Lutein microcapsule and its preparation method and application

Abstract

The present invention belongs to the technical field of pharmaceutical preparations, and discloses a lutein microcapsule and a preparation method and application thereof. The present invention mixes lutein with edible alcohol to obtain a core material solution; mixes esterified starch, polyvinyl pyrrolidone and water to obtain a wall material solution; adds the core material solution to the wall material solution to obtain a coarse suspension, and then homogenizes it under high pressure to obtain a nanosuspension; and spray-dries the nanosuspension to obtain a lutein microcapsule. The present invention uses esterified starch and polyvinyl pyrrolidone as wall materials, and there is a certain hydrophobic interaction between the esterified starch and polyvinyl pyrrolidone, so that the molecular chain entanglement degree is relatively high, so as to improve the embedding rate of lutein, and the embedding rate can be as high as more than 95%.

Description

Technical Field

[0001] The present invention relates to the technical field of pharmaceutical preparations, and in particular to a lutein microcapsule and a preparation method and application thereof. Background Art

[0002] Lutein, also known as "plant lutein," is a fat-soluble active substance. Lutein's structure contains 40 carbon atoms, numerous unsaturated carbon-carbon double bonds, and two hydroxyl groups at each end of the long chain, giving it a strong polarity. These numerous unsaturated conjugated double bonds endow lutein with potent antioxidant activity, which can scavenge free radicals, boost the body's immune system, slow cell aging, and protect the retina. Lutein also has excellent coloring properties, but its stability is extremely poor and it is easily damaged by factors such as light, heat, oxygen, and metal ions. The gradual maturity and development of microencapsulation technology has pointed to new directions for addressing these issues. Microencapsulation technology can improve the stability of the core material, protect sensitive food ingredients, extend the shelf life of nutrients, mask or delay the release of flavor compounds, and transform the core material into a readily manageable solid. The selection of the microcapsule wall material is crucial to the microencapsulation process and the properties of the final product. The wall material determines microcapsule stability, microencapsulation efficiency, and the ability to control the release of the core material. Patent document CN101288662A, "A Lutein Microcapsule and Its Preparation Method," discloses a method for preparing lutein microcapsules. This method involves dissolving lutein in an organic solvent, homogenizing the mixture with gum arabic, and then solidifying the solution. After solidification, the solution is treated with magnesium stearate and dried to obtain a powder. This method is complex and inefficient.

[0003] Therefore, providing a lutein microcapsule with high embedding efficiency, high storage stability and simple preparation process is of great significance for the development of lutein microcapsules. Summary of the Invention

[0004] The purpose of the present invention is to provide a lutein microcapsule and a preparation method and application thereof, so as to solve the problems existing in the prior art.

[0005] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:

[0006] The present invention provides a method for preparing lutein microcapsules, comprising the following steps:

[0007] (1) mixing lutein with edible alcohol to obtain a core material solution;

[0008] (2) mixing esterified starch, polyvinyl pyrrolidone, and water to obtain a wall material solution;

[0009] (3) adding the core material solution to the wall material solution to obtain a coarse suspension, which is then homogenized under high pressure to obtain a nanosuspension;

[0010] (4) the nanosuspension is spray-dried to obtain lutein microcapsules;

[0011] There is no restriction on the order of steps (1) and (2).

[0012] Preferably, in the above-mentioned method for preparing lutein microcapsules, the esterified starch in step (2) is starch octenylsuccinate, starch acetate or starch citrate.

[0013] Preferably, in the above-mentioned method for preparing lutein microcapsules, the mass volume ratio of lutein to edible alcohol in step (1) is 0.5-2 g:100-400 mL, and the concentration of edible alcohol in step (1) is 90-100 wt%.

[0014] Preferably, in the above-mentioned method for preparing lutein microcapsules, the mass volume ratio of lutein in step (1) to esterified starch, polyvinyl pyrrolidone and water in step (2) is 0.5-2g:15-50g:8-12g:500-1200mL.

[0015] Preferably, in the above-mentioned method for preparing lutein microcapsules, the mixing temperature in step (2) is 55-65°C.

[0016] Preferably, in the above-mentioned method for preparing lutein microcapsules, the pressure of the high-pressure homogenization in step (3) is 20 to 80 MPa.

[0017] Preferably, in the above-mentioned method for preparing lutein microcapsules, the spray drying conditions in step (4) are: inlet temperature of 160-180°C, outlet temperature of 80-100°C, and feed rate of 6-20 mL / min.

[0018] The present invention also provides lutein microcapsules prepared by the above-mentioned lutein microcapsule preparation method.

[0019] The present invention also provides an application of lutein microcapsules in medicine preparation.

[0020] It can be seen from the above technical solutions that compared with the prior art, the present invention has the following beneficial effects:

[0021] (1) The present invention uses esterified starch and polyvinyl pyrrolidone as wall materials. The esterified starch contains ester groups introduced by the reaction of the starch molecular chain with acid, which is an amphiphilic material with good film-forming and emulsifying properties. At the same time, there is a certain hydrophobic interaction between the esterified starch and polyvinyl pyrrolidone, so that the molecular chains in the formed composite wall material have a high degree of entanglement, thereby improving the encapsulation rate of lutein.

[0022] (2) The lutein microcapsules prepared by the present invention have a high embedding rate and a high effective loading capacity of lutein, which can be as high as 95% or more. DETAILED DESCRIPTION

[0023] The present invention provides a method for preparing lutein microcapsules, comprising the following steps:

[0024] (1) mixing lutein with edible alcohol to obtain a core material solution;

[0025] (2) mixing esterified starch, polyvinyl pyrrolidone, and water to obtain a wall material solution;

[0026] (3) adding the core material solution to the wall material solution to obtain a coarse suspension, which is then homogenized under high pressure to obtain a nanosuspension;

[0027] (4) the nanosuspension is spray-dried to obtain lutein microcapsules;

[0028] There is no restriction on the order of steps (1) and (2).

[0029] In the present invention, the mass volume ratio of lutein to edible alcohol in step (1) is preferably 0.5-2 g:100-400 mL, more preferably 0.5-1.2 g:120-180 mL, and more preferably 0.6 g:150 mL.

[0030] In the present invention, the concentration of edible alcohol in step (1) is preferably 90-100 wt%, more preferably 90, 92, 94, 95, 96, 98 or 100 wt%, and more preferably 94 or 95 wt%.

[0031] In the present invention, the mass volume ratio of lutein in step (1) to esterified starch, polyvinyl pyrrolidone and water in step (2) is preferably 0.5-2g:15-50g:8-12g:500-1200mL, more preferably 0.5-1.2g:17-28g:7.5-11g:750-1000mL, and more preferably 0.6g:22.5g:10g:900mL.

[0032] In the present invention, the esterified starch in step (2) is preferably starch octenylsuccinate, starch acetate or starch citrate, more preferably starch octenylsuccinate or starch citrate, and more preferably starch octenylsuccinate.

[0033] In the present invention, the specific process of mixing in step (2) is: stirring at a rotation speed of 100 to 130 r / min for 2 to 4 hours.

[0034] In the present invention, the mixing temperature in step (2) is preferably 55-65°C, more preferably 55, 56, 57, 58, 59, 60, 61, 62, 63, 64 or 65°C, and more preferably 58, 59 or 60°C.

[0035] In the present invention, after adding the core material solution to the wall material solution in step (3), the step further includes: obtaining a coarse suspension by high-speed shearing, wherein the rotation speed of the high-speed shearing is preferably 8000-12000 r / min, more preferably 8000, 8500, 9000, 9500, 10000, 10500, 11000, 11500 or 12000 r / min, further preferably 10000, 10500 or 11000 r / min; the time of the high-speed shearing is preferably 2-5 min, more preferably 2, 2.5, 3, 3.5, 4, 4.5 or 5 min, more preferably 3 or 3.5 min.

[0036] In the present invention, the pressure of the high-pressure homogenization in step (3) is preferably 20 to 80 MPa, more preferably 20, 25, 30, 35, 40, 45, 50, 55, 60, 65, 70, 75 or 80 MPa, and more preferably 40, 45 or 50 MPa.

[0037] In the present invention, the spray drying conditions in step (4) are as follows: the inlet temperature is preferably 160-180°C, more preferably 160, 162, 165, 167, 170, 173, 175, 178 or 180°C, more preferably 165, 167 or 170°C; the outlet temperature is preferably 80-100°C, more preferably 80, 82, 84, 85, 88, 90, 92, 94, 95, 98 or 100°C, more preferably 88 or 90°C; the feed rate is preferably 6-20 mL / min, more preferably 6, 8, 10, 12, 14, 15, 16, 18 or 20 mL / min, more preferably 10, 12 or 14 mL / min.

[0038] The present invention also provides lutein microcapsules prepared by the above-mentioned lutein microcapsule preparation method.

[0039] The present invention also provides an application of lutein microcapsules in medicine preparation.

[0040] The following is a clear and complete description of the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts are within the scope of protection of the present invention.

[0041] Example 1

[0042] (1) 0.6 g of lutein was dissolved in 150 mL of 95 wt% edible alcohol to obtain a core material solution; 18 g of octenyl succinate starch, 8 g of polyvinylpyrrolidone, and 900 mL of deionized water were mixed, and then stirred at 60°C and 120 r / min for 2 h to obtain a wall material solution;

[0043] (2) adding the core material solution to the wall material solution, and then shearing and emulsifying at a speed of 8000 r / min for 3 min to obtain a coarse suspension, and then homogenizing once at a pressure of 30 MPa to obtain a nanosuspension;

[0044] (3) The nanosuspension was spray-dried to obtain lutein microcapsules; wherein, the conditions during the spray-drying process were: inlet temperature of 170°C, outlet temperature of 90°C, and feed rate of 15 mL / min.

[0045] Example 2

[0046] (1) 0.5 g of lutein was dissolved in 100 mL of 100 wt% edible alcohol to obtain a core material solution; 22 g of starch citrate, 9 g of polyvinylpyrrolidone, and 700 mL of deionized water were mixed, and then stirred at 65°C and 130 r / min for 2.5 h to obtain a wall material solution;

[0047] (2) adding the core material solution to the wall material solution, and then shearing and emulsifying at a speed of 10000 r / min for 2 min to obtain a coarse suspension, and then homogenizing once at a pressure of 50 MPa to obtain a nanosuspension;

[0048] (3) The nanosuspension was spray-dried to obtain lutein microcapsules; wherein, the conditions during the spray-drying process were: inlet temperature of 165°C, outlet temperature of 95°C, and feed rate of 12 mL / min.

[0049] Example 3

[0050] (1) 1.8 g of lutein was dissolved in 400 mL of 92 wt% edible alcohol to obtain a core material solution; 50 g of starch acetate, 10.5 g of polyvinylpyrrolidone, and 1200 mL of deionized water were mixed, and then stirred at 60°C and 100 rpm for 3 h to obtain a wall material solution;

[0051] (2) The core material solution was added to the wall material solution, and then sheared and emulsified at a speed of 11000 r / min for 3 min to obtain a coarse suspension, and then homogenized once at a pressure of 65 MPa to obtain a nanosuspension;

[0052] (3) The nanosuspension was spray-dried to obtain lutein microcapsules; wherein, the conditions during the spray-drying process were: inlet temperature of 175°C, outlet temperature of 85°C, and feed rate of 10 mL / min.

[0053] Example 4

[0054] (1) 0.5 g of lutein was dissolved in 120 mL of 95 wt% edible alcohol to obtain a core material solution; 28 g of octenyl succinate starch, 11 g of polyvinyl pyrrolidone, and 800 mL of deionized water were mixed, and then stirred at 60°C and 120 r / min for 2 h to obtain a wall material solution;

[0055] (2) adding the core material solution to the wall material solution, and then shearing and emulsifying at a speed of 12000 r / min for 2 min to obtain a coarse suspension, and then homogenizing once at a pressure of 70 MPa to obtain a nanosuspension;

[0056] (3) The nanosuspension was spray-dried to obtain lutein microcapsules; wherein, the conditions during the spray-drying process were: inlet temperature of 180°C, outlet temperature of 90°C, and feed rate of 16 mL / min.

[0057] Experimental example

[0058] Determination of lutein microcapsule embedding efficiency:

[0059] (1) Determination of total lutein content in microcapsules:

[0060] Weigh 100 mg of lutein microcapsules, add 5 mL of purified water, sonicate, and dissolve completely. After cooling, dilute to 100 mL with anhydrous ethanol. Shake well and filter. Transfer 1 mL of the filtrate to a 25 mL brown volumetric flask and dilute to 25 mL with anhydrous ethanol. Measure the absorbance at 446 nm using anhydrous ethanol as the blank solution. Repeat three times. Calculate according to the following formula:

[0061]

[0062] Where: A: absorbance of the sample solution at 446 nm; 2550: extinction coefficient of lutein in anhydrous ethanol; W: actual weight of the sample, g.

[0063] (2) Determination of lutein content on the surface of microcapsules:

[0064] Weigh 0.2 g of microcapsules into a 10 mL centrifuge tube, add 10 mL of n-hexane, shake vigorously for 1 min, centrifuge (3000 r / min) for 5 min, take 2 mL of the upper layer, blow dry with nitrogen, and redissolve in anhydrous ethanol. Use anhydrous ethanol to make up the volume to a 25 mL brown volumetric flask. Use anhydrous ethanol as the blank solution and measure the absorbance at 446 nm. Repeat three times. Calculate according to the formula in (1).

[0065] (3) Determination of microcapsule embedding efficiency:

[0066] The corresponding experimental operations were performed according to (1) the determination of total lutein content and (2) the determination of surface lutein content, and the embedding rate was calculated according to the following formula:

[0067]

[0068] Table 1 Lutein microcapsule embedding efficiency

[0069] sample Embedding rate / % Example 1 96.85 Example 2 95.93 Example 3 95.83 Example 4 96.37

[0070] The experimental results are shown in Table 1. The lutein microcapsules prepared by using esterified starch and polyvinyl pyrrolidone as wall materials have an embedding rate of over 95%, and the effective loading capacity of lutein is relatively high.

[0071] The above is only a preferred embodiment of the present invention. It should be pointed out that ordinary technicians in this technical field can make several improvements and modifications without departing from the principles of the present invention. These improvements and modifications should also be regarded as within the scope of protection of the present invention.

Claims

1. A method for preparing lutein microcapsules, characterized in that: The following steps are involved: (1) mixing lutein with edible alcohol to obtain a core material solution; (2) mixing esterified starch, polyvinyl pyrrolidone and water to obtain a wall material solution; (3) adding the core material solution to the wall material solution to obtain a coarse suspension, and then homogenizing under high pressure to obtain a nanosuspension; (4) the nanosuspension is spray-dried to obtain lutein microcapsules; There is no order restriction for steps (1) and (2); The mass volume ratio of lutein in step (1) to esterified starch, polyvinyl pyrrolidone and water in step (2) is 0.5-2 g: 15-50 g: 8-12 g: 500-1200 mL; The pressure of high pressure homogenization in step (3) is 20-80 MPa; In the step (2), the esterified starch is octenyl succinate starch, acetate starch or citrate starch; The mass volume ratio of lutein to edible alcohol in step (1) is 0.5-2 g:100-400 mL, and the concentration of edible alcohol in step (1) is 90-100 wt %.

2. The method for preparing lutein microcapsules according to claim 1, characterized in that: The mixing temperature in step (2) is 55-65°C.

3. The method for preparing lutein microcapsules according to claim 1, characterized in that: The spray drying conditions in step (4) are: inlet temperature of 160-180° C., outlet temperature of 80-100° C., and feed rate of 6-20 mL / min.

4. Lutein microcapsules prepared by the method for preparing lutein microcapsules according to any one of claims 1 to 3.

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