CN107019669B - Zeaxanthin nanosuspension and preparation method thereof - Google Patents

Zeaxanthin nanosuspension and preparation method thereof Download PDF

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CN107019669B
CN107019669B CN201710240773.0A CN201710240773A CN107019669B CN 107019669 B CN107019669 B CN 107019669B CN 201710240773 A CN201710240773 A CN 201710240773A CN 107019669 B CN107019669 B CN 107019669B
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zeaxanthin
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vegetable oil
antioxidant
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CN107019669A (en
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李勇
刘温来
李田田
杨国强
王晓燕
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SHANDONG TIANYIN BIOTECHNOLOGY CO Ltd
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    • A61K47/44—Oils, fats or waxes according to two or more groups of A61K47/02-A61K47/42; Natural or modified natural oils, fats or waxes, e.g. castor oil, polyethoxylated castor oil, montan wax, lignite, shellac, rosin, beeswax or lanolin
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Abstract

A zeaxanthin nanosuspension and a preparation method thereof belong to the technical field of food additive preparation, and are characterized in that the zeaxanthin nanosuspension comprises, by weight, 50 ~ parts of vegetable oil, 0.1 ~.0 parts of antioxidant, 0.1 ~.0 parts of emulsifier, and 6 ~ parts of zeaxanthin crystals with the content of 60% 3680%, and the zeaxanthin nanosuspension comprises the following steps of A) mixing the emulsifier, the antioxidant and the vegetable oil, heating to 35 ℃ and ~ ℃, fully stirring and mixing uniformly, B) carrying out superfine grinding on zeaxanthin, adding the zeaxanthin into the vegetable oil mixed liquid, C) carrying out high shear emulsifying machine to obtain a coarse nanosuspension, D) carrying out high energy emulsifying equipment on the coarse nanosuspension to reduce the particle size to a nanometer level, and preparing the zeaxanthin nanosuspension.

Description

Zeaxanthin nanosuspension and preparation method thereof
Technical Field
A zeaxanthin nano suspension and a preparation method thereof belong to the technical field of food additive preparation.
Background
Zeaxanthin belongs to isoprenoids, is an oxygen-containing carotenoid, belongs to an isomer with xanthophyll, and is widely present in green leaf vegetables, flowers, fruits and yellow corn. Often coexisting in nature with lutein, beta-carotene, cryptoxanthin, etc., constitute carotenoid mixtures.
Zeaxanthin is a novel oil-soluble natural pigment with high nutritive value and is also a compound necessary for human bodies. In human body, zeaxanthin is a strong antioxidant, can protect body cells through antioxidant actions such as quenching singlet oxygen and scavenging free radicals, and also has physiological functions such as anticancer effect, cardiovascular disease prevention and cataract prevention. In addition, the zeaxanthin has high nutritive value, can be converted into bioactive vitamin A in human liver after being eaten, and has special effects of promoting the growth and development of human body, protecting eyesight and epithelial cells, improving disease resistance, prolonging life and the like.
Zeaxanthin cannot be synthesized by a human body and can only be supplemented by food containing lutein, but the content of carotenoid in common food is low, and a certain amount of zeaxanthin added into food can not only meet the basic requirements of the human body, but also play a certain role in health care.
Zeaxanthin contains a unique conjugated double bond structure which determines its instability, is easily oxidized and isomerized under the conditions of illumination, high temperature and oxygen, and is not favorable for storage and application. In order to solve the problem, the zeaxanthin crystals can be crushed and suspended in the vegetable oil to obtain a zeaxanthin oil suspension, but the particle size of the zeaxanthin crystals in the final product is large, the bioavailability of the product is low, the product is easy to precipitate, and the product is easy to separate after being stored for a period of time.
At present, no patent report is found on the preparation of the zeaxanthin nano suspension at home and abroad. According to the invention, the zeaxanthin is dispersed in the vegetable oil, and the particle size reaches the nanometer level through the high-energy emulsification equipment, so that the liquid drop is finer and the particle size distribution is narrower, therefore, the generated suspension has better stability, the physical stability of the zeaxanthin oil suspension is improved, and the bioavailability of the zeaxanthin is improved.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcomes the defects of the prior art, and provides a zeaxanthin nano suspension with high stability and high bioavailability and a preparation method thereof.
The zeaxanthin nano suspension is characterized by comprising, by weight, 50 parts of vegetable oil, 50 parts of 50 ~ 90 parts of antioxidant, 0.1 part of 0.1 ~ 5.0.0 part of emulsifier, 0.1 part of 0.1 ~ 6.0.0 part of the antioxidant, and 6 parts of 6 ~ 40 parts of zeaxanthin with the zeaxanthin crystal content of 60% ~ 80% and 6 parts of ~ parts of zeaxanthin.
The particle size of the nanosuspension prepared by the formula and the matching process reaches the nanometer level, so that the nanosuspension is more beneficial to the absorption and utilization of a human body, and the bioavailability of the zeaxanthin is improved. The zeaxanthin is uniformly dispersed in the vegetable oil in the formula, the oil solubility is good, the application range of the zeaxanthin is widened, and the zeaxanthin can be used in food, medicine and health care products, including products such as cream, edible oil, sandwich, salad sauce and the like, and can also be used for preparing core materials of soft capsules.
Preferably, the constituents include (by weight portions) vegetable oil 65 ~ 75 parts, antioxidant 2.3 ~ 3.7.7 parts, emulsifying agent 3.2 ~ 4.2.2 parts, zeaxanthin crystal content 60% ~ 80% zeaxanthin 18 ~ 22 parts.
The optimal weight ratio can ensure that the zeaxanthin is more uniformly dispersed into the vegetable oil to achieve a state similar to activation, and the activity is better, thereby achieving better oil solubility.
Preferably, the emulsifier in the step A) is one or a mixture of more than two of lecithin, monoglyceride, span and Tween. The invention provides a plurality of emulsifier choices, which can meet the basic requirements of the invention.
Preferably, the emulsifier in the step A) is a mixed emulsifier prepared from lecithin and span according to the mass ratio of 7 ~ 9.6.6: 1.
The inventors also provide an emulsifier which is most effective in the present invention. The two emulsifiers are required to be mixed according to a specific ratio, the adaptability is best in the invention, and after the two emulsifiers are mixed with the antioxidant and the vegetable oil, the zeaxanthin crystals are coated more uniformly, and the particle size of the obtained nano-particles is more uniform.
Preferably, the antioxidant in step a) is one or more than two mixed antioxidants selected from tea polyphenol, phytic acid, mixed tocopherol, flavonoid, butyl hydroxy anisole, dibutyl hydroxy toluene, tert-butyl hydroquinone, vitamin E, ascorbic acid and ascorbyl palmitate. The invention provides a plurality of antioxidant choices which can meet the basic requirements of the invention.
Preferably, the antioxidant in the step A) is a mixed antioxidant prepared by mixing tea polyphenol, butyl hydroxy anisole, vitamin E and ascorbyl palmitate according to the mass ratio of 10: 5 ~ 7.6.6: 3 ~ 4.6.6: 1 ~ 2.3.3.
Preferably, the vegetable oil in step a) is one or a mixture of more than two of sunflower oil, peanut oil, soybean oil, linseed oil, castor oil, rapeseed oil, corn oil and safflower oil. The invention provides various vegetable oil choices, which can meet the basic requirements of the invention.
The preparation method of the zeaxanthin nanosuspension is characterized by comprising the following steps of:
A) mixing emulsifier, antioxidant and vegetable oil, heating to 35 deg.C of ~ 70 deg.C, stirring thoroughly;
B) micronizing zeaxanthin, and adding the zeaxanthin into the vegetable oil mixed solution obtained in the step A);
C) passing the liquid prepared in the step B) through a high-shear emulsifying machine to obtain a coarse nano suspension;
D) and (3) passing the coarse nano suspension through high-energy emulsification equipment, reducing the particle size to a nano level, and preparing the zeaxanthin nano suspension.
The invention provides a preparation method of zeaxanthin nanosuspension, which comprises the steps of mixing an emulsifier, an antioxidant and vegetable oil, heating, fully stirring and uniformly mixing; micronizing zeaxanthin crystals, and adding into vegetable oil mixed solution; and (3) passing the liquid through a high-shear emulsifying machine, passing the coarse nano suspension through high-energy emulsifying equipment, and reducing the particle size to a nanometer level to prepare the zeaxanthin nano suspension. The method is simple, easy to operate and suitable for large-scale production, and the prepared zeaxanthin nano-suspension has good stability, is not layered and separated from oil, has a particle size reaching the nanometer level, and improves the bioavailability of zeaxanthin.
Preferably, the high-energy emulsification device in the step D) is a high-pressure homogenizer, a micro-jet ultra-high pressure homogenizer or an ultrasonic disperser. The formula and the method have good adaptability to equipment, and the optimized high-energy emulsifying equipment can meet the process requirements.
Preferably, the zeaxanthin content of the zeaxanthin nanosuspension in step D) is 5% ~ 25%.
The invention provides a preparation method of a zeaxanthin nano suspension. The crushed zeaxanthin powder and the vegetable oil are mixed according to a certain proportion to prepare the oil-soluble zeaxanthin nano-suspension with the particle size reaching the nano level, so that the stability of the zeaxanthin is improved on one hand, and the bioavailability of the zeaxanthin is improved on the other hand.
Compared with the prior art, the preparation method of the zeaxanthin nanosuspension has the beneficial effects that: the zeaxanthin average particle size reaches the nanometer level after the coarse nano suspension is processed by high-energy emulsification equipment, and the zeaxanthin oil suspension is uniform in state, good in physical stability and free of layering after being stored for six months in a standing way at room temperature. The particle size of the prepared nano suspension reaches the nano level, so that the nano suspension is more beneficial to the absorption and utilization of a human body, and the bioavailability of the zeaxanthin is improved. The zeaxanthin is uniformly dispersed in the vegetable oil, the oil solubility is good, the application range of the zeaxanthin is widened, and the zeaxanthin can be used in foods, medicines and health products, including products such as cream, edible oil, sandwich, salad sauce and the like, and can also be used for preparing core materials of soft capsules. The method has the advantages of short time consumption, simple operation and stable product quality, and is suitable for large-scale industrial production.
Detailed Description
The present invention is further illustrated by the following specific examples, of which example 1 is the most preferred.
Example 1
To prepare the zeaxanthin nanosuspension, the following steps were followed:
A) heating 70kg of sunflower seed oil to 50 ℃, adding 2.5kg of antioxidant and 3.8kg of emulsifier, and fully and uniformly stirring to obtain a vegetable oil mixed solution; antioxidant tea polyphenol, butyl hydroxy anisole, vitamin E and ascorbyl palmitate according to the mass ratio of 10: 6.2: 3.9: 1.8 preparing mixed antioxidant; the emulsifier is lecithin and span according to a mass ratio of 7.8: 1, preparing a mixed emulsifier;
B) pulverizing zeaxanthin crystals 71.5% de zeaxanthin to more than 30 meshes by using a universal pulverizer, adding 20kg of the zeaxanthin crystals into the vegetable oil mixed solution, and fully stirring and uniformly mixing;
C) homogenizing the mixed solution with a high-shear homogenizer at 10000rpm for 30min at 60 deg.C to obtain coarse nanosuspension;
D) the crude nanosuspension is treated by a high-pressure homogenizer under the pressure of 90Mpa, the content of the prepared 68kg zeaxanthin nanosuspension is 10.5 percent, the average particle size is 146nm, the maximum particle size is 153nm, the physical stability is good, and the zeaxanthin oil suspension is uniform in state and has no layering after standing and storing at room temperature for sixteen months.
Example 2
To prepare the zeaxanthin nanosuspension, the following steps were followed:
A) heating 65kg of soybean oil to 60 ℃, adding 3.7kg of antioxidant and 3.2kg of emulsifier, and fully and uniformly stirring to obtain a vegetable oil mixed solution; antioxidant tea polyphenol, butyl hydroxy anisole, vitamin E and ascorbyl palmitate according to the mass ratio of 10: 5: 4.6: 1, preparing a mixed antioxidant; the emulsifier is lecithin and span according to the mass ratio of 7: 1, preparing a mixed emulsifier;
B) pulverizing zeaxanthin with a content of 75% of zeaxanthin crystals to above 40 mesh with a universal pulverizer, adding 18kg of zeaxanthin crystals into the vegetable oil mixture, and stirring thoroughly;
C) homogenizing the mixed solution with high-shear homogenizer at 13000rpm for 5min at 60 deg.C to obtain coarse nanometer suspension;
D) the crude nanosuspension is treated by a high-pressure homogenizer under the pressure of 50Mpa, the content of the prepared 47kg zeaxanthin nanosuspension is 15.7 percent, the average particle size is 152nm, the maximum particle size is 175nm, the physical stability is good, and the zeaxanthin oil suspension is uniform in state and has no layering after standing and storing at room temperature for thirteen months.
Example 3
To prepare the zeaxanthin nanosuspension, the following steps were followed:
A) heating 75kg of soybean oil to 65 ℃, adding 2.3kg of antioxidant and 4.2kg of emulsifier, and fully and uniformly stirring to obtain a vegetable oil mixed solution; antioxidant tea polyphenol, butyl hydroxy anisole, vitamin E and ascorbyl palmitate according to the mass ratio of 10: 7.6: 3: 2.3 preparing mixed antioxidant; the emulsifier is lecithin and span according to a mass ratio of 9.6: 1, preparing a mixed emulsifier;
B) pulverizing zeaxanthin crystal 62.4% of zeaxanthin with universal pulverizer to more than 30 mesh, adding 22kg into the above vegetable oil mixture, stirring thoroughly and mixing;
C) homogenizing the mixed solution with a high-shear homogenizer at 9000rpm for 30min at 60 deg.C to obtain coarse nanosuspension;
D) carrying out ultrasonic treatment on the coarse nano suspension in an ultrasonic dispersion instrument, wherein the power is 300W, and the ratio of the working time to the intermittent time is 10 seconds: and 10 seconds, wherein the content of the prepared 120kg zeaxanthin nano suspension is 25%, the average particle size is 157nm, the maximum particle size is 168nm, and the zeaxanthin oil suspension is uniform in state, good in physical stability and free of layering after standing and storing at room temperature for thirteen months.
Example 4
To prepare the zeaxanthin nanosuspension, the following steps were followed:
A) heating 65kg of soybean oil to 50 ℃, adding 3.7kg of mixed tocopherol and 3.2kg of lecithin, and fully and uniformly stirring to obtain a vegetable oil mixed solution;
B) pulverizing zeaxanthin crystal 62.4% of zeaxanthin with universal pulverizer to more than 30 mesh, adding 17kg into the above vegetable oil mixture, stirring thoroughly and mixing;
C) homogenizing the mixed solution with a high-shear homogenizer at 9000rpm for 30min at 60 deg.C to obtain coarse nanosuspension;
D) carrying out ultrasonic treatment on the coarse nano suspension in an ultrasonic dispersion instrument, wherein the power is 300W, and the ratio of the working time to the intermittent time is 10 seconds: the content of the prepared 120kg zeaxanthin nano suspension is 15.2 percent in 10 seconds, the average particle size is 197nm, the maximum particle size is 230nm, the physical stability is good, and the phenomenon of oil separation and layering are started after standing for ten months.
Example 5
To prepare the zeaxanthin nanosuspension, the following steps were followed:
A) heating 50kg of corn oil to 35 ℃, adding 0.1kg of mixed tocopherol and 6.0kg of lecithin, and fully and uniformly stirring to obtain a vegetable oil mixed solution;
B) pulverizing zeaxanthin with crystal content of 60% of zeaxanthin with universal pulverizer to more than 30 mesh, adding 6kg into the above vegetable oil mixture, stirring thoroughly and mixing;
C) homogenizing the mixed solution with a high-shear homogenizer at 9000rpm for 30min at 60 deg.C to obtain coarse nanosuspension;
D) carrying out ultrasonic treatment on the coarse nano suspension in an ultrasonic dispersion instrument, wherein the power is 300W, and the ratio of the working time to the intermittent time is 10 seconds: and the content of the prepared 120kg zeaxanthin nano suspension is 5.0 percent in 10 seconds, the average particle size is 230nm, the maximum particle size is 275nm, the physical stability is good, and the phenomenon of oil separation and layering starts after standing for six months.
Example 6
To prepare the zeaxanthin nanosuspension, the following steps were followed:
A) heating 90kg of corn oil to 70 ℃, adding 5.0kg of butylated hydroxyanisole and 0.1kg of monoglyceride, and fully and uniformly stirring to obtain a vegetable oil mixed solution;
B) pulverizing zeaxanthin 80% of zeaxanthin crystals to more than 30 meshes by using a universal pulverizer, adding 40kg of zeaxanthin crystals into the vegetable oil mixed solution, and fully stirring and uniformly mixing;
C) homogenizing the mixed solution with a high-shear homogenizer at 9000rpm for 30min at 60 deg.C to obtain coarse nanosuspension;
D) carrying out ultrasonic treatment on the coarse nano suspension in an ultrasonic dispersion instrument, wherein the power is 300W, and the ratio of the working time to the intermittent time is 10 seconds: 10 seconds, the content of the prepared 120kg zeaxanthin nano suspension is 18.6 percent, the average particle size is 226nm, the maximum particle size is 282nm, the physical stability is good, and the phenomenon of oil separation and layering starts after standing for five months.
Comparative example 1
To prepare the zeaxanthin nanosuspension, the following steps were followed:
A) heating 70kg sunflower seed oil to 50 deg.C, directly adding 2.5kg antioxidant, 3.8kg emulsifier, and 20kg 71.5% zeaxanthin crystal of 30 mesh above, and stirring;
B) homogenizing the mixed solution with a high-shear homogenizer at 10000rpm for 30min at 60 deg.C to obtain coarse nanosuspension;
C) the crude nanosuspension is treated by a high-pressure homogenizer under the pressure of 90Mpa, the content of the prepared 68kg zeaxanthin nanosuspension is 10.5 percent, the average particle size is 146nm, the maximum particle size is 153nm, the physical stability is good, and layering appears after standing and storing for two months at room temperature.
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.

Claims (5)

1. A zeaxanthin nano suspension is characterized by comprising, by weight, 50 ~ 90 parts of vegetable oil, 0.1 ~ 5.0.0 part of an antioxidant, 0.1 ~ 6.0.0 part of an emulsifier, and 6 ~ 40 parts of zeaxanthin with the zeaxanthin crystal content of 60% ~ 80% and 80%;
the emulsifier is a mixed emulsifier prepared from lecithin and span according to the mass ratio of 7 ~ 9.6.6: 1, and the antioxidant is a mixed antioxidant prepared from tea polyphenol, butyl hydroxy anisole, vitamin E and ascorbyl palmitate according to the mass ratio of 10: 5 ~ 7.6.6: 3 ~ 4.6.6: 1 ~ 2.3.3;
the preparation method comprises the following steps:
A) mixing emulsifier, antioxidant and vegetable oil, heating to 35 deg.C of ~ 70 deg.C, stirring thoroughly;
B) micronizing zeaxanthin, and adding the zeaxanthin into the vegetable oil mixed solution obtained in the step A);
C) passing the liquid prepared in the step B) through a high-shear emulsifying machine to obtain a coarse nano suspension;
D) and (3) passing the coarse nano suspension through high-energy emulsification equipment, reducing the particle size to a nano level, and preparing the zeaxanthin nano suspension.
2. The zeaxanthin nanosuspension of claim 1, which comprises, by weight, 65 ~ 75 parts of vegetable oil, 2.3 ~ 3.7.7 parts of antioxidant, 3.2 ~ 4.2.2 parts of emulsifier, and 18 ~ 22 parts of zeaxanthin with a zeaxanthin crystal content of 60% ~ 80% and 80% respectively.
3. A zeaxanthin nanosuspension according to claim 1 or 2, wherein: the vegetable oil is one or more of sunflower seed oil, peanut oil, soybean oil, linseed oil, castor oil, rapeseed oil, corn oil and safflower oil.
4. A process for the preparation of a zeaxanthin nanosuspension according to any one of claims 1 ~ 3, comprising the steps of:
A) mixing emulsifier, antioxidant and vegetable oil, heating to 35 deg.C of ~ 70 deg.C, stirring thoroughly;
B) micronizing zeaxanthin, and adding the zeaxanthin into the vegetable oil mixed solution obtained in the step A);
C) passing the liquid prepared in the step B) through a high-shear emulsifying machine to obtain a coarse nano suspension;
D) and (3) passing the coarse nano suspension through high-energy emulsification equipment, reducing the particle size to a nano level, and preparing the zeaxanthin nano suspension.
5. The method of preparing a zeaxanthin nanosuspension of claim 4, wherein: the high-energy emulsification equipment in the step D) is a high-pressure homogenizer or an ultrasonic dispersion instrument.
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