CN115778917A - Lutein microcapsule and preparation method and application thereof - Google Patents

Lutein microcapsule and preparation method and application thereof Download PDF

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Publication number
CN115778917A
CN115778917A CN202310002184.4A CN202310002184A CN115778917A CN 115778917 A CN115778917 A CN 115778917A CN 202310002184 A CN202310002184 A CN 202310002184A CN 115778917 A CN115778917 A CN 115778917A
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lutein
material solution
microcapsule
preparation
polyvinylpyrrolidone
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丁壮
王正平
韩军
王晓
王利利
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Haimen Pinshang Medicine Science & Technology Co ltd
Shandong Liangjian Biotechnology Co ltd
Liaocheng University
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Haimen Pinshang Medicine Science & Technology Co ltd
Shandong Liangjian Biotechnology Co ltd
Liaocheng University
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Abstract

The invention belongs to the technical field of pharmaceutical preparations, and discloses a lutein microcapsule, and a preparation method and application thereof. Mixing lutein and edible alcohol to obtain a core material solution; mixing esterified starch, polyvinylpyrrolidone and water to obtain a wall material solution; adding the core material solution into the wall material solution to obtain a coarse mixed suspension, and then homogenizing under high pressure to obtain a nano mixed suspension; and spray drying the nanometer suspension to obtain lutein microcapsules. The method adopts the esterified starch and the polyvinylpyrrolidone as wall materials, and the esterified starch and the polyvinylpyrrolidone have certain hydrophobic interaction, so that the molecular chain entanglement degree is higher, the embedding rate of the lutein is improved, and the embedding rate can be up to more than 95%.

Description

Lutein microcapsule and preparation method and application thereof
Technical Field
The invention relates to the technical field of pharmaceutical preparations, in particular to a lutein microcapsule and a preparation method and application thereof.
Background
Lutein (Lutein), also known as "phytoxanthin", a fat-soluble active substance. The structure of the lutein contains 40 carbon atoms, a large number of unsaturated carbon-carbon double bonds exist, two hydroxyl groups are connected to two ends of a long chain, and the polarity is strong. The unsaturated conjugated double bonds endow xanthophyll with strong antioxidant activity, and can remove free radicals, improve immunity, slow down cell aging, and protect retina. Lutein has good coloring effect, but has poor stability and is easily damaged by factors such as light, heat, oxygen, metal ions and the like. The gradual maturation and development of microcapsule technology has pointed out a new direction for the solution of these problems. The microcapsule technology has the functions of improving the stability of the core material, protecting sensitive food components, prolonging the shelf life of nutrient substances, covering or delaying the release of flavor substances, converting the core material into a solid substance easy to process and the like. The selection of the wall material of the microcapsule is crucial to the microencapsulation process and the properties of the final product, and the wall material determines the stability, the microencapsulation efficiency and the controlled release capability of the core material of the microcapsule. The prior patent document CN101288662A, "a lutein microcapsule and a preparation method thereof" discloses a preparation method of the lutein microcapsule. Firstly, dissolving lutein in an organic solvent, then mixing the lutein with Arabic gum for homogenization, then curing, treating the lutein with magnesium stearate after curing, and drying the lutein to obtain powder. The method has complicated process and low efficiency.
Therefore, the lutein microcapsule with high embedding rate, high storage stability and simple preparation process is provided, and has important significance for the development of the lutein microcapsule.
Disclosure of Invention
The invention aims to provide a lutein microcapsule, and a preparation method and application thereof, so as to solve the problems in the prior art.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a lutein microcapsule, which comprises the following steps:
(1) Mixing lutein with edible alcohol to obtain core material solution;
(2) Mixing esterified starch, polyvinylpyrrolidone and water to obtain a wall material solution;
(3) Adding the core material solution into the wall material solution to obtain a coarse mixed suspension, and then homogenizing under high pressure to obtain a nano mixed suspension;
(4) Spray drying the nanometer suspension to obtain lutein microcapsule;
the steps (1) and (2) are not limited in order.
Preferably, in the above preparation method of a lutein microcapsule, the esterified starch in step (2) is starch octenyl succinate, starch acetate or starch citrate.
Preferably, in the above preparation method of lutein microcapsule, the mass volume ratio of lutein to edible alcohol in step (1) is 0.5-2 g: 100-400 mL, wherein the concentration of the edible alcohol in the step (1) is 90-100 wt%.
Preferably, in the above preparation method of lutein microcapsule, the mass-to-volume ratio of lutein in step (1) to esterified starch, polyvinylpyrrolidone and water in step (2) is 0.5-2 g: 15-50 g: 8-12 g: 500-1200 mL.
Preferably, in the above method for preparing lutein microcapsule, the mixing temperature in the step (2) is 55-65 ℃.
Preferably, in the above preparation method of lutein microcapsule, the pressure for high-pressure homogenization in step (3) is 20 to 80MPa.
Preferably, in the above preparation method of lutein microcapsule, the spray drying conditions in step (4) are as follows: the inlet temperature is 160-180 ℃, the outlet temperature is 80-100 ℃, and the feeding speed is 6-20 mL/min.
The invention also provides the lutein microcapsule prepared by the preparation method of the lutein microcapsule.
The invention also provides an application of the lutein microcapsule in medicine preparation.
Through the technical scheme, compared with the prior art, the invention has the following beneficial effects:
(1) The invention adopts esterified starch and polyvinylpyrrolidone as wall materials, ester groups introduced by reaction of starch molecular chains and acid exist in the esterified starch, and the esterified starch is an amphiphilic material and has good film-forming property and emulsifying property; meanwhile, a certain hydrophobic interaction exists between the esterified starch and the polyvinylpyrrolidone, so that molecular chains in the formed composite wall material have higher entanglement degree, and the embedding rate of the lutein is improved.
(2) The lutein microcapsule prepared by the method has high embedding rate, and the effective loading capacity of lutein is higher and can reach more than 95%.
Detailed Description
The invention provides a preparation method of lutein microcapsules, which comprises the following steps:
(1) Mixing lutein with edible alcohol to obtain core material solution;
(2) Mixing esterified starch, polyvinylpyrrolidone and water to obtain a wall material solution;
(3) Adding the core material solution into the wall material solution to obtain a coarse mixed suspension, and then homogenizing under high pressure to obtain a nano mixed suspension;
(4) Spray drying the nanometer suspension to obtain lutein microcapsule;
the steps (1) and (2) are not limited in order.
In the present invention, the mass volume ratio of lutein to edible alcohol in the step (1) is preferably 0.5 to 2g:100 to 400mL, more preferably 0.5 to 1.2g:120 to 180mL, more preferably 0.6g:150mL.
In the present invention, the concentration of the edible alcohol in the step (1) is preferably 90 to 100wt%, more preferably 90, 92, 94, 95, 96, 98 or 100wt%, and still more preferably 94 or 95wt%.
In the present invention, the mass volume ratio of the lutein in the step (1) to the esterified starch, polyvinylpyrrolidone and water in the step (2) is preferably 0.5 to 2g: 15-50 g: 8-12 g:500 to 1200mL, more preferably 0.5 to 1.2g: 17-28 g: 7.5-11 g:750 to 1000mL, more preferably 0.6g:22.5g:10g:900mL.
In the present invention, the esterified starch in the step (2) is preferably starch octenyl succinate, starch acetate or starch citrate, more preferably starch octenyl succinate or starch citrate, and still more preferably starch octenyl succinate.
In the present invention, the specific process of mixing in step (2) is as follows: stirring for 2-4 h at the rotating speed of 100-130 r/min.
In the present invention, the temperature of mixing in the step (2) is preferably 55 to 65 ℃, more preferably 55, 56, 57, 58, 59, 60, 61, 62, 63, 64 or 65 ℃, and still more preferably 58, 59 or 60 ℃.
In the present invention, after the step (3) of adding the core material solution to the wall material solution, the method further comprises: obtaining coarse suspension through high-speed shearing, wherein the rotating speed of the high-speed shearing is preferably 8000-12000 r/min, more preferably 8000, 8500, 9000, 9500, 10000, 10500, 11000, 11500 or 12000r/min, and more preferably 10000, 10500 or 11000r/min; the time of the high-speed shearing is preferably 2 to 5min, more preferably 2, 2.5, 3, 3.5, 4, 4.5 or 5min, and still more preferably 3 or 3.5min.
In the present invention, the pressure for high-pressure homogenization in the step (3) is preferably 20 to 80MPa, more preferably 20, 25, 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, or 80MPa, and even more preferably 40, 45, or 50MPa.
In the present invention, the conditions of the spray drying in the step (4) are: the inlet temperature is preferably 160 to 180 ℃, more preferably 160, 162, 165, 167, 170, 173, 175, 178 or 180 ℃, and even more preferably 165, 167 or 170 ℃; the outlet temperature is preferably 80 to 100 ℃, more preferably 80, 82, 84, 85, 88, 90, 92, 94, 95, 98 or 100 ℃, and more preferably 88 or 90 ℃; the feed rate is preferably 6 to 20mL/min, more preferably 6, 8, 10, 12, 14, 15, 16, 18 or 20mL/min, and still more preferably 10, 12 or 14mL/min.
The invention also provides the lutein microcapsule prepared by the preparation method of the lutein microcapsule.
The invention also provides an application of the lutein microcapsule in medicine preparation.
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) Dissolving 0.6g xanthophyll in 150mL edible alcohol with 95wt% to obtain core material solution; mixing 18g of starch octenylsuccinate, 8g of polyvinylpyrrolidone and 900mL of deionized water, and stirring at 60 ℃ at a rotating speed of 120r/min for 2h to obtain a wall material solution;
(2) Adding the core material solution into the wall material solution, shearing and emulsifying at a rotation speed of 8000r/min for 3min to obtain a coarse suspension, and homogenizing under a pressure of 30MPa for 1 time to obtain a nano suspension;
(3) Spray drying the nanometer suspension to obtain lutein microcapsule; wherein the conditions in the spray drying process are as follows: the inlet temperature was 170 deg.C, the outlet temperature was 90 deg.C, and the feed rate was 15mL/min.
Example 2
(1) Dissolving 0.5g lutein in 100mL edible alcohol of 100wt% to obtain core material solution; mixing 22g of starch citrate, 9g of polyvinylpyrrolidone and 700mL of deionized water, and stirring at 65 ℃ at a rotating speed of 130r/min for 2.5 hours to obtain a wall material solution;
(2) Adding the core material solution into the wall material solution, shearing and emulsifying for 2min at the rotating speed of 10000r/min to obtain a coarse suspension, and homogenizing for 1 time at the pressure of 50MPa to obtain a nano suspension;
(3) Spray drying the nanometer suspension to obtain lutein microcapsule; wherein the conditions in the spray drying process are as follows: the inlet temperature was 165 deg.C, the outlet temperature 95 deg.C, and the feed rate 12mL/min.
Example 3
(1) Dissolving 1.8g of lutein in 400mL of 92wt% edible alcohol to obtain a core material solution; mixing 50g of starch acetate, 10.5g of polyvinylpyrrolidone and 1200mL of deionized water, and stirring at 60 ℃ at a rotating speed of 100r/min for 3 hours to obtain a wall material solution;
(2) Adding the core material solution into the wall material solution, shearing and emulsifying for 3min at the rotating speed of 11000r/min to obtain a coarse suspension, and homogenizing for 1 time under the pressure of 65MPa to obtain a nano suspension;
(3) Spray drying the nanometer suspension to obtain lutein microcapsule; wherein the conditions in the spray drying process are as follows: the inlet temperature was 175 deg.C, the outlet temperature was 85 deg.C, and the feed rate was 10mL/min.
Example 4
(1) Dissolving 0.5g lutein in 120mL 95wt% edible alcohol to obtain core material solution; mixing 28g of starch octenyl succinate, 11g of polyvinylpyrrolidone and 800mL of deionized water, and stirring at 60 ℃ at a rotating speed of 120r/min for 2 hours to obtain a wall material solution;
(2) Adding the core material solution into the wall material solution, shearing and emulsifying for 2min at the rotating speed of 12000r/min to obtain a coarse suspension, and homogenizing for 1 time under the pressure of 70MPa to obtain a nano suspension;
(3) Spray drying the nanometer suspension to obtain lutein microcapsule; wherein the conditions in the spray drying process are as follows: the inlet temperature was 180 ℃, the outlet temperature was 90 ℃ and the feed rate was 16mL/min.
Examples of the experiments
Determination of lutein microcapsule embedding rate:
(1) Determination of the total lutein content in the microcapsules:
weighing 100mg lutein microcapsule, adding 5mL purified water for ultrasonic treatment, after completely dissolving and cooling, fixing the volume to 100mL by absolute ethyl alcohol, shaking up, filtering, taking 1mL of the filtrate to a 25mL brown volumetric flask, fixing the volume to 25mL by absolute ethyl alcohol, taking absolute ethyl alcohol as blank liquid, measuring absorbance at 446nm, and repeating for three times. The calculation was performed according to the following formula:
Figure BDA0004035554590000061
in the formula: a: absorbance value of the sample solution at 446 nm; 2550: extinction coefficient of lutein in absolute ethanol; w: actual weight of sample, g.
(2) And (3) measuring the content of lutein on the surface of the microcapsule:
weighing 0.2g of microcapsules in a 10mL centrifuge tube, adding 10mL of n-hexane, violently shaking for 1min, centrifuging (3000 r/min) for 5min, taking 2mL of supernatant, drying by using nitrogen gas, redissolving in absolute ethyl alcohol, fixing the volume to a 25mL brown volumetric flask by using the absolute ethyl alcohol as a blank solution, measuring absorbance at 446nm, and repeating for three times. And (3) calculating according to the formula in (1).
(3) Determination of the encapsulation efficiency of the microcapsules:
carrying out corresponding experimental operation according to (1) the measurement of the total lutein content and (2) the measurement of the surface lutein content, and calculating the embedding rate according to the following formula:
Figure BDA0004035554590000062
TABLE 1 embedding Rate of lutein microcapsules
Sample (I) Percentage of incorporation/%)
Example 1 96.85
Example 2 95.93
Example 3 95.83
Example 4 96.37
The experimental results are shown in table 1, the embedding rate of the lutein microcapsule prepared by using the esterified starch and the polyvinylpyrrolidone as the wall materials can reach more than 95%, and the effective loading capacity of the lutein is high.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that it is obvious to those skilled in the art that various modifications and improvements can be made without departing from the principle of the present invention, and these modifications and improvements should also be considered as the protection scope of the present invention.

Claims (9)

1. A preparation method of lutein microcapsules is characterized by comprising the following steps:
(1) Mixing lutein with edible alcohol to obtain core material solution;
(2) Mixing esterified starch, polyvinylpyrrolidone and water to obtain a wall material solution;
(3) Adding the core material solution into the wall material solution to obtain a coarse mixed suspension, and then homogenizing under high pressure to obtain a nano mixed suspension;
(4) Spray drying the nanometer suspension to obtain lutein microcapsule;
the steps (1) and (2) are not limited in order.
2. The method for preparing lutein microcapsule according to claim 1, wherein the esterified starch in step (2) is octenyl succinate starch ester, acetate starch ester or citrate starch ester.
3. The preparation method of the lutein microcapsule according to claim 2, wherein the mass volume ratio of lutein to edible alcohol in the step (1) is 0.5-2 g: 100-400 mL, wherein the concentration of the edible alcohol in the step (1) is 90-100 wt%.
4. The preparation method of the lutein microcapsule according to claim 2 or 3, wherein the mass volume ratio of the lutein in step (1) to the esterified starch, polyvinylpyrrolidone and water in step (2) is 0.5-2 g: 15-50 g: 8-12 g: 500-1200 mL.
5. The method for preparing lutein microcapsule according to claim 4, wherein the temperature of mixing in the step (2) is 55-65 ℃.
6. The method for preparing lutein microcapsule according to claim 5, wherein the pressure of high pressure homogenization in step (3) is 20-80 MPa.
7. The process for preparing lutein microcapsules according to claim 5 or 6, wherein the conditions of spray drying in step (4) are: the inlet temperature is 160-180 ℃, the outlet temperature is 80-100 ℃, and the feeding speed is 6-20 mL/min.
8. The lutein microcapsule obtained by the method for preparing lutein microcapsule according to any one of claims 1 to 7.
9. Use of lutein microcapsules according to claim 8 in the preparation of a medicament.
CN202310002184.4A 2023-01-03 2023-01-03 Lutein microcapsule and preparation method and application thereof Pending CN115778917A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20160143332A1 (en) * 2014-11-26 2016-05-26 Omniactive Health Technologies Limited Stable oil suspensions with enhanced bioavailability and compositions thereof
CN107136503A (en) * 2017-04-10 2017-09-08 华南理工大学 A kind of method that starch embedding lutein prepares microcapsules

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20160143332A1 (en) * 2014-11-26 2016-05-26 Omniactive Health Technologies Limited Stable oil suspensions with enhanced bioavailability and compositions thereof
CN107136503A (en) * 2017-04-10 2017-09-08 华南理工大学 A kind of method that starch embedding lutein prepares microcapsules

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
PRAVIN B.NALAWADE 等: "Microencapsulation of lutein extracted from marigold flowers(Tagetes erecta L.) using full factorial design", JOURNAL OF DRUG DELIVERY SCIENCE AND TECHNOLOGY, no. 33, 1 April 2016 (2016-04-01), pages 75 - 87 *
王闯等: "叶黄素微胶囊化研究", 食品科学, vol. 32, no. 2, 31 December 2011 (2011-12-31), pages 43 - 47 *

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