CN103125946A - Lutein nanoparticle and its preparation method - Google Patents

Lutein nanoparticle and its preparation method Download PDF

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Publication number
CN103125946A
CN103125946A CN2013100635607A CN201310063560A CN103125946A CN 103125946 A CN103125946 A CN 103125946A CN 2013100635607 A CN2013100635607 A CN 2013100635607A CN 201310063560 A CN201310063560 A CN 201310063560A CN 103125946 A CN103125946 A CN 103125946A
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China
Prior art keywords
lutein
oil phase
water
eudragit
nanometer particle
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CN2013100635607A
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Chinese (zh)
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高子彬
张丽男
孙勇军
张莉
谢英花
刘磊
吴韶梅
杨恩芸
李硕
王晓君
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Hebei University of Science and Technology
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Hebei University of Science and Technology
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Priority to CN2013100635607A priority Critical patent/CN103125946A/en
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Abstract

The invention discloses a lutein nanoparticle and its preparation method to solve problems comprising bad stability and low bioavailability of lutein crystals. The lutein nanoparticle comprises 0.2-25 parts by weight of lutein, 10-70 parts by weight of a water phase, 1-20 parts by weight of eudragit L100-55, 3-30 parts by weight of 0.2mol/L NaOH, and 5-70 parts by weight of an oil phase. The preparation method comprises the following steps: adding eudragit L100-55 to the water phase to prepare an L100-55 water dispersion, successively adding lutein and the oil phase, stirring until complete dissolving, volatilizing the organic solvent, and carrying out spray drying to obtain the lutein nanoparticle. Compared with common lutein crystals, the lutein nanoparticle has the advantages of low temperature sensitivity, obviously-improved stability in air, obviously-enhanced illumination resistance, obviously-improved acid resistance, benefiting for the addition of lutein into foods and medicines, low production cost and use convenience.

Description

A kind of lutein nanometer particle and preparation method thereof
Technical field
The present invention relates to a kind of food or drug additive and preparation method, particularly lutein nanometer particle and preparation method thereof.
Background technology
Lutein is a kind of natural materials that extensively is present in the plants such as vegetables, flowers, fruit, is attributed to " carotenoids class " family's material.In medical experiment proof plant, contained natural carotenol is a kind of antioxidant of excellent performance, add a certain amount of lutein can prevent cell ageing and biological organs aging in food, the visual impairment that also can prevent simultaneously senile eyeball macula retinae to degenerate to cause and blind, by a series of medical research, carotenoid has been proposed as the cancer prevention agent, life extends agent, the ulcer inhibitor, the inhibitor of heart attack and coronary artery disease, simultaneously, also be used as painted in food industry and the nutrition and health care agent.Lutein is of great advantage to health, but find after deliberation, the light of lutein itself, poor heat stability, tolerance range to pH value of human body is little, lutein crystal is water insoluble, slightly soluble in oil, and itself is oxidation very easily, these characteristics have determined that the bioavailability of lutein crystal is very low, and its application is limited by very large.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of lutein nanometer particle that improves product stability and water dispersible and preparation method thereof.
The alleged problem of the present invention is solved by following technical scheme:
A kind of lutein nanometer particle, its special feature is: described lutein nanometer particulate material proportioning is counted by weight: lutein 0.2-25, water 10-70, Eudragit L100-55 1-20,0.2mol/L NaOH 3-30, oil phase 5-70; Wherein, described Eudragit L100-55 is acrylic acid and the ethyl acrylate copolymer of 1:1, and described oil phase is oxolane, carrene, dimethyl sulfoxide (DMSO) or chloroform.
Above-mentioned lutein nanometer particle, described lutein nanometer particulate material optimum ratio is counted by weight: lutein 0.5-10, water 15-60, Eudragit L100-55 2-15,0.2mol/L NaOH 5-26, oil phase 10-60.
Above-mentioned lutein nanometer particle, described aqueous phase adds additive, and described additive is a kind of or its mixture in soluble starch, sucrose, Vc-Na; Wherein, the soluble starch addition is 0.15-0.30g/mL, and the sucrose addition is 0.05-0.20g/mL, and the Vc-Na addition is 0.02-0.10g/mL; Described oil phase is oxolane.
A kind of method for preparing the lutein nanometer particle, it carries out as follows:
A, take lutein nanometer particulate material constituent by proportioning;
B, Eudragit L100-55 is joined aqueous phase stir, add 0.2mol/L NaOH to continue to stir 30-40min by proportional quantity, obtain the L100-55 aqueous dispersion;
C, the lutein of proportional quantity is added add oil phase after stirring in the L100-55 aqueous dispersion, until lutein is dissolved as mixed liquor fully;
D, the mixed liquor of c step is moved into 58-62 ℃ of water-bath, be stirred to oil phase and volatilize fully, obtain red slurry, spray-drying namely makes the lutein nanometer particle.
Above-mentioned lutein nanometer preparation method of granules, described aqueous phase adds additive to operate as follows: take cold water, additive by proportional quantity; Additive is added in cold water, after it dissolves fully, regulate water pH to 8-9 with 0.1moL/LNaOH solution.
The present invention is directed to existing lutein crystal poor stability, problem that bioavailability is low is improved, and by selecting additive, ingenious use enteric auxiliary material Eudragit L100-55, makes the spherical of 100-200nm or elliposoidal lutein nanometer particle.Show through contrast test, product of the present invention is than the Reduced susceptibility of common lutein crystal to temperature, and aerial stability obviously improves, and anti-illumination ability obviously strengthens, and acid-fast ability is also obviously heightened.Lutein nanometer particle by the present invention's preparation, disperse in Yi Zaishui, improved the tolerance of lutein to air, illumination, acid, improved the lutein transportation, the stability after storing and taking, be conducive to the interpolation of lutein in food and medicine, and production cost is low, easy to use.
Description of drawings
Fig. 1 is particle diameter distribution map of the present invention;
Fig. 2 is scanning electron microscope (SEM) photograph;
Fig. 3 is transmission electron microscope picture;
Fig. 4 is temperature influence curve to lutein crystal and nanoparticle stability thereof when being 40 ℃;
Fig. 5 is that air (oxygen) is to the influence curve of lutein crystal and nanoparticle stability thereof;
Fig. 6 is that illumination is to the influence curve of lutein crystal and nanoparticle stability thereof;
Fig. 7 is that acid (pH 1.0) is to the influence curve of lutein crystal and nanoparticle stability thereof.
The specific embodiment
The present invention is directed to and improve lutein stability and bioavailability, a kind of lutein nanometer particle and preparation method thereof is provided.The form of its product lutein nanometer particle is the spherical or ellipsoidal particle of 100-200nm.Quality and the pharmaceutical formulation of lutein nanometer particle product are closely related, and it is related to the indexs such as medicine homogeneity, stability, particle diameter.During the present invention filled a prescription and forms, the proportioning of each component not only directly affected product quality, also affects the bioavilability of medicine.The raw material proportioning of described lutein nanometer particle comprises the constituent of following weight parts: lutein 0.2-25, water 10-70, Eudragit L100-55 1-20,0.2mol/L NaOH 3-30, oil phase 5-70, its Lutein is lutein, and Eudragit L100-55 is acrylic acid and the ethyl acrylate copolymer of 1:1, and oil phase is oxolane or carrene or dimethyl sulfoxide (DMSO) or chloroform.The optimum ratio of described lutein nanometer particle comprises the constituent of following weight parts: lutein 0.5-10, water 15-60, Eudragit L100-55 2-15,0.2mol/L NaOH 5-26, oil phase 10-60.Described water preferably adds a kind of or its mixture in additive soluble starch, sucrose, Vc-Na, and wherein the soluble starch addition is 0.15-0.30g/mL, and the sucrose addition is 0.05-0.20g/mL, and the Vc-Na addition is 0.02-0.10g/mL; Described oil phase is oxolane.
The preparation method of lutein nanometer particle is: first the pharmaceutic adjuvant Eudragit L100-55 is added aqueous phase, make the L100-55 aqueous dispersion, more successively add lutein and oil phase, stir until medicine dissolves fully, with the organic solvent volatilization, spray-drying makes the lutein nanometer particle.Preparation method of the present invention is when adding NaOH by proportioning, hydrophilic and the hydrophobic grouping of L100-55 just in time is in such ratio: walk in the process of organic solvent in volatilization, lutein can constantly be separated out, and the lutein of separating out can be had the L100-55 parcel of proper proportion hydrophobic grouping, the hydrophilic radical of L100-55 is towards aqueous dispersion medium, with regard to making this slightly solubility material of lutein be distributed in water with the form of nanoparticle, improved the water dispersible of lutein like this; And due to the dissolution characteristics of L100-55 self, make this nanoparticle have the characteristic of enteric, avoided lutein destruction under one's belt.
Several specific embodiments of the invention below are provided:
Embodiment 1, take the constituent of preparation lutein nanometer particle: lutein 0.2Kg, water 10 Kg, Eudragit L100-55 1 Kg, 0.2mol/L NaOH 4 Kg, oxolane 7 Kg.
Embodiment 2, take the constituent of preparation lutein nanometer particle: lutein 0.5Kg, water 15 Kg, Eudragit L100-55 2 Kg, 0.2mol/L NaOH 5 Kg, carrene 10 Kg.
Embodiment 3, take the constituent of preparation lutein nanometer particle: lutein 0.3Kg, water 17 Kg, Eudragit L100-55 1.5 Kg, 0.2mol/L NaOH 3 Kg, chloroform 5 Kg.
Embodiment 4, take the constituent of preparation lutein nanometer particle: lutein 10Kg, water 60 Kg(aqueous phases contain soluble starch 15 Kg), Eudragit L100-55 15 Kg, 0.2mol/L NaOH 25Kg, dimethyl sulfoxide (DMSO) 60 Kg.
Embodiment 5, take the constituent of preparation lutein nanometer particle: lutein 25Kg, water 70 Kg(aqueous phases contain sucrose 3.5 Kg, Vc-Na 7 Kg), Eudragit L100-55 20 Kg, 0.2mol/L NaOH 30 Kg, oxolane 70 Kg.
Embodiment 6, take the constituent of preparation lutein nanometer particle: lutein 4Kg, water 50 Kg(aqueous phases contain sucrose 10 Kg, Vc-Na 1Kg), Eudragit L100-55 5 Kg, 0.2mol/L NaOH 25 Kg, oxolane 30 Kg.
Embodiment 7, take the constituent of preparation lutein nanometer particle: lutein 0.8Kg, water 26 Kg(aqueous phases contain soluble starch 4.7Kg, sucrose 4.7 Kg, Vc-Na 1Kg), Eudragit L100-55 3Kg, 0.2mol/L NaOH 20 Kg, oxolane 50 Kg.
The lutein nanometer preparation method of granules is as follows: take lutein nanometer particulate material constituent by the embodiment proportioning; Eudragit L100-55 is joined aqueous phase stir, add 0.2mol/L NaOH to continue to stir 30-40min by proportional quantity, obtain the L100-55 aqueous dispersion; The lutein of proportional quantity is added add oil phase after stirring in the L100-55 aqueous dispersion, until lutein is dissolved as mixed liquor fully; Above-mentioned mixed liquor is moved into 58-62 ℃ of water-bath, be stirred to oil phase and evaporate fully, obtain red slurry, spray-drying namely makes the lutein nanometer particle.If aqueous phase used contains additive, take cold water, additive by proportional quantity; Additive is added in cold water, after it dissolves fully, regulate water pH to 8-9 with 0.1moL/LNaOH solution.
The lutein nanometer particle that will prepare according to the proportioning of embodiment 7 carries out dispersion experiment in water: (100 rev/mins of rotating speeds, 50ml water) under the same conditions, disperse the 50mg lutein crystal or contain the lutein nanometer particle of 50mg lutein, 50mg lutein almost can not disperse in water, and the lutein nanometer particle that contains 50mg lutein disperseed in 50 seconds, was orange transparency liquid.
The lutein nanometer particle that will prepare according to the proportioning of embodiment 7 is investigated its particle diameter, form, stability etc., and result is as follows: its particle diameter is in 100 ~ 200nm left and right, spherical or elliposoidal.
Get the lutein nanometer particle of embodiment 7 preparations, its stability is as follows with lutein crystal contrast test data: the Reduced susceptibility of lutein nanometer particle to temperature, under the lutein nanometer particle condition of 40 ℃, 8 hours, storage rate is 94.2%, and under similarity condition, the storage rate of lutein crystal is 89.9%; The aerial stability of lutein nanometer particle obviously improves, oxidation resistance strengthens, and the lutein nanometer particle exposes the storage rate of 8 hours in air be 97.5%, and under similarity condition, the storage rate of lutein crystal is 90.1%; The anti-illumination ability of lutein nanometer particle obviously strengthens, and helps to contain the medicine of lutein or the storage and transport of food, and 8 hours storage rates of lutein nanometer particle solar radiation are 97.9%, and under similarity condition, the storage rate of lutein crystal is 91.5%; Lutein nanometer particle acid-fast ability is also obviously heightened, and helps lutein to avoid under one's belt destroying, and improves bioavilability, and the lutein nanometer particle is 96.9% at pH1.0,8 hours storage rates, and under similarity condition, the storage rate of lutein crystal is 85.3%.
In sum, the total lutein nanometer particle of goods of the present invention disperses in Yi Zaishui, improved the tolerance of lutein to air, illumination, acid, be conducive to the interpolation of lutein in food and medicine, improve the stability after transporting, storing and take, have good effect.

Claims (5)

1. lutein nanometer particle, it is characterized in that: described lutein nanometer particulate material proportioning is counted by weight: lutein 0.2-25, water 10-70, Eudragit L100-55 1-20,0.2mol/L NaOH 3-30, oil phase 5-70; Wherein, described Eudragit L100-55 is acrylic acid and the ethyl acrylate copolymer of 1:1, and oil phase is oxolane, carrene, dimethyl sulfoxide (DMSO) or chloroform.
2. lutein nanometer particle according to claim 1, it is characterized in that: described lutein nanometer particulate material proportioning is counted by weight: lutein 0.5-10, water 15-60, Eudragit L100-55 2-15,0.2mol/L NaOH 5-26, oil phase 10-60.
3. lutein nanometer particle according to claim 2, it is characterized in that: described aqueous phase adds additive, and described additive is a kind of or its mixture in soluble starch, sucrose, Vc-Na; Wherein, the soluble starch addition is 0.15-0.30g/mL, and the sucrose addition is 0.05-0.20g/mL, and the Vc-Na addition is 0.02-0.10g/mL; Described oil phase is oxolane.
4. method for preparing as claim 1,2 or 3 described lutein nanometer particles, it is characterized in that: it carries out as follows:
A, take lutein nanometer particulate material constituent by proportioning;
B, Eudragit L100-55 is joined aqueous phase stir, add 0.2mol/L NaOH to continue to stir 30-40min by proportional quantity, obtain the L100-55 aqueous dispersion;
C, the lutein of proportional quantity is added add oil phase after stirring in the L100-55 aqueous dispersion, until lutein is dissolved as mixed liquor fully;
D, the mixed liquor of c step is moved into 58-62 ℃ of water-bath, be stirred to oil phase and volatilize fully, obtain red slurry, spray-drying namely makes the lutein nanometer particle.
5. preparation method according to claim 4, it is characterized in that: described aqueous phase adds additive to operate as follows: take cold water, additive by proportional quantity; Additive is added in cold water, after it dissolves fully, regulate water pH to 8-9 with 0.1moL/LNaOH solution.
CN2013100635607A 2013-02-28 2013-02-28 Lutein nanoparticle and its preparation method Pending CN103125946A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1348483A (en) * 1999-04-29 2002-05-08 Basf公司 Stable, aqueous dispersions and stable, water-dispersible dry powders of xanthophylls, and production and use of the same
CN1391467A (en) * 1999-11-17 2003-01-15 泰谷生物技术有限公司 Method of microencapsulation
CN101177540A (en) * 2006-11-10 2008-05-14 浙江医药股份有限公司新昌制药厂 Method for preparing lutein water-soluble dry powder
CN101433528A (en) * 2008-11-19 2009-05-20 黑龙江省嘉宝生物技术开发有限公司 Method for preparing stable water dispersion xanthophyll microcapsule from xanthophyll crystal
EP1480736B1 (en) * 2002-02-01 2009-11-04 Kemin Foods, L.C. Microcapsules having high carotenoid content

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1348483A (en) * 1999-04-29 2002-05-08 Basf公司 Stable, aqueous dispersions and stable, water-dispersible dry powders of xanthophylls, and production and use of the same
CN1391467A (en) * 1999-11-17 2003-01-15 泰谷生物技术有限公司 Method of microencapsulation
EP1480736B1 (en) * 2002-02-01 2009-11-04 Kemin Foods, L.C. Microcapsules having high carotenoid content
CN101177540A (en) * 2006-11-10 2008-05-14 浙江医药股份有限公司新昌制药厂 Method for preparing lutein water-soluble dry powder
CN101433528A (en) * 2008-11-19 2009-05-20 黑龙江省嘉宝生物技术开发有限公司 Method for preparing stable water dispersion xanthophyll microcapsule from xanthophyll crystal

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
XIAO-YING QV,等: "Preparation of lutein microencapsulation by complex coacervation method and its physicochemical properties and stability", 《FOOD HYDROCOLLOIDS》 *

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Application publication date: 20130605