CN113243422A - Preparation method of lycopene Pickering nanoemulsion and primary application of lycopene Pickering nanoemulsion in food - Google Patents

Preparation method of lycopene Pickering nanoemulsion and primary application of lycopene Pickering nanoemulsion in food Download PDF

Info

Publication number
CN113243422A
CN113243422A CN202110515895.2A CN202110515895A CN113243422A CN 113243422 A CN113243422 A CN 113243422A CN 202110515895 A CN202110515895 A CN 202110515895A CN 113243422 A CN113243422 A CN 113243422A
Authority
CN
China
Prior art keywords
lycopene
pickering
nanoemulsion
osa
emulsion
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202110515895.2A
Other languages
Chinese (zh)
Inventor
杜先锋
袁增慧
丁双琨
杨海波
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Anhui Agricultural University AHAU
Original Assignee
Anhui Agricultural University AHAU
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Anhui Agricultural University AHAU filed Critical Anhui Agricultural University AHAU
Priority to CN202110515895.2A priority Critical patent/CN113243422A/en
Publication of CN113243422A publication Critical patent/CN113243422A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23CDAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
    • A23C9/00Milk preparations; Milk powder or milk powder preparations
    • A23C9/152Milk preparations; Milk powder or milk powder preparations containing additives
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23CDAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
    • A23C9/00Milk preparations; Milk powder or milk powder preparations
    • A23C9/152Milk preparations; Milk powder or milk powder preparations containing additives
    • A23C9/1526Amino acids; Peptides; Protein hydrolysates; Nucleic acids; Derivatives thereof
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23CDAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
    • A23C9/00Milk preparations; Milk powder or milk powder preparations
    • A23C9/152Milk preparations; Milk powder or milk powder preparations containing additives
    • A23C9/156Flavoured milk preparations ; Addition of fruits, vegetables, sugars, sugar alcohols or sweeteners
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/30Foods or foodstuffs containing additives; Preparation or treatment thereof containing carbohydrate syrups; containing sugars; containing sugar alcohols, e.g. xylitol; containing starch hydrolysates, e.g. dextrin
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L3/00Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3454Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
    • A23L3/3463Organic compounds; Microorganisms; Enzymes
    • A23L3/3562Sugars; Derivatives thereof
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L3/00Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/40Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by drying or kilning; Subsequent reconstitution
    • A23L3/46Spray-drying
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/105Plant extracts, their artificial duplicates or their derivatives
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23PSHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00Shaping or working of foodstuffs characterised by the products
    • A23P10/30Encapsulation of particles, e.g. foodstuff additives
    • 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

Landscapes

  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Health & Medical Sciences (AREA)
  • Nutrition Science (AREA)
  • Molecular Biology (AREA)
  • Mycology (AREA)
  • Botany (AREA)
  • Biochemistry (AREA)
  • Proteomics, Peptides & Aminoacids (AREA)
  • Microbiology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)
  • Medicinal Preparation (AREA)

Abstract

The invention discloses a preparation method of lycopene Pickering nano-emulsion and primary application in food, wherein OSA (octenyl succinic anhydride) modified OSA-glutinous rice starch is dissolved in water to form a water phase, the water phase is mixed with an oil phase formed by soybean oil dissolved with lycopene to form stable lycopene nano-emulsion after high-speed shearing and high-pressure homogenization, then the nano-emulsion is spray-dried to form OSA-lycopene powder, and the OSA-lycopene powder is added into soft sweets to realize the primary application. The method has simple process and convenient operation. And the storage stability of the lycopene is greatly improved, and the water-insoluble characteristic of the lycopene is improved, so that the lycopene can be better applied to food production.

Description

Preparation method of lycopene Pickering nanoemulsion and primary application of lycopene Pickering nanoemulsion in food
Technical Field
The invention relates to the technical field related to food processing, in particular to a preparation method of lycopene Pickering nano-emulsion and a primary application of the lycopene Pickering nano-emulsion in food.
Background
Lycopene (lycopene) is one of carotenoids, has a dark red crystal appearance, is widely distributed in various mature fruits and vegetables, has wide biological activity, can effectively prevent diseases, prevent and treat cancers and resist aging, and is recognized as a type A nutrient by the Food and Agriculture Organization (FAO), the World Health Organization (WHO) and the joint food additive expert Committee (JECFA) of the United nations. Lycopene can be used as nutritional supplement and colorant. The structure schematic diagram is as follows:
Figure BDA0003062064030000011
lycopene has molecular formula of C40H56Has a molecular weight of 536.85, and is a carotenoid with simple structure (vogel A C. effective environmental factors upper the color soft and of water carotenoid [ J ]]Plant Physiology,1937,12(4): 929-. Because the molecule contains 11 conjugated carbon-carbon double bonds, the lycopene is red, but at the same time, the 11 conjugated and 2 non-conjugated carbon-carbon double bonds make the lycopene extremely unstable in property, and is easy to be oxidized under the action of light, oxygen, high temperature, acid, metal ions and catalysts (Rodriguez-Amaya D B.A guide to carotenoid analysis in foods [ M)]Washington, D.C. International Life Sciences Institute, 1999.1-45.). Lycopene is present in most food materials in a thermostable trans structure, but undergoes conformational changes during processing.
Lycopene, as a natural functional substance, has wide biological activity and wide development prospect. In recent years, research reports continuously discover and confirm that lycopene has various efficacies of preventing and treating cancers, preventing and treating cardiovascular diseases, enhancing immunocompetence and the like, and the development of the carotenoid product becomes a hot spot of international functional food research.
But the properties of lycopene largely limit its utility (Chen J, Shi J, Xues J, et.. Comparison of lycopen stability in and of doilba and of food model system and of pigment and pigment treatment [ J]LWT-Food Science and Technology,2009,42(3): 740-. Lycopene has long aliphatic hydrocarbon chain to make it easily soluble in lipid and insoluble in water, and has structure with beta-ionone ring lacking to make it not have VAThe original activity. In addition, the existence of a plurality of unsaturated double bonds in the molecule directly causes the lycopene to be easily subjected to oxidative decomposition and cis-trans isomerization under the action of illumination, temperature, oxygen, pH value, metal ions and catalysts. Among them, water insolubility and instability are two of the most important factors, and a great deal of stabilization studies have been conducted on these problems, and the types of lycopene products that have been produced are nanocapsules, liposomes, tablets, microemulsions, and the like (Choudhuri S, Bajaj I, Singhal R, et al]Journal of food processing Engineering,2012,35(1): 91-103). The microcapsule is prepared by embedding lycopene with different wall materials, so that the microcapsule has good stability and water solubility. Linn (Complex coacervation method for preparing lycopene nanocapsule [ D)]Jiangnan university 2014.) the lycopene nanoparticles are prepared by using gelatin and Arabic gum as composite wall materials and using a complex coacervation method, and the retention rate can reach 80 percent after being stored for 25 days.
Pickering emulsion refers to an emulsion system stabilized by colloidal particles instead of traditional emulsifiers. Compared with the traditional emulsion, the Pickering emulsion has the advantages of less emulsifier dosage, low cost, less toxic and side effects on human bodies and less related environmental problems; the emulsion has good stability and is not easily influenced by environmental factors such as pH, salt ions, temperature and the like of receptor systems.
In addition, the natural starch is poor in hydrophilicity, OSA modified starch molecules have double characteristics by adding hydrophobic alkenyl and hydrophilic carboxylic acid groups, in emulsion particles, hydrophobic octenyl long chains extend into a hydrophobic region, hydrophilic carboxylic acid groups extend to a continuous phase, and a plurality of polysaccharide long chains are spread on a diffusion layer to form an interface film with compact structure and high viscoelasticity. The interface film structure of the layer has good space barrier effect, and the collision rate and frequency between particles are effectively reduced (Zhuwei red, xu Shi Ying, Jiangfu. the interface property and the emulsification stability of the microcapsule wall material octenyl succinic acid esterified starch [ J ] food science, 2006(12): 79-84.). The OSA starch has amphiphilic properties due to grafting of hydrophobic OSA groups, and thus has good film-forming properties and stability as an emulsifier, is widely used in the fields of food, pharmaceuticals, cosmetics, and the like, and exhibits excellent emulsifying properties and embedding properties.
The glutinous rice starch is the starch with the smallest particle size in all natural starches, so that embedding lycopene by the modified glutinous rice starch becomes the basis for constructing nano-scale emulsion in the invention. Furthermore, once the nano-scale carrier has appeared, the functional nutritional ingredients show more excellent functions of absorption, controlled release and targeting in vivo depending on the characteristics of small particles, large surface area, high surface reactivity, strong adsorption capacity, etc. (ChenHD, Weiss JC, Shahidi F. Nanotechnology in nutritional foods [ J ]. Food Technology,2006,60(3): 30.). The article indicates that small-sized nanoparticles can be adsorbed directly to small intestinal epithelial cells to prolong the release time of active substances, or absorbed directly by small intestinal epithelial cells into the human circulation, both of which avoid the diffusional absorption pathway of gel or microparticles, contributing to the increase in the absorption efficiency of bioactive substances (Chen L, Remondetto G E, Subiode M. food-based materials as nuclear delivery systems [ J ]. Trends in food Science & Technology,2006,17(5): 272-.
Therefore, the invention provides a preparation method of the lycopene Pickering nanoemulsion and a primary application of the lycopene Pickering nanoemulsion in food aiming at the problems of the nano-emulsion carrying system and the preservation and use of lycopene.
Disclosure of Invention
The invention aims to provide a preparation method of lycopene Pickering nano-emulsion and primary application in food, wherein modified glutinous rice starch is used as a wall material, nano-emulsion is formed through high-pressure homogenization, and lycopene is added to form nano-microcapsule, so that the speed of oxidative decomposition of lycopene is reduced, and the physiological function of lycopene is kept, thereby solving the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of lycopene Pickering nano-emulsion and primary application in food, wherein the method comprises the following steps;
(1) dissolving OSA (octenyl succinic anhydride) modified OSA-glutinous rice starch in water, stirring thoroughly to form water phase, dissolving lycopene powder in oil phase, mixing water phase and oil phase, and stirring;
(2) stirring the mixed phase for 5 minutes by a high-speed disperser, and homogenizing the mixed primary emulsion by a high-pressure homogenizer after sieving the mixed primary emulsion by a 200-mesh sieve to form a lycopene Pickering emulsion;
(3) spray drying the lycopene Pickering emulsion to prepare lycopene Pickering emulsion powder;
(4) 10g of gelatin is fully soaked, 400ml of water is added, and the mixture is heated to 80 ℃ until the gelatin is completely dissolved. Taking 600g of white granulated sugar and 200g of whole milk powder, adding a proper amount of water, decocting, completely melting to be viscous and threadlike, adding 35g of lycopene Pickering emulsion powder while hot, and rapidly stirring. Pouring into a mould, cooling and solidifying, taking out and demoulding.
Specifically, the invention is realized by the following technical scheme:
1. a preparation method of lycopene Pickering nanoemulsion and a primary application of the lycopene Pickering nanoemulsion in food comprise the following steps:
(1) dissolving OSA (octenyl succinic anhydride) modified OSA-glutinous rice starch in water, stirring thoroughly to form water phase, dissolving lycopene powder in oil phase, mixing water phase with oil tank, and stirring;
(2) stirring the mixed phase for 5 minutes by a high-speed disperser, and homogenizing the mixed primary emulsion by a high-pressure homogenizer after sieving the mixed primary emulsion by a 200-mesh sieve to form a lycopene Pickering emulsion;
(3) spray drying the lycopene Pickering emulsion to prepare lycopene Pickering emulsion powder;
(4) 10g of gelatin is fully soaked, 400ml of water is added, and the mixture is heated to 80 ℃ until the gelatin is completely dissolved. Taking 600g of white granulated sugar and 200g of whole milk powder, adding a proper amount of water, decocting, completely melting to be viscous and threadlike, adding 35g of lycopene Pickering emulsion powder while hot, and rapidly stirring. Pouring into a mould, cooling and solidifying, taking out and demoulding.
2. The OSA-glutinous rice starch in the step (1) is prepared by adding glutinous rice starch into Octenyl Succinic Anhydride (OSA), reacting for 3 hours under alkaline conditions, adding acid to stop the reaction, washing, drying and grinding. The OSA-glutinous rice starch has substitution degree of 2.23 × 10-2
3. In the step (1), the ratio of OSA-glutinous rice starch to water is 1:10, the ratio of lycopene to oil phase is 1:50, and the ratio of water phase to oil phase is 9: 1;
4. the oil phase selected in the step (1) is soybean oil, the lycopene powder is of an analysis control grade, and the purity is not lower than 99%;
5. homogenizing for 3 times at the rotation speed of the high-speed disperser 16000r/min and the pressure of the high-pressure homogenizer 50MPa in the step (2);
6. a process for the preparation of lycopene Pickering nanoemulsion and the preliminary application in food according to claim 1, characterized in that: the particle size of the lycopene Pickering nanoemulsion in the step (1) is 270 +/-33.12 nm;
7. the operation conditions of the spray drying in the step (3) are as follows: the air inlet temperature is 140 ℃, the air outlet temperature is 85 ℃, and the feeding speed is 20 ml/min.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention adopts the starch-based Pickering emulsion to prepare the lycopene, and the starch-based Pickering emulsion has the characteristics of the Pickering emulsion and has the unique advantages of wide starch source, rich resources and low price, and is a renewable resource; secondly, the starch is degradable and has no pollution to the environment; starch is used as a natural macromolecular substance, has good biocompatibility, no anaphylactic reaction to human bodies, is non-toxic and harmless, and can be widely applied to the field of food; compared with a Pickering emulsion system with stable protein and lipid, the starch base can resist the influence of environmental factors such as temperature, pH and ionic strength;
2. according to the invention, the lycopene is embedded by the Pickering emulsion, so that the lycopene has good stability, is easy to store and transport, and can be better applied to production and use;
3. the modified glutinous rice starch is used as a wall material, the starch with the minimum particle size in all natural starches of the glutinous rice starch is homogenized by an ultrahigh pressure nano homogenizer, so that the particle size of emulsion droplets reaches the nano level, and the absorption efficiency of the embedded lycopene bioactive substances is improved.
4. The lycopene nanopowder is prepared by spray drying process, the dissolution property of the nanopowder is not affected in the spray drying process, and the DPPH free radical quenching capability of the lycopene is improved to a certain extent after the lycopene is subjected to embedding and spraying treatment. The storage and transportation stability of the emulsion is far higher than that of an emulsion product.
Drawings
FIG. 1 is an OSA-lycopene SEM image;
FIG. 2 is a graph of OSA-lycopene powder;
FIG. 3 is an infrared spectrum of lycopene powder;
FIG. 4 is an HPLC profile of an OSA-lycopene nanoemulsion;
fig. 5 is a graph showing antioxidant capacity of a fondant containing OSA-lycopene powder.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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.
Referring to fig. 1-5, the present invention provides a technical solution: a preparation method of lycopene Pickering nanoemulsion and a preliminary application of the lycopene Pickering nanoemulsion in food are as follows:
1. dissolving OSA (octenyl succinic anhydride) modified OSA-glutinous rice starch in water, stirring thoroughly to form water phase, dissolving lycopene powder in oil phase, mixing water phase with oil tank, and stirring;
2. stirring the mixed phase for 5 minutes by a high-speed disperser, and homogenizing the mixed primary emulsion by a high-pressure homogenizer after sieving the mixed primary emulsion by a 200-mesh sieve to form lycopene Pickering nanoemulsion;
3. spray drying the lycopene Pickering emulsion to prepare lycopene Pickering emulsion powder;
4. fully soaking 10g of gelatin, adding 400ml of water, heating to 80 ℃ until the gelatin is completely dissolved, taking 600g of white granulated sugar and 200g of whole milk powder, adding a proper amount of water, decocting, completely melting to be viscous and threadlike, adding 35g of lycopene Pickering emulsion powder while hot, and rapidly stirring. Pouring into a mould, cooling and solidifying, taking out and demoulding.
By adopting the scheme, the OSA-glutinous rice starch in the step 1 is prepared by adding glutinous rice starch into Octenyl Succinic Anhydride (OSA), reacting for 3 hours under alkaline conditions, adding acid to stop the reaction, washing, drying and grinding. The OSA-glutinous rice starch has substitution degree of 2.23 × 10-2
Specifically, in the step 1, the ratio of OSA-glutinous rice starch to water is 1:10, the ratio of lycopene to oil phase is 1:50, and the ratio of water phase to oil phase is 9: 1.
Specifically, the oil phase selected in the step 1 is soybean oil, the lycopene powder is of an analysis control grade, and the purity is not lower than 99%.
Specifically, the particle size of the lycopene Pickering nanoemulsion in the step 1 is 270 +/-33.12 nm.
By adopting the scheme, the rotating speed of the high-speed disperser in the step 2 is 16000r/min, the pressure of the high-pressure homogenizer is 50MPa, and the homogenization is carried out for 3 times.
Specifically, the operation conditions of the spray drying in the step 3 are as follows: the air inlet temperature is 140 ℃, the air outlet temperature is 85 ℃, and the feeding speed is 20 ml/min.
Specifically, the materials used in the experiment of step 1 are food grade, wherein lycopene is a food additive. The homogenizer used in the experiment was an AH-BASIC I ultra-high pressure nano homogenizer.
Example 1
The lycopene Pickering emulsion is prepared by adopting the scheme, deionized water is used for diluting original emulsion by 3000 times before all samples are tested by utilizing a nano-particle size and Zeta potential analyzer to determine the particle size and the dispersion coefficient of the emulsion, then a proper amount of solution to be tested is absorbed and added into a quartz cuvette, the temperature is kept for 2-3 min at 25 +/-0.1 ℃, and each sample is tested for three times. As a result, it was found that the particle size of the lycopene Pickering emulsion was 270. + -. 33.12 nm.
Example 2
And (3) determining the content of the lycopene in the nano emulsion by using a high performance liquid chromatography. And (4) drawing a standard curve, namely accurately weighing 2.1mg of lycopene standard, and dissolving pyrogallic acid-dichloromethane solution to a constant volume of 10mL to obtain No. 1 mother liquor. Sucking 10, 50, 100, 500, 1000, 2000 μ L into No. 1 mother liquor, placing into 6 10mL volumetric flasks, adding pyrogallic acid-dichloromethane solution to scale, shaking to obtain standard solution with lycopene mass concentration of 0.2, 1.0, 5.0, 10.0, 20.0, 40.0 μ g/mL. The solution is ready for use. The purity was determined by liquid chromatography normalization before use.
And (3) measuring the content of the lycopene in the emulsion, namely weighing 1.0g of uniform sample, putting the uniform sample into a 25ml brown volumetric flask, adding 0.2g of pyrogallic acid and 5ml of N, N-dimethyl amide, carrying out ultrasonic extraction for 30min, then carrying out constant volume to a scale with the pyrogallic acid-dichloromethane solution, shaking up, filtering with a 0.45um filter membrane, and taking the filtrate to pass through a column. The results were calculated from a standard curve.
Figure BDA0003062064030000081
The loading rate of the lycopene in the emulsion obtained by calculation in the standard curve is 54 percent.
Example 3
As shown in fig. 1, lycopene nanoemulsion powder was prepared by spray drying, and the powder cooled at room temperature was stored in an electric heating constant temperature air blast oven at a temperature of 25 ℃ for drying. The drying temperature is set very low because the water is slowly evaporated to ensure that all samples to be tested have almost the same moisture content and at the same time reduce the influence of water loss on the internal structure of the emulsion. Secondly, fixing the dried powder on an aluminum plate by using conductive adhesive, and ensuring that the section to be observed is upward due to the possible difference between the section to be observed and the natural section. Spraying gold in a vacuum evaporator for 40 seconds. And finally, transferring the powder subjected to metal spraying into an electron microscope bin, and observing the morphology structure of the sample under the mode that the acceleration voltage is 3.0 kilovolt.
The lycopene spray-dried powder has uniform color and dispersity, no caking phenomenon and good spray-drying effect, and the particles can be obviously separated and not stuck together from SEM micrographs. The shape of single powder particles under the microcosmic condition is close to a spherical shape, the surface of the sphere shows high continuous compactness and no obvious cracks or pores, which indicates that the lycopene is well wrapped in the particles, and meanwhile, the phenomenon that partial areas on the spherical surface are sunken can be found, which is a typical phenomenon that powder products prepared by a spray drying process are easy to generate
Example 4
Weighing a proper amount of 1mg of lycopene, OSA modified starch and a lycopene nanoemulsion powder sample, respectively, fully mixing the lycopene, OSA modified starch and lycopene nanoemulsion powder sample with 100mg of potassium bromide, grinding the mixture under the irradiation of an infrared lamp, pouring the ground mixture powder on parchment paper, pouring a pressing die, pressing the mixture powder into a transparent sheet by using a tablet press, taking out the sheet, placing the sheet into a sample chamber of an infrared spectrometer, scanning the sample chamber within the range of 400-4000 cm < -1 >, wherein the spectral resolution is 4cm < -1 >, and when molecules are irradiated by infrared light, different chemical bonds or functional groups in the molecules can vibrate and absorb at a specific frequency to form an infrared absorption spectrogram, so that the information of which chemical bonds or functional groups are contained in the molecules can be obtained. In the experiment, air is used as a blank, and the infrared spectrogram of the sample is obtained after scanning signals are accumulated for 32 times. The OSA modified starch, lycopene powder particles and lycopene crystals were detected separately using infrared spectroscopy, and the substances were mapped by changes in the absorption spectra.
As shown in FIG. 2, all samples were close to 3410cm-1The absorption peak is due in part to the water absorption peak due to the potassium bromide moisture absorption during tableting. OSA modified starch at 1726cm-1There was an absorption peak, which is a stretching vibration peak of carbonyl group, indicating that starch successfully introduced hydrophilic ester group. After the nanoemulsion powder was formed at 1745cm-1An intense absorption peak is formed nearby, here the typical C ═ O stretching vibration, which represents the ester bond in the oil phase in the powder system, indicating that a good bond is formed between the oil phase loaded in the emulsion and the starch molecules, while lycopene crystals are at a wavelength of 959cm-1The characteristic peak of strong trans-form is covered, which shows that the lycopene is completely embedded by the starch molecule emulsion layer and 765cm-1A new absorption peak appears nearby, which indicates that part of lycopene in the nano system is in cis R1HC=CR2The H structure exists, which may be lycopene cis-isomer generation caused by local short-time high-temperature action in the process of dissolution or high-pressure homogenization. Further, the OSA modified starch is good for carrying and embedding lycopene.
Example 5
As shown in fig. 4, the soft candy containing lycopene nano-emulsion powder was prepared by the above method, and the antioxidant ability of the lycopene nano-powder particles was evaluated by using DPPH radical scavenging. The method for consulting the Yangyheng is slightly modified, and the specific process is as follows: the reconstituted milk was prepared as in 1.2.3. Three tubes were taken to define tube A1 as the sample, tube A2 as the reference, and tube A3 as the blank. The reagents were added as in Table 2.2, wherein the groups were water-washed at 25 ℃ for 30min, after which the absorbance was determined at 517nm, respectively, and zeroed with 95% ethanol solution, each sample was repeated 3 times, and the average was taken. The control group was an aqueous solution of lycopene in tetrahydrofuran/dimethylsulfoxide (1/1, v/v).
DPPH radical scavenging ratio (%) - [1- (A)1-A3)÷A2]×100
DPPH free radical scavenging ratio of lycopene powder and OSA-lycopene powder after spray drying is calculated. Under the condition of the same concentration, the quenching capacity of the lycopene Pickering nanoemulsion is slightly larger than that of OSA-lycopene powder, and the quenching capacity of the lycopene in the soft candy is slightly lower than that of the lycopene Pickering nanoemulsion and OSA-lycopene, so that the lycopene is probably slightly influenced by heating in the application process, but good oxidation resistance is still kept. The results show that the nano embedding can improve the chemical antioxidant activity of the lycopene, and the chemical characteristics of the nano emulsion are not greatly influenced in the spray drying process.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (7)

1. A preparation method of lycopene Pickering nanoemulsion and a primary application of the lycopene Pickering nanoemulsion in food are disclosed, wherein the method comprises the following steps:
(1) dissolving OSA (octenyl succinic anhydride) modified OSA-glutinous rice starch in water, stirring thoroughly to form water phase, dissolving lycopene powder in oil phase, mixing water phase with oil tank, and stirring;
(2) stirring the mixed phase for 5 minutes by a high-speed disperser, and homogenizing the mixed primary emulsion by a high-pressure homogenizer after sieving the mixed primary emulsion by a 200-mesh sieve to form lycopene Pickering nanoemulsion;
(3) preparing lycopene Pickering emulsion powder by spray drying the lycopene Pickering nano emulsion;
(4) fully soaking 10g of gelatin, adding 400ml of water, heating to 80 ℃ until the gelatin is completely dissolved, taking 600g of white granulated sugar and 200g of whole milk powder, adding a proper amount of water, decocting, completely melting to be viscous and threadlike, adding 35g of lycopene Pickering emulsion powder while hot, and rapidly stirring. Pouring into a mould, cooling and solidifying, taking out and demoulding.
2. Lycopene Pickerin according to claim 1g nano emulsion preparation method and preliminary application in food, which is characterized in that: the OSA-glutinous rice starch in the step (1) is prepared by adding glutinous rice starch into Octenyl Succinic Anhydride (OSA), reacting for 3 hours under alkaline conditions, adding acid to stop the reaction, washing, drying and grinding. The OSA-glutinous rice starch has substitution degree of 2.23 × 10-2
3. A process for the preparation of lycopene Pickering nanoemulsion and the preliminary application in food according to claim 1, characterized in that: in the step (1), the ratio of OSA-glutinous rice starch to water is 1:10, the ratio of lycopene to oil phase is 1:50, and the ratio of water phase to oil phase is 9: 1.
4. A process for the preparation of lycopene Pickering nanoemulsion and the preliminary application in food according to claim 1, characterized in that: the oil phase selected in the step (1) is soybean oil, the purity of the lycopene powder is an analysis control level, and the purity is not lower than 99%.
5. A process for the preparation of lycopene Pickering nanoemulsion and the preliminary application in food according to claim 1, characterized in that: and (3) homogenizing for 3 times at the rotating speed of the high-speed disperser in the step (2) of 16000r/min and the pressure of the high-pressure homogenizer of 50 MPa.
6. A process for the preparation of lycopene Pickering nanoemulsion and the preliminary application in food according to claim 1, characterized in that: the particle size of the lycopene Pickering nanoemulsion in the step (1) is 270 +/-33.12 nm.
7. A process for the preparation of lycopene Pickering nanoemulsion and the preliminary application in food according to claim 1, characterized in that: the operation conditions of the spray drying in the step (3) are that the air inlet temperature is 140 ℃, the air outlet temperature is 85 ℃, and the feeding speed is 20 ml/min.
CN202110515895.2A 2021-05-12 2021-05-12 Preparation method of lycopene Pickering nanoemulsion and primary application of lycopene Pickering nanoemulsion in food Pending CN113243422A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110515895.2A CN113243422A (en) 2021-05-12 2021-05-12 Preparation method of lycopene Pickering nanoemulsion and primary application of lycopene Pickering nanoemulsion in food

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110515895.2A CN113243422A (en) 2021-05-12 2021-05-12 Preparation method of lycopene Pickering nanoemulsion and primary application of lycopene Pickering nanoemulsion in food

Publications (1)

Publication Number Publication Date
CN113243422A true CN113243422A (en) 2021-08-13

Family

ID=77222926

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110515895.2A Pending CN113243422A (en) 2021-05-12 2021-05-12 Preparation method of lycopene Pickering nanoemulsion and primary application of lycopene Pickering nanoemulsion in food

Country Status (1)

Country Link
CN (1) CN113243422A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115399414A (en) * 2022-03-09 2022-11-29 山东省食品发酵工业研究设计院 Formula and production method of fruit nano-film preservative

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105124096A (en) * 2015-08-27 2015-12-09 颍上县好圆食品有限公司 Anti-radiation nougat
CN109601999A (en) * 2018-11-01 2019-04-12 华南农业大学 A kind of lycopene nanometer powder and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105124096A (en) * 2015-08-27 2015-12-09 颍上县好圆食品有限公司 Anti-radiation nougat
CN109601999A (en) * 2018-11-01 2019-04-12 华南农业大学 A kind of lycopene nanometer powder and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
卞希良: "辛烯基琥珀酸糯米淀粉酯的制备及其性质研究", 《四川农业大学硕士学位论文》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115399414A (en) * 2022-03-09 2022-11-29 山东省食品发酵工业研究设计院 Formula and production method of fruit nano-film preservative
CN115399414B (en) * 2022-03-09 2024-05-17 山东省食品发酵工业研究设计院 Fruit nano-film preservative and production method thereof

Similar Documents

Publication Publication Date Title
Ren et al. Effects of frequency ultrasound on the properties of zein-chitosan complex coacervation for resveratrol encapsulation
WO2021082271A1 (en) Pickering emulsion stabilized with gingko shell cellulose and preparation method therefor
Ćujić et al. Chokeberry (Aronia melanocarpa L.) extract loaded in alginate and alginate/inulin system
Dadkhodazade et al. Yeast cell microcapsules as a novel carrier for cholecalciferol encapsulation: development, characterization and release properties
Desai et al. Effect of manufacturing parameters on the characteristics of vitamin C encapsulated tripolyphosphate-chitosan microspheres prepared by spray-drying
Chen et al. Microencapsulation of Sichuan pepper essential oil in soybean protein isolate-Sichuan pepper seed soluble dietary fiber complex coacervates
CN104758315B (en) A method of fish oil is wrapped up using zeins
CN105876792B (en) A kind of preparation method of novel beta carotene microcapsules
US20230276832A1 (en) Ultrasonic preparation method of protein-derived peptide-polysaccharide nanoparticles loaded with bioactive components
Wardhani et al. The effect of spray-drying inlet conditions on iron encapsulation using hydrolysed glucomannan as a matrix
Niu et al. Rheological aspects in fabricating pullulan-whey protein isolate emulsion suitable for electrospraying: Application in improving β-carotene stability
Raj et al. Microencapsulation of betacyanin from dragon fruit peel by complex coacervation: Physicochemical characteristics, thermal stability, and release profile of microcapsules
CN113243422A (en) Preparation method of lycopene Pickering nanoemulsion and primary application of lycopene Pickering nanoemulsion in food
Zhang et al. Study on the preparation of genipin crosslinked chitosan microspheres of resveratrol and in vitro release
Agarry et al. Chlorophyll encapsulation by complex coacervation and vibration nozzle technology: Characterization and stability study
Chen et al. Quinoa protein isolate-gum Arabic coacervates cross-linked with sodium tripolyphosphate: Characterization, environmental stability, and Sichuan pepper essential oil microencapsulation
Feng et al. Effect of V-type crystallinity and starch particle structure on the oil loading capacity and anti-oxidation
Xiao et al. Evaluation of a novel self-emulsifiable dodecenyl succinylated agarose in microencapsulation of docosahexaenoic acid (DHA) through spray-chilling process
Rezvankhah et al. Investigating the effects of maltodextrin, gum arabic, and whey protein concentrate on the microencapsulation efficiency and oxidation stability of hemp seed oil
Arumugham et al. Spray dried date fruit extract with a maltodextrin/gum arabic binary blend carrier agent system: Process optimization and product quality
Zhang et al. Fabrication of curcumin encapsulated in casein-ethyl cellulose complexes and its antibacterial activity when applied in combination with blue LED irradiation
Rikhtehgaran et al. Casein-based nanodelivery of olive leaf phenolics: Preparation, characterization and release study
Huang et al. Preparation and characterization of astaxanthin‐loaded microcapsules and its application in effervescent tablets
Mishra et al. Applicability of spray drying technique to prepare nano-micro carriers: A review
Ledri et al. Comparative analysis of freeze drying and spray drying methods for encapsulation of chlorophyll with maltodextrin and whey protein isolate

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20210813