CN107348507A - Carry the preparation of bata-carotene PLA (PLA) nanoparticle - Google Patents

Carry the preparation of bata-carotene PLA (PLA) nanoparticle Download PDF

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Publication number
CN107348507A
CN107348507A CN201710558759.5A CN201710558759A CN107348507A CN 107348507 A CN107348507 A CN 107348507A CN 201710558759 A CN201710558759 A CN 201710558759A CN 107348507 A CN107348507 A CN 107348507A
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Prior art keywords
pla
carotene
bata
preparation
nanoparticle
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CN201710558759.5A
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Chinese (zh)
Inventor
潘杰
雷帅权
李具恒
李佩娇
尚如梦
万冬
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Tianjin Polytechnic University
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Tianjin Polytechnic University
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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/105—Plant extracts, their artificial duplicates or their derivatives
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/10—Foods or foodstuffs containing additives; Preparation or treatment thereof containing emulsifiers
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
    • A23L5/20—Removal of unwanted matter, e.g. deodorisation or detoxification
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Nutrition Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Mycology (AREA)
  • Botany (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Cosmetics (AREA)

Abstract

Main process field of paddling of the invention, designs a kind of scheme, is specifically prepared for edibility, the polylactic acid nano particle of the load bata-carotene of biodegradability.This method comprises the following steps：(1) preparation of PLA (PLA)；(2) preparation of emulsifying agent (PVA)；(3) preparation of PLA (PLA) nanoparticle of bata-carotene is carried, finally gives product.The method has low for equipment requirements, and simple to operate, fabrication cycle is short, and edible is nontoxic, there is good biodegradability and biocompatibility.The edible that this method can be prepared carries the polylactic acid nano particle of bata-carotene.

Description

Carry the preparation of beta carotene PLA (PLA) nanoparticle
Technical field
Present invention is mainly applied in order to be prepared for edibility, the PLA of the load beta carotene of biodegradability Nanoparticle.
Background technology
Water is Source of life, and Water resources security and processing have countless ties with Earth Health, energy products and economic development Relation.Since 20th century, public drinking water health, agricultural development etc., water supply system and wastewater processing technology are provided Rapid progress is achieved, concurrently, is improved rapidly with the living standard of our people, by western countries' culture and consumption view The influence of thought, the habits and customs of China town dweller gradually receive the life style of western sciences, and risk of drinking water pollution triggers Drinking water quality problem be increasingly subject to the attention of people, it is general with water quality problem to be that current people solve using household water filter Time selection.And in the material of numerous water treatment applications, representative of the nano material as tip materials, superior performance together, Wide development space, it is especially noticeable.
Currently used drinking water water purification further treatment technique has deep layer contact filtration technology, membrane filtration technique, compound gold Belong to media filtration technology.Wherein membrane filtration technique is a kind of water process skill for starting to put into engineer applied recent years in China Art.It is different according to membrane aperture, micro-filtration, ultrafiltration, reverse osmosis technology can be divided into.According to the material of filter membrane, can be divided into organic filter membrane and Inorganic filter membrane.Membrane technology mainly removes water pollutant, the removal object master of the technology using the Physical entrapment effect of film To depend on the physical dimension of material.Organic film is compared with inoranic membrane, and big with area of passage, disposal ability is big, manufacturing process The advantages of ripe.Inoranic membrane impact resistance is poor, broken, easy blocking, difficult cleaning.So our fluorescence PLA is as new Nanoparticle, can preferably examine membrane aperture, the optimization and improvement of product are reached with this.
With the development of the social economy, the problem of current world's water pollution is increasingly severe, water treatment problems also become to get over Come severeer.The useless of China, quantity of wastewater effluent are very big, account for more than the 10% of the world, and in China, domestic total output value is about Account for the 5.5% of the world.But the wastewater treatment rate of Chinese city only has 36%, most of raw sewerage is all direct Rivers,lakes and seas are discharged into, destroy ecological environment, make environment more severe, so, sewage disposal technology is particularly important.In addition, Drinking water quality problem caused by our risk of drinking water pollution also increasingly receives the attention of people, is mesh using household water filter Preceding people are solved with the universal selection of water quality problem.
Beta carotene is Alphalin, can be converted into vitamin A at any time when somagenic need, helps and maintains eyes to be good for Health.Strengthen body immune system, anti-oxidation protection is provided to heart and other organs, help to maintain the strong of skin and hair Health, oil-soluble pigment is eaten, can be as the tracer of edibility.
PLA [Poly (lactic Acid), PLA] is a kind of high molecular polymer, and molecular formula is (C3H4O2) n, is gathered Lactic acid is formed by lactide ring-opening polymerisation, or direct polycondensation of lactic acid.PLA has good biodegradability And biocompatibility, carbon dioxide and water can be degraded to, intermediate product lactic acid is also internal normal glycometabolism product, will not Assemble in vitals, be all widely used in biomedical, material etc., be preferable Green Polymer Material.
At present, membrane filtration technique all has at many aspects and is extremely widely applied, and its principle and feature can help me Solve problem present in some real lifes.Except applying in terms of water process, nano-film filtration technology is in processing chemical industry Synthesis waste liquid in application can also effectively reclaim can not biodegradable organic matter, concentrate valuable organic matter etc.； Membrane technology mainly removes water pollutant using the Physical entrapment effect of film, and the removal object of the technology depends primarily on thing The physical dimension of matter.
The advantages of by combining beta carotene, PLA and membrane filtration, we are made that edibility, biodegradable Property load beta carotene polylactic acid nano particle.
A kind of polylactic acid nano particle for carrying beta carotene of the present invention, new approaches are being provided with membrane filtration water problems.
The content of the invention
In order to solve problems of the prior art, this invention inventor has carried out research extensively and profoundly, finally The present invention is obtained.
It is an object of the invention to in membrane filtration water problems, being prepared for edibility, the load of biodegradability The polylactic acid nano particle of beta carotene.
The purpose of the present invention is achieved through the following technical solutions.
Step 1, carry bata-carotene PLA (PLA) nanoparticle preparation：
1) balance weighs PLA, and rufous bata-carotene is added in methylene chloride, ultrasound about 5 minutes to completely it is molten Solution, now solution is in crocus, standby；
2) balance weighs emulsifying agent (PVA or TPGS), adds distilled water, is heated with stirring to and is completely dissolved, standby；
3) at room temperature, step 1) is poured slowly into step 2), can visually see that crocus oily drop produces, use Supersonic cell disintegrating machine it is stirred by ultrasonic about 2min, to there is no oil droplet residual, obtained crocus homogeneous latex emulsion are standby With；
4) by emulsion rotary evaporation about 30 minutes obtained by step 3), volatilized completely to solvent, now, solution is changed into somewhat shallow The orange colour of a bit, it is standby；
5) at room temperature, step 4) is centrifuged using centrifuge, makes to be washed with deionized gained and precipitates, washing three times, from Three times, after third time washing centrifugation, centrifuge the clear liquid of gained does not almost have color to the heart, white transparence, illustrates that washing is dry Only, it is standby；
6) obtained precipitation is dissolved in about a little pure water, resulting solution is freeze-dried 2 days, that is, obtains orange powder shape Load bata-carotene PLA nanoparticles；
The method applied in the present invention is the mon-galacta method of improvement, but is not limited to mon-galacta method, can also use multi-emulsion method.
The preparation method of nanoparticle provided by the invention is simple and easy to control, reproducible, and industrially scalable, high efficiency can be achieved Produce the product of steady quality.The stability of nanoparticle can be proven by the measurement result of particle diameter and current potential.Take and carry β recklessly The PLA nanoparticles of radish element are appropriate, observed after natural drying under thermal field ESEM under (SEM), particle diameter is in 100~300nm Between, as shown in Figure 1, Figure 2, Figure 3 shows.
Compared with prior art, innovative point is the nanoparticle of the present invention：Nanoparticle stability is good, and has edibility, The nanoparticle of the load beta carotene of biodegradability.
Brief description of the drawings
Fig. 1 is the grain size distribution for the PLA nanoparticles for carrying bata-carotene；
Fig. 2 is the potential image for the PLA nanoparticles for carrying bata-carotene；
Fig. 3 is the scanning electron microscopic picture for the PLA nanoparticles for carrying bata-carotene；
Fig. 4 is the scattered picture in the distilled water for the PLA nanoparticles for carrying bata-carotene；
Fig. 5 be carry bata-carotene PLA nanoparticles from hollow-fibre membrane filtering after picture；
Fig. 6 is that the PLA nanoparticles for carrying bata-carotene pass through the picture after the filtering of 0.45 micron membrane filter；
Embodiment
With reference to example, the invention will be further described.
Embodiment 1
20mg PLA, 1mg bata-carotenes are weighed, adds 6ml dichloromethane, ultrasound makes material and bata-carotene fully molten Solution, balance weigh emulsifying agent PVA 0.5g, are dissolved in 100ml distilled water, are completely dissolved it, the material configured is poured into In 30ml emulsifying agents, about 2min is stirred by ultrasonic to it using supersonic cell disintegrating machine, crocus homogeneous latex emulsion, rotation is made Turn evaporation emulsion 30min, centrifuged again three times with distillation water washing afterwards, add a little distilled water, 4 DEG C are sealed.
Lyophilized technique：It is degerming with 0.45 μm of filtering with microporous membrane, suspension is obtained after filtering and is fitted into culture dish, is put in refrigerator - 20 DEG C of pre-freeze 2h, -50 DEG C, 48h in freeze drier are then placed in, obtain the PLA nanometers that the loose shape of orange colour carries bata-carotene Grain, the freeze-dried material adds 2mL distilled water can be in being completely dispersed through ultrasound in 1min.
As a result：Be made carry bata-carotene PLA nanoparticles average grain diameter be 340.7 ± 6.1nm average potentials be- 19.5mV
Embodiment 2
20mg PLA, 1mg bata-carotenes are weighed, adds 6ml dichloromethane, ultrasound makes material and bata-carotene fully molten Solution, balance weigh emulsifying agent TPGS 0.5g, are dissolved in 100ml distilled water, are completely dissolved it, the material configured is poured into In 30ml emulsifying agents, about 2min is stirred by ultrasonic to it using supersonic cell disintegrating machine, crocus homogeneous latex emulsion, rotation is made Turn evaporation emulsion 30min, centrifuged again three times with distillation water washing afterwards, add a little distilled water, 4 DEG C are sealed.
Lyophilized technique：It is degerming with 0.45 μm of filtering with microporous membrane, suspension is obtained after filtering and is fitted into culture dish, is put in refrigerator - 20 DEG C of pre-freeze 2h, -50 DEG C, 48h in freeze drier are then placed in, obtain the PLA nanometers that the loose shape of orange colour carries bata-carotene Grain, the freeze-dried material adds 2mL distilled water can be in being completely dispersed through ultrasound in 1min.
As a result：Be made carry bata-carotene PLA nanoparticles average grain diameter be 319.1 ± 4.4nm average potentials be- 36.4mV
Embodiment 3
20mg PLA, 1mg bata-carotenes are weighed, adds 6ml dichloromethane, ultrasound makes material and bata-carotene fully molten Solution, balance weigh emulsifying agent PVA 0.66g, are dissolved in 100ml distilled water, are completely dissolved it, the material configured is poured into In 30ml emulsifying agents, about 2min is stirred by ultrasonic to it using supersonic cell disintegrating machine, crocus homogeneous latex emulsion, rotation is made Turn evaporation emulsion 30min, centrifuged again three times with distillation water washing afterwards, add a little distilled water, 4 DEG C are sealed.
Lyophilized technique：It is degerming with 0.45 μm of filtering with microporous membrane, suspension is obtained after filtering and is fitted into culture dish, is put in refrigerator - 20 DEG C of pre-freeze 2h, -50 DEG C, 48h in freeze drier are then placed in, obtain the PLA nanometers that the loose shape of orange colour carries bata-carotene Grain, the freeze-dried material adds 2mL distilled water can be in being completely dispersed through ultrasound in 1min.
As a result：Be made carry bata-carotene PLA nanoparticles average grain diameter be 211.2 ± 3.4nm average potentials be- 19.8mV
Embodiment 4
20mg PLA, 1mg bata-carotenes are weighed, adds 6ml dichloromethane, ultrasound makes material and bata-carotene fully molten Solution, balance weigh emulsifying agent TPGS 0.66g, are dissolved in 100ml distilled water, are completely dissolved it, the material configured is poured into In 30ml emulsifying agents, about 2min is stirred by ultrasonic to it using supersonic cell disintegrating machine, crocus homogeneous latex emulsion, rotation is made Turn evaporation emulsion 30min, centrifuged again three times with distillation water washing afterwards, add a little distilled water, 4 DEG C are sealed.
Lyophilized technique：It is degerming with 0.45 μm of filtering with microporous membrane, suspension is obtained after filtering and is fitted into culture dish, is put in refrigerator - 20 DEG C of pre-freeze 2h, -50 DEG C, 48h in freeze drier are then placed in, obtain the PLA nanometers that the loose shape of orange colour carries bata-carotene Grain, the freeze-dried material adds 2mL distilled water can be in being completely dispersed through ultrasound in 1min.
As a result：Be made carry bata-carotene PLA nanoparticles average grain diameter be 209.1 ± 2.3nm average potentials be- 39.4mV
Embodiment 5
40mg PLA, 1mg bata-carotenes are weighed, adds 6ml dichloromethane, ultrasound makes material and bata-carotene fully molten Solution, balance weigh emulsifying agent TPGS 0.66g, are dissolved in 100ml distilled water, are completely dissolved it, the material configured is poured into In 30ml emulsifying agents, about 2min is stirred by ultrasonic to it using supersonic cell disintegrating machine, crocus homogeneous latex emulsion, rotation is made Turn evaporation emulsion 30min, centrifuged again three times with distillation water washing afterwards, add a little distilled water, 4 DEG C are sealed.
Lyophilized technique：It is degerming with 0.45 μm of filtering with microporous membrane, suspension is obtained after filtering and is fitted into culture dish, is put in refrigerator - 20 DEG C of pre-freeze 2h, -50 DEG C, 48h in freeze drier are then placed in, obtain the PLA nanometers that the loose shape of orange colour carries bata-carotene Grain, the freeze-dried material adds 2mL distilled water can be in being completely dispersed through ultrasound in 1min.
As a result：Be made carry bata-carotene PLA nanoparticles average grain diameter be 340.5.1 ± 5.3nm average potentials be- 30.1mV
Embodiment 6
40mg PLA, 4mg bata-carotenes are weighed, adds 6ml dichloromethane, ultrasound makes material and bata-carotene fully molten Solution, balance weigh emulsifying agent TPGS 0.66g, are dissolved in 100ml distilled water, are completely dissolved it, the material configured is poured into In 30ml emulsifying agents, about 2min is stirred by ultrasonic to it using supersonic cell disintegrating machine, crocus homogeneous latex emulsion, rotation is made Turn evaporation emulsion 30min, centrifuged again three times with distillation water washing afterwards, add a little distilled water, 4 DEG C are sealed.
Lyophilized technique：It is degerming with 0.45 μm of filtering with microporous membrane, suspension is obtained after filtering and is fitted into culture dish, is put in refrigerator - 20 DEG C of pre-freeze 2h, -50 DEG C, 48h in freeze drier are then placed in, obtain the PLA nanometers that the loose shape of orange colour carries bata-carotene Grain, the freeze-dried material adds 2mL distilled water can be in being completely dispersed through ultrasound in 1min.
As a result：Be made carry bata-carotene PLA nanoparticles average grain diameter be 437.7 ± 6.3nm average potentials be- 27.1mV。

Claims (8)

1. in order to be prepared for edibility, PLA (PLA) nanoparticle of the load beta carotene of biodegradability, Yi Zhongxin The nanoparticle of the edibility of type, comprises the following steps：
Step 1, carry bata-carotene PLA (PLA) nanoparticle preparation：
1) balance weighs PLA, and rufous bata-carotene is added in methylene chloride, ultrasound about 5 minutes to being completely dissolved, this When solution be in crocus, it is standby；
2) balance weighs emulsifying agent (PVA or TPGS), adds distilled water, is heated with stirring to and is completely dissolved, standby；
3) at room temperature, step 1) is poured slowly into step 2), can visually see that crocus oily drop produces, use ultrasound Ripple cell disintegrating machine it is stirred by ultrasonic about 2min, to there is no oil droplet residual, obtained crocus homogeneous latex emulsion are standby；
4) by emulsion rotary evaporation about 30 minutes obtained by step 3), volatilized completely to solvent, now, solution is changed into somewhat more shallow Orange colour, it is standby；
5) at room temperature, step 4) is centrifuged using centrifuge, makes gained precipitation is washed with deionized, washing three times, centrifuges three Secondary, after third time washing centrifugation, the clear liquid for centrifuging gained does not almost have color, white transparence, illustrates washes clean, standby With；
6) obtained precipitation is dissolved in about a little pure water, resulting solution is freeze-dried 2 days, that is, obtains the load of orange powder shape The PLA nanoparticles of bata-carotene；
Step 2, carry bata-carotene PLA (PLA) nanoparticle sign：
PLA (PLA) nanoparticle for carrying bata-carotene is examined using nano particle size, Zeta potential, SEM Survey：Characterize the size of granularity according to nano particle size, Zeta potential surveys its stability, and SEM makes us can be with Intuitively observe the initial size and pattern of nanoparticle.
2. preparation method according to claim 1, it is characterised in that：What is contained is edibility, biodegradability β- Carrotene.
3. preparation method according to claim 1, it is characterised in that：Emulsifying agent includes TPGS and PVA, with the breast that must be obtained Agent mass percentage concentration is 0.33%, 0.5%, 0.66%, and preferred emulsifier is that TPGS mass percentage concentrations are 0.66%.
4. preparation method according to claim 1, it is characterised in that：Described PLA (PLA) and bata-carotene mixing Its mass ratio of thing is 20: 1.
5. preparation method according to claim 1, it is characterised in that：The PLA (PLA) of described load bata-carotene is received In the preparation of the grain of rice, suitable ultrasound condition is 70W-80W.
6. preparation method according to claim 1, it is characterised in that：Product after centrifugation is washed with deionized 3 It is secondary, remove unreacted material.
7. preparation method according to claim 1, it is characterised in that：The PLA for the load bata-carotene being prepared (PLA) nanoparticle.
8. preparation method according to claim 1, it is characterised in that：The PLA for the load bata-carotene being prepared (PLA) nano-granule freeze-dried powder end.
CN201710558759.5A 2017-07-06 2017-07-06 Carry the preparation of bata-carotene PLA (PLA) nanoparticle Pending CN107348507A (en)

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Publication number Priority date Publication date Assignee Title
CN109381447A (en) * 2018-12-10 2019-02-26 上海交通大学医学院附属第九人民医院 A kind of load astaxanthin phosphatide nanoparticle and the preparation method and application thereof
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Application publication date: 20171117