CN109222179B - Preparation method of curcumin nano-microcapsule - Google Patents

Preparation method of curcumin nano-microcapsule Download PDF

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CN109222179B
CN109222179B CN201810867543.1A CN201810867543A CN109222179B CN 109222179 B CN109222179 B CN 109222179B CN 201810867543 A CN201810867543 A CN 201810867543A CN 109222179 B CN109222179 B CN 109222179B
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curcumin
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starch
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CN109222179A (en
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安凤平
宋洪波
万成
何丹
黄群
滕慧
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Fujian Agriculture and Forestry University
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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00—Shaping or working of foodstuffs characterised by the products
    • A23P10/30—Encapsulation of particles, e.g. foodstuff additives
    • 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
    • A23L29/03—Organic compounds
    • 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
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/30—Foods 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
    • 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
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3454—Preservation 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
    • A23L3/3463—Organic compounds; Microorganisms; Enzymes
    • A23L3/3481—Organic compounds containing oxygen
    • A23L3/3499—Organic compounds containing oxygen with doubly-bound oxygen
    • 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
    • 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

Abstract

The invention relates to a preparation method of curcumin nano-microcapsules, belonging to the technical field of functional foods. The invention takes waxy corn as a base material, prepares composite modified waxy corn starch by esterification and ball milling modification, takes curcumin as a functional component, diglyceride dioleate as an emulsifier and refined soybean oil as base oil, prepares oil liquid by homogenization, adopts a Pickering method combined with moderate heating to obtain O/W type gelatinized nano emulsion, and prepares the curcumin nano microcapsule by high-speed centrifugal spray drying. The invention has the advantages of advanced process, good safety, high encapsulation rate of curcumin, small product granularity, easy absorption and the like.

Description

Preparation method of curcumin nano-microcapsule
Technical Field
The invention relates to a preparation method of curcumin nano-microcapsules, belonging to the technical field of functional foods.
Background
Curcumin is a low relative molecular weight polyphenolic compound extracted from turmeric. Curcumin is one of the natural food pigments with the largest sale amount in the world at present, and is a food additive which is approved by the world health organization and multiple countries. Besides excellent coloring capability, curcumin also has health care efficacy and pharmacological action, and has been found to have physiological activities of resisting inflammation, resisting oxidation, reducing blood fat, resisting virus, resisting atherosclerosis and the like, and has low toxicity and small adverse reaction. However, curcumin has poor water solubility, is partially dissolved in oil and fat, has good acid resistance, but has poor stability in light, heat and oxygen environments, so that the bioavailability is low, and the application of curcumin in the fields of food, medicines and the like is restricted.
The preparation of the curcumin microcapsule or the nano microcapsule by adopting the embedding technology is an important means for improving the stability of the curcumin in the storage period, particularly the small-size effect, the surface effect and the strong adsorbability of the nano microcapsule, and the utilization degree of the encapsulated effective components can be effectively improved. The currently disclosed preparation method of curcumin nano microcapsule emulsion and the product still have defects, the utilization rate of curcumin as a raw material is not high due to unreasonable preparation process, the stability of effective component curcumin in the product is not good, and oil and fat are easy to crystallize; due to the improper encapsulation material, the dissolution or degradation performance in the digestive tract is poor, so that the curcumin cannot be released in time to influence the absorption and utilization of the curcumin.
Pickering emulsion refers to an emulsion obtained by using ultrafine solid particles as an emulsifier, and is also called Pickering emulsion. The method for preparing the O/W type emulsion by taking the starch as the superfine solid particles is a common method and has the advantages of good product safety, easy digestion and the like; however, the emulsifying property of common starch is not ideal enough, and particularly, when a microcapsule product is prepared by adopting the Pickering technology, the coating starch layer can only form a cross-linked network structure and cannot form a compact coating layer, so that the encapsulation efficiency and the product stability are influenced.
Disclosure of Invention
The invention aims to provide a preparation method of curcumin nano-microcapsules aiming at the problems of poor stability or low absorption and utilization rate of the existing curcumin nano-microcapsules, and the prepared curcumin nano-microcapsules have good storage stability, can be directly taken with water and are beneficial to absorption.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing curcumin nano-microcapsule comprises the technological links of compound modified waxy corn starch, curcumin dissolution and emulsification, preparation of gelatinized nano-emulsion, high-speed centrifugal spray drying and the like, and the curcumin nano-microcapsule is prepared.
The method comprises the following specific steps:
(1) composite modified waxy corn starch: adding octenyl succinic anhydride accounting for 2.5-3.5% of the dry mass of starch into waxy corn starch milk accounting for 30-35% of the mass fraction, continuously stirring for 1.5-2 h at 35 ℃, adjusting the pH to 8.0 by using NaOH accounting for 3% of the mass fraction, reacting for 3-5 h at 35 ℃, adjusting the pH to 6.5 by using HCl solution accounting for 3% of the mass fraction, stopping the reaction, centrifuging for 10min at 5000r/min, washing twice by using water and ethanol accounting for 70% of the volume fraction respectively, drying for 24h at 40 ℃, crushing and sieving by using a 100-mesh sieve to obtain esterified starch; treating the esterified starch for 2-5 h by using a planetary ball mill at the rotation speed of 400-600 r/min and 200-300 r/min in a revolution manner to prepare the composite modified starch;
(2) preparing curcumin oil liquid: dispersing curcumin in refined soybean oil, and adding an emulsifier diglycerol dioleate, wherein the mass fraction ratio of the curcumin to the refined soybean oil is as follows: curcumin, diglycerol dioleate, refined soybean oil and refined soybean oil, wherein the ratio of the mass fraction of curcumin to diglycerol dioleate to the mass fraction of refined soybean oil is 5% -20% -1% -2% -78% -94%, and the sum of the mass fractions of curcumin, diglycerol dioleate and refined soybean oil is 100%; homogenizing for 20 min-40 min at 18000 r/min-35000 r/min by adopting a high-speed homogenizer to obtain curcumin oil liquid;
(3) preparing the gelatinized nano emulsion: adding composite modified starch into purified water according to the mass fraction of 0.5-3.0%, adding curcumin oil according to the volume fraction of 10-30%, homogenizing at 15000-25000 r/min by using a high-speed dispersion homogenizer for 2-5 min to prepare O/W type Pickering nano emulsion, heating to 52-65 ℃ and keeping for 1-3 min to ensure that composite modified starch particles on the surface of oil drops are properly gelatinized to form a compact encapsulating layer, thus obtaining the gelatinized nano emulsion;
(4) centrifugal spray drying: and drying the gelatinized nano emulsion by using a centrifugal spray dryer, wherein the rotating speed of a centrifugal atomizer is 8000 r/min-20000 r/min, the inlet air temperature is 120-180 ℃, and the outlet temperature is 90-100 ℃, so as to prepare the curcumin nano microcapsule.
The curcumin nano microcapsule prepared by the method has the particle size of less than 100 mu m, wherein more than 90 percent of particles have the diameter of 15 mu m-60 mu m, and the curcumin encapsulation rate reaches more than 90 percent.
The invention has the following remarkable advantages:
(1) refined soybean oil is used as a carrier, diglycerol dioleate is used as an emulsifier, so that the dispersibility and the solubility of curcumin can be improved, and the crystallization phenomenon of the product in the shelf life can be inhibited; (2) the O/W type Pickering emulsion is prepared by taking waxy corn starch subjected to esterification and ball milling modification after octenyl succinic anhydride as a wall material, and a spherical shell with a compact structure is formed through gelatinization treatment, so that compact embedding of oil is realized, the encapsulation rate of curcumin is effectively improved, the stability of a product and the digestibility of a coating layer are ensured, and the release and utilization of curcumin in gastrointestinal tracts are facilitated; (3) the oil liquid is not subjected to centrifugal treatment in the preparation process, and is combined with Pickering emulsion preparation and gelatinization treatment, so that the curcumin waste is reduced to the maximum extent, and the high utilization rate of the curcumin is ensured.
Drawings
Fig. 1 is a particle size distribution diagram of curcumin nano-microcapsule measured by a laser particle sizer.
Detailed Description
The method is realized by the following technical steps:
a method for preparing curcumin nano-microcapsule comprises the following specific steps:
(1) composite modified waxy corn starch: adding octenyl succinic anhydride accounting for 2.5-3.5% of the dry mass of starch into waxy corn starch milk accounting for 30-35% of the mass fraction, continuously stirring for 1.5-2 h at 35 ℃, adjusting the pH to 8.0 by using NaOH accounting for 3% of the mass fraction, reacting for 3-5 h at 35 ℃, adjusting the pH to 6.5 by using HCl solution accounting for 3% of the mass fraction, stopping the reaction, centrifuging for 10min at 5000r/min, washing twice by using water and ethanol accounting for 70% of the volume fraction respectively, drying for 24h at 40 ℃, crushing and sieving by using a 100-mesh sieve to obtain esterified starch; treating the esterified starch for 2-5 h by using a planetary ball mill at the rotation speed of 400-600 r/min and 200-300 r/min in a revolution manner to prepare the composite modified starch;
(2) preparing curcumin oil liquid: dispersing curcumin in refined soybean oil, and adding an emulsifier diglycerol dioleate, wherein the mass fraction ratio of the curcumin to the refined soybean oil is as follows: curcumin, diglycerol dioleate, refined soybean oil and refined soybean oil, wherein the ratio of the mass fraction of curcumin to diglycerol dioleate to the mass fraction of refined soybean oil is 5% -20% -1% -2% -78% -94%, and the sum of the mass fractions of curcumin, diglycerol dioleate and refined soybean oil is 100%; homogenizing for 20 min-40 min at 18000 r/min-35000 r/min by adopting a high-speed homogenizer to obtain curcumin oil liquid;
(3) preparing the gelatinized nano emulsion: adding the composite modified starch into purified water according to the mass fraction of 0.5-3.0%, adding curcumin oil according to the volume fraction of 10-30%, homogenizing for 2-5 min at 15000-25000 r/min by adopting a high-speed dispersion homogenizer to prepare O/W type Pickering nano emulsion, heating to 52-65 ℃ and keeping for 1-3 min to obtain gelatinized nano emulsion;
(4) high-speed centrifugal spray drying: and drying the gelatinized nano emulsion by using a centrifugal spray dryer, wherein the rotating speed of a centrifugal atomizer is 8000 r/min-20000 r/min, the inlet air temperature is 120-180 ℃, and the outlet temperature is 90-100 ℃, so as to prepare the curcumin nano microcapsule.
In order to fully disclose the method for preparing curcumin nano-microcapsule of the present invention, the following is described with reference to examples.
Example 1
(1) Composite modified waxy corn starch: adding octenyl succinic anhydride accounting for 2.5 percent of the dry mass of the starch into waxy corn starch milk accounting for 30 percent of the mass fraction, continuously stirring for 1.5 hours at 35 ℃, adjusting the pH to 8.0 by using NaOH accounting for 3 percent of the mass fraction, reacting for 3 hours at 35 ℃, adjusting the pH to 6.5 by using HCl solution accounting for 3 percent of the mass fraction to terminate the reaction, centrifuging for 10 minutes at 5000r/min, washing for two times by using water and ethanol accounting for 70 percent of the volume fraction respectively, drying for 24 hours at 40 ℃, and crushing and sieving by using a 100-mesh sieve to obtain esterified starch; treating the esterified starch for 5 hours by using a planetary ball mill at the rotating speed of 400r/min of autorotation and 200r/min of revolution to prepare composite modified starch;
(2) preparing curcumin oil liquid: dispersing curcumin in refined soybean oil, and adding an emulsifier diglycerol dioleate, wherein the mass fraction ratio of the curcumin to the refined soybean oil is as follows: homogenizing curcumin/diglycerol dioleate/refined soybean oil 5: 1: 94 with high speed homogenizer at 18000r/min for 40min to obtain curcumin oil solution;
(3) preparing the gelatinized nano emulsion: adding the composite modified starch into purified water according to the mass fraction of 0.5%, adding curcumin oil according to the volume fraction of 10%, homogenizing for 5min at 15000r/min by adopting a high-speed dispersion homogenizer to prepare O/W type Pickering nano emulsion, heating to 52 ℃ and keeping for 3min to obtain gelatinized nano emulsion;
(4) high-speed centrifugal spray drying: drying the gelatinized Pickering nano emulsion by using a centrifugal spray dryer, wherein the rotating speed of a centrifugal atomizer is 8000r/min, the inlet air temperature is 180 ℃, and the outlet temperature is 100 ℃, so as to prepare the curcumin nano microcapsule.
The curcumin nano microcapsule prepared by the embodiment has the encapsulation rate of 91 percent.
Example 2
(1) Composite modified waxy corn starch: adding octenyl succinic anhydride accounting for 3% of the dry mass of the starch into waxy corn starch milk accounting for 32% of the mass fraction, continuously stirring for 1.8h at 35 ℃, adjusting the pH to 8.0 by using NaOH accounting for 3% of the mass fraction, reacting for 4h at 35 ℃, adjusting the pH to 6.5 by using HCl solution accounting for 3% of the mass fraction to terminate the reaction, centrifuging for 10min at 5000r/min, washing twice by using water and ethanol accounting for 70% of the volume fraction respectively, drying for 24h at 40 ℃, crushing and sieving by using a 100-mesh sieve to obtain esterified starch; treating the esterified starch for 3 hours by using a planetary ball mill at the rotating speed of 500r/min of autorotation and 250r/min of revolution to prepare composite modified starch;
(2) preparing curcumin oil liquid: dispersing curcumin in refined soybean oil, and adding an emulsifier diglycerol dioleate, wherein the mass fraction ratio of the curcumin to the refined soybean oil is as follows: homogenizing curcumin/diglycerol dioleate/refined soybean oil 15: 1.5: 83.5% with high speed homogenizer at 23000r/min for 30min to obtain curcumin oil solution;
(3) preparing the gelatinized nano emulsion: adding the composite modified starch into purified water according to the mass fraction of 1.5%, adding curcumin oil according to the volume fraction of 20%, homogenizing for 4min at 20000r/min by using a high-speed dispersion homogenizer to obtain O/W type Pickering nano emulsion, heating to 58 ℃ and keeping for 2min to obtain gelatinized nano emulsion;
(4) high-speed centrifugal spray drying: drying the gelatinized Pickering nano emulsion by using a centrifugal spray dryer, wherein the rotating speed of a centrifugal atomizer is 15000r/min, the inlet air temperature is 150 ℃, and the outlet temperature is 95 ℃, so as to prepare the curcumin nano microcapsule.
The curcumin nano microcapsule prepared by the embodiment has the encapsulation rate of 93 percent.
Example 3
(1) Composite modified waxy corn starch: adding octenyl succinic anhydride accounting for 3.5 percent of the dry mass of the starch into waxy corn starch milk accounting for 35 percent of the mass fraction, continuously stirring for 2 hours at 35 ℃, adjusting the pH to 8.0 by using NaOH accounting for 3 percent of the mass fraction, reacting for 5 hours at 35 ℃, adjusting the pH to 6.5 by using HCl solution accounting for 3 percent of the mass fraction to terminate the reaction, centrifuging for 10 minutes at 5000r/min, washing twice by using water and ethanol accounting for 70 percent of the volume fraction respectively, drying for 24 hours at 40 ℃, crushing and sieving by using a 100-mesh sieve to obtain esterified starch; treating the esterified starch for 2 hours by using a planetary ball mill at the rotating speed of 600r/min of rotation and 300r/min of revolution to prepare the composite modified starch;
(2) preparing curcumin oil liquid: dispersing curcumin in refined soybean oil, and adding an emulsifier diglycerol dioleate, wherein the mass fraction ratio of the curcumin to the refined soybean oil is as follows: homogenizing curcumin/diglycerol dioleate/refined soybean oil at 35000r/min for 20min by high-speed homogenizer to obtain curcumin oil solution;
(3) preparing the gelatinized nano emulsion: adding the composite modified starch into purified water according to the mass fraction of 3.0%, adding curcumin oil according to the volume fraction of 30%, homogenizing for 2min at 25000r/min by adopting a high-speed dispersion homogenizer to prepare O/W type Pickering nano emulsion, heating to 65 ℃ and keeping for 1min to obtain gelatinized nano emulsion;
(4) high-speed centrifugal spray drying: drying the gelatinized Pickering nano emulsion by using a centrifugal spray dryer, wherein the rotating speed of a centrifugal atomizer is 20000r/min, the inlet air temperature is 120 ℃, and the outlet temperature is 90 ℃, so as to prepare the curcumin nano microcapsule.
The curcumin nano microcapsule prepared by the embodiment has the encapsulation rate of 94 percent.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.

Claims (4)

1. A preparation method of curcumin nano-microcapsules is characterized by comprising the following steps:
(1) composite modified waxy corn starch: esterifying and modifying waxy corn starch by using octenyl succinic anhydride, and performing ball milling modification to prepare composite modified starch;
(2) preparing curcumin oil liquid: dispersing curcumin in oil, adding emulsifier, and homogenizing to obtain curcumin oil solution;
(3) preparing the gelatinized nano emulsion: processing curcumin oil into O/W type Pickering nano emulsion, and pasting a starch coating of oil drops to obtain the pasted nano emulsion;
(4) high-speed centrifugal spray drying: centrifugal spray drying of the gelatinized nano emulsion to prepare curcumin nano microcapsule;
the oil in the step (2) is refined soybean oil, the emulsifier is diglycerol dioleate, the mass fraction ratio of curcumin to diglycerol dioleate to refined soybean oil is 5-20: 1-2: 78-94%, and the sum of the mass fractions of curcumin, diglycerol dioleate and refined soybean oil is 100%; the homogenization treatment is to homogenize for 20-40 min at 18000-35000 r/min by adopting a high-speed homogenizer;
the O/W type Pickering nanoemulsion obtained in the step (3) is processed by adding composite modified starch into purified water according to the mass fraction of 0.5% -3.0%, adding curcumin oil according to the volume fraction of 10% -30%, and homogenizing for 2 min-5 min at 15000 r/min-25000 r/min by adopting a high-speed dispersion homogenizer; the gelatinization of the starch coating is to heat the Pickering nano emulsion to 52-65 ℃ and keep the temperature for 1-3 min.
2. The preparation method of a curcumin nano microcapsule as claimed in claim 1, wherein the esterification modification in step (1) is to add octenyl succinic anhydride accounting for 2.5% -3.5% of the dry mass of starch into waxy corn starch milk accounting for 30% -35% of the mass fraction, continuously stir for 1.5-2 h at 35 ℃, adjust the pH to 8.0 with NaOH accounting for 3% of the mass fraction, react for 3-5 h at 35 ℃, adjust the pH to 6.5 with HCl solution accounting for 3% of the mass fraction, stop the reaction, centrifuge at 5000r/min for 10min, wash twice with water and ethanol accounting for 70% of the volume fraction respectively, dry for 24h at 40 ℃, crush and pass through a 100-mesh sieve to obtain esterified starch; the ball milling modification is to treat the esterified starch for 2 to 5 hours by adopting a planetary ball mill at the rotating speed of 400 to 600r/min of autorotation and 200 to 300r/min of revolution.
3. The method for preparing curcumin nano-microcapsule as claimed in claim 1, wherein the technical parameters of the high speed centrifugal spray drying in step (4) are as follows: the rotating speed of the centrifugal atomizer is 8000 r/min-20000 r/min, the inlet air temperature is 120-180 ℃, and the outlet temperature is 90-100 ℃.
4. The curcumin nano-microcapsule prepared by the preparation method according to any one of claims 1 to 3.
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