CN106617085A - Preparation method of ulva fasciata polysaccharide-tween 20 compounded beta-carotene emulsion - Google Patents

Preparation method of ulva fasciata polysaccharide-tween 20 compounded beta-carotene emulsion Download PDF

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CN106617085A
CN106617085A CN201611086778.4A CN201611086778A CN106617085A CN 106617085 A CN106617085 A CN 106617085A CN 201611086778 A CN201611086778 A CN 201611086778A CN 106617085 A CN106617085 A CN 106617085A
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beta carotene
sea lettuce
emulsion
polysaccharide
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CN106617085B (en
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邵平
邱镪
朱岳琼
孙培龙
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Zhejiang University of Technology ZJUT
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/10Dispersions; Emulsions
    • A61K9/107Emulsions ; Emulsion preconcentrates; Micelles
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00Medicinal preparations containing organic active ingredients
    • A61K31/01Hydrocarbons
    • A61K31/015Hydrocarbons carbocyclic
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/06Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
    • A61K47/26Carbohydrates, e.g. sugar alcohols, amino sugars, nucleic acids, mono-, di- or oligo-saccharides; Derivatives thereof, e.g. polysorbates, sorbitan fatty acid esters or glycyrrhizin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/30Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
    • A61K47/36Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

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Abstract

The invention discloses a preparation method of an ulva fasciata polysaccharide-tween 20 compounded beta-carotene emulsion. The method comprises steps as follows: (1) ulva fasciata polysaccharide and tween 20 are dispersed in water in the mass ratio being 3: 2, and an ulva fasciata polysaccharide-tween 20 compounded solution with the mass concentration of 3%-4%, namely, an aqueous phase, is obtained; (2) an oil phase is obtained by dissolving beta-carotene in edible vegetable oil, the mass percentage of beta-carotene is 0.3%-0.5%, and the temperature is kept at 60 DEG C or below in the dissolution process; (3) the oil phase obtained in step (2) and the aqueous phase obtained in step (1) are mixed in the mass ratio being 1: (10-20) for shear emulsification, high-pressure homogenization is performed in an ice-water bath, and the beta-carotene emulsion is obtained. The method is convenient to operate, the cost is low, and the beta-carotene emulsion prepared with the method has high bioavailability, good stability and high biosafety.

Description

A kind of sliver sea lettuce polysaccharide-polysorbas20 compounds the preparation method of beta carotene emulsion
(1) technical field
The present invention relates to medicine, food, health food processed and applied technical field, it is related to a kind of sliver sea lettuce polysaccharide-tell Temperature 20 compounds the preparation method of beta carotene emulsion.
(2) background technology
With economic continuous development and the raising of human living standard, the mankind are to healthy concern also more and more higher, phase Hope by simpler mode get it is more it is daily needed for various nutriments, meet the daily demand of human body and right The prevention of disease, functional food arises at the historic moment and obtains huge concern.Beta carotene is used as a kind of natural pigment, anti- Oxidant and efficient vitamin A precursor, can be as a kind of safe additive application in field of food, but β-Hu Luo The dissolubility of Bu Su it is poor, unstable and it is oxidizable the characteristic such as decompose, limit its application in food.To overcome this problem, often Beta carotene is designed in the food transport system such as stable oil-in-water emulsion, and then is dissolved into the food of complexity and produced In product, this is beneficial to the physiologically active for protecting carrotene and improves its absorption rate.
In recent years, food-grade emulsion is widely used in the embedding and transmission of food function composition and nutrient, is a kind of letter Single effectively embedding transportation system emulsion.The method for now food function factor being made into emulsion is a lot, but these methods have Some defects.β-carrot emulsion particle diameter as prepared by patent CN100571684C is little, but it is organic molten to be the use of n-hexane etc. Agent, limits its application in food system;Patent CN1079212C, by carotenoid and the aqueous suspension of protective colloid Liquid is heated to 180 DEG C -250 DEG C and makes carotenoid fusing, then obtains emulsion by high-pressure homogeneous, and beta carotene high temperature Easily decompose extremely unstable, the loss of beta carotene can be caused.
Emulsifying agent is that emulsion is rely stable key, and conventional emulsifying agent has protein, polysaccharide, surfactant etc..Tell 20 (TW20) of temperature are nonionic surfactants, as emulsifying agent high concentration electrolyte and pH value change to its emulsifying capacity shadow Very little is rung, is the excellent oil/water type emulsifying agent of a big class.Contribute to the formation of emulsion, emulsion as emulsifying agent by the use of polysorbas20 Particle diameter is little, but the interfacial film mechanical strength that dispersed phase drop surface is formed is low, and anti-droplet coalescence ability stores cycle is short.And Polysaccharide can improve the rheological behavior of emulsion continuous phase, or form spacial framework, prevent what phase separation and gravity caused Creaming.Sliver sea lettuce is extremely rich in natural resources in China's seaweeds, and sliver sea lettuce polysaccharide is polymeric acidic polysaccharide, Solubility is high, with good heat endurance and absolute acid stability, possesses preferable emulsifying property.And it is low with Arabic gum high concentration Unlike viscometric properties, sliver sea lettuce polysaccharide solution just has very high viscosity in low concentration, can weaken between oil droplet molecule The mechanical performance of emulsion is improve after the auto-polymerization caused due to molecular brownian motion, with polysorbas20 compounding.But sliver stone Under intermediate concentration consumption, the effect (promoting breast analysis) of drop flocculation increase particle effective volume is more than raising continuous phase for water shield polysaccharide The effect (suppressing breast analysis) of viscosity, so as to cause system breast analysis unstable.Therefore preparation method of the present invention selects sliver Sea lettuce polysaccharide, as emulsifying agent, is obtained good emulsifying effectiveness with polysorbas20 compound.
(3) content of the invention
It is an object of the invention to provide one kind prepares O/W types with sliver sea lettuce polysaccharide and polysorbas20 compound as emulsifying agent The method of beta carotene emulsion, the method is easy to operate, low cost, and the beta carotene emulsion biology prepared using the method Utilization rate height, good stability, biological safety are high.
For achieving the above object, the technical solution used in the present invention is:
A kind of sliver sea lettuce polysaccharide-polysorbas20 compounds the preparation method of beta carotene emulsion, comprises the steps:
(1) sliver sea lettuce polysaccharide and polysorbas20 are taken according to mass ratio 3:2 are dispersed in water, and obtain mass concentration for 3%- 4% sliver sea lettuce polysaccharide-polysorbas20 combination solution, i.e. water phase;
(2) beta carotene is dissolved in edible vegetable oil and obtains oil phase, the weight/mass percentage composition of wherein beta carotene is 0.3-0.5%, maintains the temperature at less than 60 DEG C in course of dissolution, to avoid temperature from producing unfavorable shadow to beta carotene stability Ring;
(3) by water obtained by the step (2) gained oil phase and step (1) according to mass ratio 1:10~20 mixing are cut Cut emulsification, then carry out high-pressure homogeneous, whole homogenizing process is carried out under ice-water bath, prevents Oxidation of Fat and Oils, obtains beta carotene Emulsion.
Further, at least one of the edible vegetable oil in soybean oil, maize germ oil and sunflower oil.
Further, the weight/mass percentage composition of beta carotene is 0.5%.
Further, the speed of emulsification pretreatment is 10000-26000r/min, and preferably 26000r/min, the time is 3- 5min, preferably 3min.
Further, high-pressure homogeneous pressure is 50-75MPa, and preferably 75MPa, cycle-index is 1-3 time, preferably 3 times.
The preferably preparation method of the invention is carried out in accordance with the following steps:
(1) sliver sea lettuce polysaccharide and polysorbas20 are taken according to mass ratio 3:2 are dispersed in water, and obtain mass concentration for 3%- 4% sliver sea lettuce polysaccharide-polysorbas20 combination solution, i.e. water phase;
(2) beta carotene is dissolved in edible vegetable oil and obtains oil phase, the weight/mass percentage composition of wherein beta carotene is 0.3-0.5%, maintains the temperature at less than 60 DEG C in course of dissolution;
(3) by water obtained by the step (2) gained oil phase and step (1) according to mass ratio 1:10~20 mixing are cut Cut emulsification, the speed of emulsification pretreatment is 10000-26000r/min, and the time is 3-5min, then carry out it is high-pressure homogeneous, it is high-pressure homogeneous Pressure is 50-75MPa, and cycle-index is 1-3 time, and whole homogenizing process is carried out under ice-water bath, obtains beta carotene breast Liquid.
The beneficial effects are mainly as follows:
(1) it is characteristic of the invention that using sliver sea lettuce polysaccharide-polysorbas20 compound as beta carotene emulsion emulsification Agent, obtained stability of emulsion is high, and (in Fig. 2, sliver sea lettuce polysaccharide-polysorbas20 compounds beta carotene emulsion, after accelerated test Its average grain diameter D [3,2] is 1.38 μm, hence it is evident that less than 2.04 μm of same concentration sliver sea lettuce polysaccharide beta carotene emulsion).This It is because that polysorbas20 molecular structure is compact, sterically hindered effect is little, and the emulsification oxidant layer of densification is easily formed in oil-water interfaces, so as to It is rapid to reduce interfacial tension, promote short grained formation;And sliver sea lettuce polysaccharide is polyhydroxy natural macromolecular, with certain Molecular polarity, can be combined with each other with oil droplets in the form of Van der Waals force, and in droplet surface good hydrophilic colloid is formed Film, prevents the polymerization between oil droplet, so as to increase the emulsifying capacity and stability of system.
(2) laurate in polysorbas20 has the ability of certain dissolving beta carotene so as to reduce external influence effect Really, (in table 1, after 4 DEG C and 25 DEG C are stored 30 days, the beta carotene retention rate of two kinds of emulsions is poor to improve beta carotene retention rate It is not especially big;But after 55 DEG C are stored 30 days, sliver sea lettuce polysaccharide-polysorbas20 compounding beta carotene emulsion beta carotene is protected Rate is stayed to be 72%, and 55%) sliver sea lettuce polysaccharide beta carotene emulsion is only.
(3) in whole technical process of the invention, relatively low temperature is employed, beta carotene in food can be effectively improved Biological utilisation effect (in Fig. 3, sliver sea lettuce polysaccharide-polysorbas20 compounding beta carotene emulsion bioavailability is 48.7%, Sliver sea lettuce polysaccharide beta carotene emulsion is 37.8%, and biological dissolved with the oil phase with the beta carotene of same ratio in emulsion Utilization rate is only 4.44%), to help absorption of the human body to beta carotene, and solve that beta carotene is difficult to be absorbed by the body asks Topic.
(4) the emulsifying agent abundance used in the present invention, biodegradable, security;Emulsion preparation method is simple, behaviour Facilitate, it is adaptable to industrialized production.
(4) illustrate
Fig. 1 is the preparation technology flow chart that the sliver sea lettuce polysaccharide-polysorbas20 of the present invention compounds beta carotene emulsion.
Fig. 2 is the sliver sea lettuce polysaccharide-polysorbas20 compounding beta carotene emulsion and sliver sea lettuce polysaccharide β-Hu Luo of the present invention Bu Su stability of emulsion contrast (60 DEG C are placed 3d, 5d, 7d).
Fig. 3 is the sliver sea lettuce polysaccharide-polysorbas20 compounding beta carotene emulsion and sliver sea lettuce polysaccharide β-Hu Luo of the present invention The beta carotene utilization rate contrast of Bu Su emulsions is (dissolved with right as blank with the oil phase of the beta carotene of same ratio in emulsion According to).
(5) specific embodiment
Below technical scheme is described further with specific embodiment, but protection scope of the present invention is not limited In this:
In the embodiment of the present invention, polysorbas20, soybean oil, beta carotene are purchased from Aladdin (aladdin) Reagent Company; Sliver sea lettuce polysaccharide is picked up by oneself using Hot water extraction, and sliver sea lettuce takes from Wenzhou District of Zhejiang Province Pingyang County southern foot archipelago.
Embodiment 1
(1) sliver sea lettuce Polyose extraction:A certain amount of sliver sea lettuce is cleaned, water is controlled, 60 DEG C of drying in baking oven are placed in, is cut It is broken.Plus 95% ethanol solution submergence degreasing, stand overnight.Sliver sea lettuce after degreasing is taken out and is dried, by 1:10 solid-liquid ratios add Enter distilled water, 95 DEG C of water-bath 3h repeat to extract 3 times.Hot water is extracted and terminates rear cooling and standings, refrigerated centrifuge.Take supernatant rotation It is concentrated by evaporation to certain volume.Add 95% ethanol solution to be 80% to final volume fraction of ethanol, stand overnight, 8000r/ Min low-temperature centrifugations, take precipitation, add a small amount of distillation water dissolves, and rotary evaporation will remain alcohol evaporating completely, and be concentrated into certain Volume, with the de- albumen of Sevage methods, repeats 5 times, and rotary evaporation is to organic reagent evaporating completely.Freeze-drying obtains sliver stone Water shield polysaccharide.
(2) prepared by beta carotene emulsion:Configuration sliver sea lettuce polysaccharide-polysorbas20 composite emulsifier, concentration is 3%, takes and splits Piece sea lettuce polysaccharide and polysorbas20 are according to mass ratio 3:2 are dispersed in water, and stir 20min, stand 4h, obtain water phase;Again by β-Hu Radish element is dissolved in soybean oil and obtains oil phase, and concentration is 0.5%.Under the stirring of high-speed shearing machine, according to oil phase and water phase quality For 1:20 ratio, is slowly added to oil phase in water phase, 26000r/min shearing 3min, forms coarse emulsion.Coarse emulsion By the further homogeneous of high pressure homogenizer 75MPa, circulate 3 times, obtain sliver sea lettuce polysaccharide-polysorbas20 compounding beta carotene breast Liquid.
Embodiment 2
(1) sliver sea lettuce Polyose extraction:A certain amount of sliver sea lettuce is cleaned, water is controlled, 60 DEG C of drying in baking oven are placed in, is cut It is broken.Plus 95% ethanol solution submergence degreasing, stand overnight.Sliver sea lettuce after degreasing is taken out and is dried, by 1:10 solid-liquid ratios add Enter distilled water, 95 DEG C of water-bath 3h repeat to extract 3 times.Hot water is extracted and terminates rear cooling and standings, refrigerated centrifuge.Take supernatant rotation It is concentrated by evaporation to certain volume.Add 95% ethanol solution to be 80% to final volume fraction of ethanol, stand overnight, 8000r/ Min low-temperature centrifugations, take precipitation, add a small amount of distillation water dissolves, and rotary evaporation will remain alcohol evaporating completely, and be concentrated into certain Volume, with the de- albumen of Sevage methods, repeats 5 times, and rotary evaporation is to organic reagent evaporating completely.Freeze-drying obtains sliver stone Water shield polysaccharide.
(2) prepared by beta carotene emulsion:Configuration sliver sea lettuce polysaccharide-polysorbas20 composite emulsifier, concentration is 4%, takes and splits Piece sea lettuce polysaccharide and polysorbas20 are according to mass ratio 3:2 are dispersed in water, and stir 20min, stand 4h, obtain water phase;Again by β-Hu Radish element is dissolved in soybean oil and obtains oil phase, and concentration is 0.3%.Under the stirring of high-speed shearing machine, according to oil phase and water phase quality For 1:10 ratio, is slowly added to oil phase in water phase, 10000r/min shearing 5min, forms coarse emulsion.Coarse emulsion By the further homogeneous of high pressure homogenizer 50MPa, circulate 3 times, obtain sliver sea lettuce polysaccharide-polysorbas20 compounding beta carotene breast Liquid.
Comparative example 1
Using single sliver sea lettuce polysaccharide as emulsifying agent, emulsifier concentration in water phase is set to be 3%, other preparation processes are same Embodiment 1, obtains sliver sea lettuce polysaccharide beta carotene emulsion.
Comparative example 2
Using single polysorbas20 as emulsifying agent, emulsifier concentration in water phase is set to be 3%, the same embodiment of other preparation processes 1, obtain polysorbas20 beta carotene emulsion.
Performance detection:
Stability of emulsion is determined:By sliver sea lettuce polysaccharide beta carotene emulsion, the polysorbas20 beta carotene of above-mentioned preparation Emulsion and sliver sea lettuce polysaccharide-polysorbas20 compound storage 3d, 5d, 7d at beta carotene emulsion is placed in 60 DEG C and carry out accelerated test, Determine its change of size and store at 4 DEG C, 25 DEG C, 55 DEG C respectively and determine after 30d beta carotene retention rate.As a result see Fig. 2 and Table 1.
Table 1
Beta carotene bioavailability is determined:For above-mentioned emulsion, external gastro-intestinal Fluid digestion is simulated, will be through simulating intestines Sample after digestion 2h is transferred in centrifuge tube, and ultracentrifugation is carried out at 4 DEG C, and centrifugal force is 10000g, and the time is 40min.Sample after centrifugation is generally divided into three layers, and the superiors are the cream layers that indigested oil phase is formed;It is loaded with nutrient Transparent micella layer at middle one layer;It is fine and close insoluble that indigested cholate, protein, starch and free fatty are formed Thing is then by centrifugation to orlop.The content of beta carotene in micella layer is determined, emulsion Jing is calculated by formula 1 and is disappeared Bioavailability after change.In here experiment, adopt dissolved with the oil phase with the beta carotene of same ratio in emulsion as blank Control.As a result Fig. 3 is seen.

Claims (8)

1. a kind of sliver sea lettuce polysaccharide-polysorbas20 compounds the preparation method of beta carotene emulsion, comprises the steps:
(1) sliver sea lettuce polysaccharide and polysorbas20 are taken according to mass ratio 3:2 are dispersed in water, and obtain mass concentration for 3%-4%'s Sliver sea lettuce polysaccharide-polysorbas20 combination solution, i.e. water phase;
(2) beta carotene is dissolved in edible vegetable oil and obtains oil phase, wherein the weight/mass percentage composition of beta carotene is 0.3- 0.5%, less than 60 DEG C are maintained the temperature in course of dissolution;
(3) by water obtained by the step (2) gained oil phase and step (1) according to mass ratio 1:10~20 mixing carry out shearing breast Change, then carry out high-pressure homogeneous, whole homogenizing process is carried out under ice-water bath, obtains beta carotene emulsion.
2. sliver sea lettuce polysaccharide as claimed in claim 1-polysorbas20 compounds the preparation method of beta carotene emulsion, its feature It is:At least one of the edible vegetable oil in soybean oil, maize germ oil and sunflower oil.
3. sliver sea lettuce polysaccharide as claimed in claim 1 or 2-polysorbas20 compounds the preparation method of beta carotene emulsion, and it is special Levy and be:In step (2), the weight/mass percentage composition of beta carotene is 0.5%.
4. sliver sea lettuce polysaccharide as claimed in claim 1 or 2-polysorbas20 compounds the preparation method of beta carotene emulsion, and it is special Levy and be:The speed of emulsification pretreatment is 10000-26000r/min, and the time is 3-5min.
5. sliver sea lettuce polysaccharide as claimed in claim 4-polysorbas20 compounds the preparation method of beta carotene emulsion, its feature It is:The speed of emulsification pretreatment is 26000r/min, and the time is 3min.
6. sliver sea lettuce polysaccharide as claimed in claim 1 or 2-polysorbas20 compounds the preparation method of beta carotene emulsion, and it is special Levy and be:High-pressure homogeneous pressure is 50-75MPa, and cycle-index is 1-3 time.
7. sliver sea lettuce polysaccharide as claimed in claim 6-polysorbas20 compounds the preparation method of beta carotene emulsion, its feature It is:High-pressure homogeneous pressure is 75MPa, and cycle-index is 3 times.
8. sliver sea lettuce polysaccharide as claimed in claim 1 or 2-polysorbas20 compounds the preparation method of beta carotene emulsion, and it is special Levy is that the preparation method is carried out in accordance with the following steps:
(1) sliver sea lettuce polysaccharide and polysorbas20 are taken according to mass ratio 3:2 are dispersed in water, and obtain mass concentration for 3%-4%'s Sliver sea lettuce polysaccharide-polysorbas20 combination solution, i.e. water phase;
(2) beta carotene is dissolved in edible vegetable oil and obtains oil phase, wherein the weight/mass percentage composition of beta carotene is 0.3- 0.5%, less than 60 DEG C are maintained the temperature in course of dissolution;
(3) by water obtained by the step (2) gained oil phase and step (1) according to mass ratio 1:10~20 mixing carry out shearing breast Change, the speed of emulsification pretreatment is 10000-26000r/min, and the time is 3-5min, then carries out high-pressure homogeneous, high-pressure homogeneous pressure For 50-75MPa, cycle-index is 1-3 time, and whole homogenizing process is carried out under ice-water bath, obtains beta carotene emulsion.
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CN108041594A (en) * 2017-11-28 2018-05-18 大连工业大学 The preparation method of Patinopecten yessoensis Male reproduction zymolyte-beta carotene lotion
CN109601994A (en) * 2018-09-06 2019-04-12 大连工业大学 A kind of preparation method of scallop protein isolate-beta carotene lotion
CN111011858A (en) * 2020-01-08 2020-04-17 中国农业科学院农产品加工研究所 Mixed oil emulsion for improving bioavailability of fat-soluble active substances and preparation method thereof
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108041594A (en) * 2017-11-28 2018-05-18 大连工业大学 The preparation method of Patinopecten yessoensis Male reproduction zymolyte-beta carotene lotion
CN109601994A (en) * 2018-09-06 2019-04-12 大连工业大学 A kind of preparation method of scallop protein isolate-beta carotene lotion
CN111011858A (en) * 2020-01-08 2020-04-17 中国农业科学院农产品加工研究所 Mixed oil emulsion for improving bioavailability of fat-soluble active substances and preparation method thereof
WO2022079063A3 (en) * 2020-10-13 2022-05-27 Givaudan Sa Composition

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