is viscous in the evaporating dish. When attempting to scrape it off, the complex adheres between the evaporating dish and the medicine spoon and forms a silk-like substance, making it impossible to scrape it off smoothly and impossible to weigh.

[0042] Comparative Example 2

[0043] (1) Add 30 ml of ethyl acetate to 2.0 g of egg yolk lecithin, reflux and stir at 50 °C until the egg yolk lecithin is completely dissolved to obtain an egg yolk lecithin ethyl acetate solution.

[0044] (2) Add 1.0 g of lycopene to the egg yolk lecithin ethyl acetate solution, reflux and stir at 50 °C for 2 h to obtain a lycopene-egg yolk lecithin ethyl acetate composite solution.

[0045] (3) Add 10 ml of ethyl acetate to 2.0 g of polyvinylpyrrolidone K30, and polyvinylpyrrolidone K30 does not dissolve to obtain a polyvinylpyrrolidone K30 ethyl acetate suspension.

[0046] (4) Add the polyvinylpyrrolidone K30 ethyl acetate suspension to the lycopene-egg yolk lecithin ethyl acetate composite solution, reflux and stir at 50 °C for 10 min to obtain a lycopene-polyvinylpyrrolidone-egg yolk lecithin ethyl acetate composite solution.

[0047] (5) Stop heating and stirring, filter the lycopene povidone egg yolk lecithin ethyl acetate composite solution by suction and evaporate its solvent to obtain the lycopene povidone phospholipid complex. The complex was viscous in the evaporating dish. When attempting to scrape it off, the complex adhered between the evaporating dish and the medicine spoon, forming a silk-like substance and could not be scraped off smoothly, making it impossible to weigh.

[0048] Comparative Example 3

[0049] (1) Add 60 ml of ethyl acetate to 2.0 g of egg yolk lecithin, reflux and stir at 50 °C until the egg yolk lecithin is completely dissolved to obtain the egg yolk lecithin ethyl acetate solution.

[0050] (2) Mix 1.0 g of lycopene and 2.0 g of povidone K30 evenly to obtain the lycopene povidone mixture.

[0051] (3) Add the lycopene povidone mixture to the egg yolk lecithin ethyl acetate solution, reflux and stir at 50 °C for 4 h to obtain the lycopene povidone egg yolk lecithin ethyl acetate composite solution.

[0052] (4) Stop heating and stirring, filter the lycopene povidone egg yolk lecithin ethyl acetate composite solution by suction and evaporate its solvent to obtain the lycopene povidone phospholipid complex. Place it in a vacuum drying oven at -0.1 MPa and 60 °C for drying for 4 h to obtain 1.80 g of the complex. The complex was viscous in the evaporating dish. When attempting to scrape it off, the complex adhered between the evaporating dish and the medicine spoon, forming a silk-like substance and could not be scraped off smoothly, making it impossible to weigh.

[0053] Comparative Example 4

[0054] (1) Add 60 ml of ethyl acetate to 2.0 g of egg yolk lecithin, reflux and stir at 50 °C until the egg yolk lecithin is completely dissolved to obtain the egg yolk lecithin ethyl acetate solution.

[0055] (2) Add 10 ml of absolute ethanol to 2.0 g of maltodextrin to obtain the maltodextrin ethanol suspension.

[0056] (3) While stirring the maltodextrin ethanol suspension, pour 1.0 g of lycopene into the egg yolk lecithin ethyl acetate solution, reflux and stir at 50 °C for 4 h to obtain the lycopene maltodextrin egg yolk lecithin ethyl acetate composite solution.

[0057] (4) Stop heating and stirring, filter the lycopene maltodextrin egg yolk lecithin ethyl acetate composite solution by suction and evaporate its solvent to obtain the lycopene maltodextrin phospholipid complex. The complex was viscous in the evaporating dish. When attempting to scrape it off, the complex adhered between the evaporating dish and the medicine spoon, forming a silk-like substance and could not be scraped off smoothly, making it impossible to weigh.

[0058] Comparative Example 5

[0059] (1) Add 60 ml of ethyl acetate to 2.0 g of egg yolk lecithin, and reflux and stir at 50 °C until the egg yolk lecithin is completely dissolved to obtain an egg yolk lecithin ethyl acetate solution.

[0060] (2) Add 10 ml of 95% ethanol to 2.0 g of tapioca starch to obtain a tapioca starch ethanol suspension.

[0061] (3) While stirring the tapioca starch ethanol suspension, add 1.0 g of lycopene to the egg yolk lecithin ethyl acetate solution, and reflux and stir at 50 °C for 2 h to obtain a lycopene tapioca starch egg yolk lecithin ethyl acetate composite solution.

[0062] (4) Stop heating and stirring, filter the lycopene tapioca starch egg yolk lecithin ethyl acetate composite solution by suction and evaporate its solvent to obtain a lycopene tapioca starch phospholipid complex. The complex is viscous in the evaporating dish. When attempting to scrape it off, the complex adheres between the evaporating dish and the spatula and forms a silk-like substance, making it impossible to scrape off smoothly and impossible to weigh.

[0063] Comparative Example 6

[0064] (1) Add 60 ml of ethyl acetate to 2.0 g of egg yolk lecithin, and reflux and stir at 50 °C until the egg yolk lecithin is completely dissolved to obtain an egg yolk lecithin ethyl acetate solution.

[0065] (2) Add 10 ml of 95% ethanol to 2.0 g of potato starch to obtain a potato starch ethanol suspension.

[0066] (3) While stirring the potato starch ethanol suspension, add 1.0 g of lycopene to the egg yolk lecithin ethyl acetate solution, and reflux and stir at 50 °C for 2 h to obtain a lycopene potato starch egg yolk lecithin ethyl acetate composite solution.

[0067] (4) Stop heating and stirring, filter the lycopene potato starch egg yolk lecithin ethyl acetate composite solution by suction and evaporate its solvent to obtain a lycopene potato starch phospholipid complex. The complex is viscous in the evaporating dish. When attempting to scrape it off, the complex adheres between the evaporating dish and the spatula and forms a silk-like substance, making it impossible to scrape off smoothly and impossible to weigh.

[0068] Comparative Example 7

[0069] (1) Add 60 ml of butyl acetate to 2.0 g of egg yolk lecithin, and reflux and stir at 50 °C until the egg yolk lecithin is completely dissolved to obtain an egg yolk lecithin butyl acetate solution.

[0070] (2) Add 10 ml of 95% ethanol to 2.0 g of polyvinylpyrrolidone K30 until the polyvinylpyrrolidone K30 is completely dissolved to obtain a polyvinylpyrrolidone K30 ethanol solution.

[0071] (3) Add 1.0 g of lycopene and polyvinylpyrrolidone K30 ethanol solution to the egg yolk lecithin butyl acetate solution, reflux and stir at 50 °C for 2 h. The lycopene agglomerates and floats on the surface of the solution without dispersing into the solution, and no lycopene phospholipid complex solution is obtained.

[0072] Comparative Example 8

[0073] (1) Add 60 ml of ethyl acetate to 2.0 g of egg yolk lecithin, reflux and stir at 50 °C until the egg yolk lecithin is completely dissolved to obtain an egg yolk lecithin ethyl acetate solution.

[0074] (2) Add 20 ml of 95% ethanol to 2.0 g of polyvinylpyrrolidone K60 and sonicate for 1 h until the polyvinylpyrrolidone K60 is completely dissolved to obtain a polyvinylpyrrolidone K60 ethanol solution.

[0075] (3) Add 1.0 g of lycopene and polyvinylpyrrolidone K60 ethanol solution to the egg yolk lecithin ethyl acetate solution, reflux and stir at 50 °C for 4 h. The lycopene agglomerates and floats on the surface of the solution without dispersing into the solution, and no lycopene phospholipid complex solution is obtained.

[0076] Comparative Example 9

[0077] (1) Add 60 ml of ethyl acetate to 2.0 g of egg yolk lecithin, reflux and stir at 50 °C until the egg yolk lecithin is completely dissolved to obtain an egg yolk lecithin ethyl acetate solution.

[0078] (2) Add 20 ml of 95% ethanol to 2.0 g of polyvinylpyrrolidone K90 and sonicate for 1 h until the polyvinylpyrrolidone K90 is completely dissolved to obtain a polyvinylpyrrolidone K90 ethanol solution.

[0079] (3) Add 1.0 g of lycopene and polyvinylpyrrolidone K90 ethanol solution to the egg yolk lecithin ethyl acetate solution, reflux and stir at 50 °C for 4 h to obtain a lycopene polyvinylpyrrolidone egg yolk lecithin ethyl acetate complex solution.

[0080] (4) Stop heating and stirring, filter the lycopene polyvinylpyrrolidone egg yolk lecithin ethyl acetate complex solution by suction filtration, and rotary evaporate to remove its solvent to obtain a lycopene polyvinylpyrrolidone phospholipid complex. Place it in a vacuum drying oven at -0.1 MPa and 50 °C for drying for 5 h to obtain 1.76 g of the complex. The complex is viscous in the evaporating dish. When trying to scrape it off, the complex adheres between the evaporating dish and the medicine spoon and forms a silk-like substance, and it cannot be scraped off smoothly and cannot be weighed.

[0081] It was observed that during the suction filtration process, polyvinylpyrrolidone K90 agglomerated into a ball and did not dissolve in the complex solution to produce a synergistic effect with phospholipids.

[0082] The above-disclosed are only the preferred embodiments of the present invention. Of course, the scope of rights of the present invention cannot be limited thereby. Therefore, equivalent changes made according to the claims of the present invention still fall within the scope covered by the present invention.

Claims

1. A preparation method of a lycopene phospholipid complex, characterized in that, It includes the following steps: S1. Dissolve phospholipids in an ester solvent to obtain a phospholipid solution; S2. Dissolve povidone K30 in an alcohol solvent to obtain a povidone solution; S3. Add lycopene and the povidone solution to the phospholipid solution, and reflux and mix to obtain a composite solution; S4. Remove the solvent from the composite solution to obtain a lycopene phospholipid complex.

2. The preparation method of the lycopene phospholipid complex according to claim 1, characterized in that, The mass ratio of the lycopene, the phospholipids, and the povidone K30 is 1:2:2 to 10.

3. The preparation method of the lycopene phospholipid complex according to claim 1, characterized in that, The volume ratio of the ester solvent to the alcohol solvent is 6:

1.

4. The preparation method of the lycopene phospholipid complex according to claim 1, characterized in that, The phospholipids include one or more of egg yolk lecithin and soy lecithin; the ester solvent includes ethyl acetate; the alcohol solvent includes ethanol and methanol.

5. The preparation method of the lycopene phospholipid complex according to claim 1, wherein, The phospholipids include egg yolk lecithin; the alcohol solvent includes ethanol with a volume fraction of 95%.

6. The preparation method of the lycopene phospholipid complex according to claim 1, characterized in that, In step S1, the mass-to-volume ratio of the phospholipids to the ester solvent is 1 g:30 ml; in step S2, the mass-to-volume ratio of the povidone K30 to the alcohol solvent is 2 to 10 g:10 to 30 ml.

7. The preparation method of the lycopene phospholipid complex according to claim 1, characterized in that, In step S1, the way of dissolving the phospholipids in the ester solvent includes reflux stirring; in step S3, the way of reflux mixing includes reflux stirring; in step S4, the way of removing the solvent includes one or more of suction filtration, evaporation to dryness, rotary evaporation, and vacuum drying.

8. The preparation method of the lycopene phospholipid complex according to claim 7, characterized in that, In step S1, the temperature of the reflux stirring is 50°C; in step S3, the temperature of the reflux mixing is 50°C, and the time is 2 to 4 h.

9. A lycopene phospholipid complex obtained by the preparation method of the lycopene phospholipid complex according to claim 1.

10. Use of the lycopene phospholipid complex as described in claim 1, characterized in that, It is used in one or more of foods and health products.