Lycopene composition and emulsion preparation thereof

Abstract

The invention relates to a lycopene composition and an emulsion preparation thereof. The lycopene composition is prepared from lutein, beta-carotene, all-trans lycopene, 9-cis lycopene, 11-cis lycopene and 13-cis lycopene. The emulsion preparation also comprises an emulsifier, a co-emulsifier, an antioxidant and water, has good solubility in water, can obtain solutions with chromaticity of L30-35, a35-40 and b25-30, and is concentrated in tone value range and stable in tone coloring.

Description

Technical Field

[0001] This invention is a divisional application of patent application No. 2018115345366, filed on December 14, 2018, entitled "A Lycopene Composition and its Emulsion Formulation". This invention relates to the field of food processing technology, specifically to a lycopene composition and its emulsion formulation. Background Technology

[0002] Lycopene is a type of carotenoid. Its molecule contains many double bonds, which gives it strong antioxidant activity. It can prevent oxidative damage to cells and prevent cancer. In addition, lycopene can also prevent cardiovascular and cerebrovascular diseases and delay aging.

[0003] Lycopene emulsion is prepared by emulsification, homogenization, or grinding of lycopene composition, emulsifier, co-emulsifier, antioxidant, water, and other excipients. As a water-dispersible red pigment, lycopene emulsion can be uniformly dispersed in both oil-based and water-based media. This overcomes the shortcomings of lycopene, which cannot dissolve or disperse uniformly in water and thus cannot effectively exert its biological effects. It can be easily added to oil-based and water-based food systems, greatly expanding the application range of lycopene in food.

[0004] Chinese patent document CN101991175B discloses a lycopene microemulsion formulation with high cis isomer content and its preparation method. The formulation uses lycopene with high cis isomer content as the main active ingredient, and is prepared by microemulsification with edible surfactants, co-surfactants, edible oils, and water to produce a red, transparent or translucent emulsion product with droplet diameters of 5-50 nm. This invention prepares a high-cis lycopene microemulsion product. Chinese patent document CN107454824A discloses a lycopene composition with improved colorant properties, prepared by grinding crystalline lycopene crystals and excipients. The 10 ppm aqueous solution of this formulation has an L value of 42-47, an a value of 25-28, and a b value of 11.5-14. However, the food and beverage industry often requires products with different color tones. Summary of the Invention

[0005] The primary objective of this invention is to provide a novel lycopene composition comprising the following components: lutein, β-carotene, all-trans lycopene, 9-cis-lycopene, 11-cis-lycopene, and 13-cis-lycopene.

[0006] By combining the above components, a strawberry-colored lycopene colorant with a concentrated hue range and stable hue can be prepared.

[0007] Preferably, by weight, the composition comprises 0.1 to 2 parts of lutein; 0.01 to 1 part of β-carotene; 90 to 98 parts of all-trans lycopene; 1 to 3 parts of 9-cis-lycopene; 0.1 to 2 parts of 11-cis-lycopene; and 0.1 to 2 parts of 13-cis-lycopene.

[0008] As a preferred embodiment, each 100 parts by weight of the composition comprises 0.1 to 2 parts of lutein, 0.03 to 1 part of β-carotene, 91 to 97.7 parts of all-trans lycopene, 1 to 2.97 parts of 9-cis-lycopene, 0.1 to 2 parts of 11-cis-lycopene, and 0.1 to 2 parts of 13-cis-lycopene.

[0009] Lycopene is not easily soluble in water. To facilitate the application of the above composition, it is prepared into a water-soluble emulsion formulation so that it can exert its full effect.

[0010] As a preferred embodiment, the lycopene emulsion formulation comprising the lycopene composition of the present invention further includes an emulsifier, a co-emulsifier, an antioxidant, and water.

[0011] Adding emulsifiers, co-emulsifiers, and antioxidants to the emulsion formulation can increase the solubility of lycopene, giving it an ideal color tone during application in aqueous systems. Furthermore, the emulsion formulation also exhibits good stability.

[0012] Preferably, the emulsifier is a mixture of mono- and diglyceride fatty acid esters and sucrose esters, wherein the mass ratio of the mono- and diglyceride fatty acid esters to the sucrose ester is 2-3:1. The above emulsifier, when used to emulsify the lycopene composition, can improve the water dispersibility of the lycopene composition.

[0013] Preferably, the co-emulsifier is glycerol, which can increase the stability of the emulsion system and the emulsifying ability of the emulsifier.

[0014] Preferably, the antioxidant is ascorbic acid, which can increase the antioxidant capacity of the lycopene composition and extend the shelf life of the formulation.

[0015] More preferably, the raw materials for preparing the emulsion formulation include, by weight, 2 parts of the lycopene composition, 8-10 parts of the emulsifier, 43-50 parts of the co-emulsifier, 2.3-2.7 parts of the antioxidant, and 12.85-13.8 parts of water.

[0016] This invention also provides a method for preparing the emulsion formulation described herein, comprising the following steps: grinding with a sand mill at an online speed of 12-13 m / s until the content of the lycopene composition in the formulation is 10 ppm and the color of the aqueous solution is L. 30~35, a 35~40, b Stop grinding at 25-30 minutes. Grinding at an online speed of 12-13 m / s ensures that the particle size of the emulsion formulation is between 300-600 μm, resulting in an ideal color tone for the product.

[0017] Preferably, the temperature is controlled at 20~50℃ during the grinding process.

[0018] As a preferred operating method, the preparation method of the emulsion formulation includes the following steps: 1) Mix all the raw materials and add them to an emulsification tank. Heat the mixture to 70-80°C and shear emulsify it at 7000-9000 rpm for 10-20 minutes to obtain an emulsion suspension. 2) Grind the mixture using a sand mill at an online speed of 12-13 m / s until the lycopene composition in the preparation is 10 ppm, at which point the color of the aqueous solution will be L. 30~35, a 35~40, b Stop grinding at 25-30°C and control the grinding temperature at 20-50°C to obtain an emulsion preparation.

[0019] In this invention, L Representing black and white, 0 is black, 100 is white, and values ​​between 0 and 100 are gray; a Representing red and green, with positive values ​​for red and negative values ​​for green; b It represents yellow and blue, with positive values ​​for yellow and negative values ​​for blue.

[0020] The present invention also protects the use of the emulsion formulation described herein in coloring.

[0021] More preferably, the colorant is used in food, feed, and cosmetics.

[0022] Specifically, during application, the emulsion formulation is diluted to a concentration of 10 ppm for the lycopene composition. Through this dilution process, a color intensity L can be obtained. 30~35, a 35~40, b Colorants with a concentrated hue range of 25-30 and stable hue.

[0023] More preferably, in actual operation, the emulsion formulation described in this application can be diluted with water by 900 to 1100 times.

[0024] The present invention has the following beneficial effects: 1) This invention first proposes a lycopene pigment composition. By using this composition, a strawberry-colored lycopene colorant can be obtained by dissolving the pigment in water.

[0025] 2) The present invention further prepared an emulsion formulation containing this pigment composition, which is ideally soluble in water and yields a color of L. 30~35, a 35~40, b The colorant has a strength of 25-30. A 10 ppm aqueous solution of this formulation showed no significant fading after 10 days at room temperature, and the aqueous solution was free of floating oil and sediment, indicating good stability. Detailed Implementation

[0026] To make the objectives, technical solutions, and advantages of this invention clearer, the technical solutions of this invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of this invention, not all embodiments. Based on the embodiments of this invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this invention.

[0027] The mono- and diglycerides of fatty acids involved in the examples were obtained directly through purchase, and the ratio of monoglycerides to diglycerides conformed to the national standard GB1886.65-2015.

[0028] Example 1 This embodiment relates to a lycopene composition, which consists of the following components: The mass fraction of lutein is 0.1%, the mass fraction of β-carotene is 1.0%, the mass fraction of all-trans lycopene is 97.7%, the mass fraction of 9-cis-lycopene is 1.0%, the mass fraction of 11-cis-lycopene is 0.1%, the mass fraction of 13-cis-lycopene is 0.1%, and the total mass of the above components is 2 kg.

[0029] This embodiment also relates to a lycopene emulsion formulation comprising the above composition. The raw materials for preparing the formulation also include an emulsifier, 6 kg of mono- and diglyceride fatty acid esters, 2 kg of sucrose esters, 43 kg of glycerol as a co-emulsifier, 2.7 kg of ascorbic acid as an antioxidant, and 13 kg of water.

[0030] This embodiment also relates to a method for preparing such an emulsion formulation, including the following steps: 1) Mix all the raw materials and add them to an emulsification tank. Heat the mixture to 75°C and shear emulsify it at 8000 rpm for 15 minutes to obtain an emulsion suspension. 2) Grind the emulsion using a sand mill at an online speed of 12 m / s and control the grinding temperature at 50℃ to obtain the emulsion preparation.

[0031] The above emulsion preparation was diluted 1000 times with purified water, and the resulting solution had a hue value of L. 30, a 36, b 26.

[0032] Example 2 This embodiment relates to a lycopene composition, which consists of the following components: The mass fraction of lutein was 2.0%, β-carotene was 0.03%, all-trans lycopene was 91%, 9-cis-lycopene was 2.97%, 11-cis-lycopene was 2.0%, and 13-cis-lycopene was 2.0%. The total mass of the above composition is 26g.

[0033] This embodiment also relates to a lycopene emulsion formulation comprising the above composition, wherein the formulation further comprises 90g of emulsifier mono- and diglyceride fatty acid esters, 30g of sucrose ester, 650g of co-emulsifier glycerol, 30g of antioxidant ascorbic acid, and 180g of water.

[0034] This embodiment also relates to a method for preparing such an emulsion formulation, including the following steps: 1) Mix all the raw materials and add them to an emulsification tank. Heat the mixture to 75°C and shear emulsify it at 8000 rpm for 15 minutes to obtain an emulsion suspension. 2) Grind the emulsion using a sand mill at an online speed of 12.5 m / s and control the grinding temperature at 30℃ to obtain the emulsion preparation.

[0035] The above emulsion preparation was diluted 1000 times with purified water, and the resulting solution had a hue value of L. 35.00, a 38.00, b 30.00.

[0036] Example 3 This embodiment relates to a lycopene composition, which consists of the following components: The mass fraction of lutein is 1.00%, the mass fraction of β-carotene is 0.50%, the mass fraction of all-trans lycopene is 95.00%, the mass fraction of 9-cis-lycopene is 1.50%, the mass fraction of 11-cis-lycopene is 1.10%, the mass fraction of 13-cis-lycopene is 0.9%, and the total mass of the above composition is 6 kg.

[0037] This embodiment also relates to a lycopene emulsion formulation comprising the above-mentioned composition, wherein the formulation further comprises 20 kg of emulsifier mono- and diglyceride fatty acid esters, 10 kg of sucrose esters; 130 kg of co-emulsifier glycerol, 8 kg of antioxidant ascorbic acid, and 40 kg of water.

[0038] This embodiment also relates to a method for preparing such an emulsion formulation, including the following steps: 1) Mix all the raw materials and add them to an emulsification tank. Heat the mixture to 75°C and shear emulsify it at 8000 rpm for 15 minutes to obtain an emulsion suspension. 2) Grind the emulsion using a sand mill at an online speed of 13 m / s and control the grinding temperature at 50℃ to obtain the emulsion preparation.

[0039] The above emulsion preparation was diluted 1000 times with purified water, and the resulting solution had a hue value of L. 34.23, a 39.21, b 27.50.

[0040] Example 4 This embodiment relates to a lycopene composition, which consists of the following components: The mass fraction of lutein is 1.00%, the mass fraction of β-carotene is 0.50%, the mass fraction of all-trans lycopene is 95.00%, the mass fraction of 9-cis-lycopene is 1.50%, the mass fraction of 11-cis-lycopene is 1.10%, the mass fraction of 13-cis-lycopene is 0.9%, and the total mass of the above composition is 2.8 kg.

[0041] This embodiment also relates to a lycopene emulsion formulation comprising the above composition, wherein the formulation further comprises 10.5 kg of emulsifier mono- and diglyceride fatty acid esters, 3.5 kg of sucrose esters; 63 kg of co-emulsifier glycerol, 3.5 kg of antioxidant ascorbic acid, and 18 kg of water.

[0042] This embodiment also relates to a method for preparing such an emulsion formulation, including the following steps: 1) Mix all the raw materials and add them to an emulsification tank. Heat the mixture to 75°C and shear emulsify it at 8000 rpm for 15 minutes to obtain an emulsion suspension. 2) Grind the emulsion using a sand mill at an online speed of 13 m / s and control the grinding temperature at 40℃ to obtain the emulsion preparation.

[0043] The above emulsion preparation was diluted 1000 times with purified water, and the resulting solution had a hue value of L. 34.23, a 39.21, b 27.50.

[0044] Comparative Example 1 Compared with Example 1, the difference is that the lycopene composition has a mass fraction of 5.00% lutein, 0.50% β-carotene, 91.00% all-trans lycopene, 1.50% 9-cis lycopene, 1.10% 11-cis lycopene, and 0.9% 13-cis lycopene.

[0045] The above emulsion preparation was diluted 1000 times with purified water, and the resulting solution had a hue value of L. 33.45, a 30.12, b 38.48.

[0046] Comparative Example 2 Compared to Example 1, the difference is that no emulsifier is added to the emulsion formulation, and the emulsion formulation is diluted 1000 times with purified water, resulting in a solution with a hue value of L. 56.48, a 12.36, b 6.02.

[0047] Comparative Example 3 Compared to Example 1, the difference lies in the addition of the emulsifier Tween-80 to the emulsion formulation, and the dilution of the emulsion formulation with purified water 1000 times, resulting in a solution with a color value of L. 42.14, a 28.63, b 21.36.

[0048] Comparative Example 4 Compared with Example 1, the difference lies in the method for preparing the formulation, which includes the following steps: grinding with a sand mill at an online speed of 10 m / s, diluting the above emulsion formulation 1000 times with purified water, and obtaining a solution with a hue value of L. 42.00, a 28. 09, b 23.12.

[0049] Experimental Example This experimental example involves testing the stability of the prepared colorant. Experimental subjects: colorants prepared in Examples 1-4 and Comparative Examples 1-4.

[0050] Experimental Method: The colorants of Examples 1-4 and Comparative Examples 1-4 were diluted 1000 times and placed at 4-8℃ for 6 months. The layering of the formulation was observed. Stability was expressed as the ratio of the upper layer ratio to the lower layer ratio. The results are shown in Table 1. Table 1

[0051] As can be seen from Table 1, the colorant of this application has good stability.

[0052] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A lycopene emulsion formulation, characterized in that, The raw materials for preparing the emulsion formulation include a lycopene composition, an emulsifier, a co-emulsifier, an antioxidant, and water; The lycopene composition comprises, by weight, 0.1-2 parts of lutein, 0.01-1 parts of β-carotene, 90-98 parts of all-trans lycopene, 1-3 parts of 9-cis lycopene, 0.1-2 parts of 11-cis lycopene and 0.1-2 parts of 13-cis lycopene; The emulsifier is a mixture of mono- and diglyceride fatty acid esters and sucrose esters, wherein the mass ratio of the mono- and diglyceride fatty acid esters to the sucrose esters is 2-3:

1.

2. The lycopene emulsion formulation according to claim 1, characterized in that, Each 100 parts by weight of the lycopene composition comprises 0.1 to 2 parts of lutein, 0.03 to 1 part of β-carotene, 91 to 97.7 parts of all-trans lycopene, 1 to 2.97 parts of 9-cis-lycopene, 0.1 to 2 parts of 11-cis-lycopene, and 0.1 to 2 parts of 13-cis-lycopene.

3. The emulsion formulation according to claim 1 or 2, characterized in that, The co-emulsifier is glycerin.

4. The emulsion formulation according to any one of claims 1 to 3, characterized in that, The antioxidant is ascorbic acid.

5. The emulsion formulation according to any one of claims 1 to 4, characterized in that, The raw materials for preparing the emulsion formulation, by weight, include 2 parts of the lycopene composition, 8-10 parts of the emulsifier, 43-50 parts of the co-emulsifier, 2.3-2.7 parts of the antioxidant, and 12.85-13.8 parts of water.

6. The emulsion formulation according to any one of claims 1 to 5, characterized in that, The particle size D of the material in the emulsion formulation 50 The thickness is 0.3~0.6μm.

7. The method for preparing the emulsion formulation according to any one of claims 1 to 6, characterized in that, During the grinding process of the emulsion formulation, the linear speed of the mill is controlled at 12-13 m / s, and the grinding continues until the content of the lycopene composition in the formulation is 10 ppm, at which point the color of the aqueous solution is L. 30~35, a 35~40, b Stop between 25 and 30.

8. The use of the emulsion formulation according to any one of claims 1 to 6 in the coloring of food, beverages and cosmetics.

9. The application according to claim 8, characterized in that, The emulsion formulation is diluted to a concentration of 10 ppm for the lycopene composition.

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