CN113575954B - Cod liver oil microcapsule and preparation method thereof - Google Patents

Cod liver oil microcapsule and preparation method thereof Download PDF

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CN113575954B
CN113575954B CN202110779352.1A CN202110779352A CN113575954B CN 113575954 B CN113575954 B CN 113575954B CN 202110779352 A CN202110779352 A CN 202110779352A CN 113575954 B CN113575954 B CN 113575954B
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liver oil
cod liver
microcapsule
parts
solution
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CN113575954A (en
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王志标
罗京
张元坤
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Anhui Jishengyuan Pharmaceutical Co ltd
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    • 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
    • A23L33/115Fatty acids or derivatives thereof; Fats or oils
    • 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
    • A23L29/20Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/244Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin from corms, tubers or roots, e.g. glucomannan
    • 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
    • A23L29/20Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/25Exudates, e.g. gum arabic, gum acacia, gum karaya or tragacanth
    • 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
    • A23L29/20Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/262Cellulose; Derivatives thereof, e.g. ethers
    • 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
    • A23L5/00Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
    • A23L5/30Physical treatment, e.g. electrical or magnetic means, wave energy or irradiation
    • A23L5/32Physical treatment, e.g. electrical or magnetic means, wave energy or irradiation using phonon wave energy, e.g. sound or ultrasonic waves
    • 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
    • A23P10/35Encapsulation of particles, e.g. foodstuff additives with oils, lipids, monoglycerides or diglycerides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02Making microcapsules or microballoons
    • 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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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Nutrition Science (AREA)
  • Dispersion Chemistry (AREA)
  • Molecular Biology (AREA)
  • Organic Chemistry (AREA)
  • Biophysics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Mycology (AREA)
  • Medicinal Preparation (AREA)
  • Manufacturing Of Micro-Capsules (AREA)

Abstract

The invention discloses a cod liver oil microcapsule, which comprises the following raw materials in parts by weight: 10-12 parts of cod liver oil, 15-18 parts of a capsule wall material and 70-75 parts of water, wherein the capsule wall material is a combination of acacia, carboxymethyl cellulose, chitosan and konjac glucomannan. The invention also discloses a preparation method of the cod liver oil microcapsule. The invention has good oxidation resistance; single component, no additive such as corrigent, antioxidant, etc.; no fishy smell, good water solubility and high embedding rate.

Description

Cod liver oil microcapsule and preparation method thereof
Technical Field
The invention relates to the technical field of cod liver oil, in particular to a cod liver oil microcapsule and a preparation method thereof.
Background
The cod liver oil is a fish oil extracted from the liver of fish, and has very complex components, and is rich in EPA and DHA, natural vitamin A, vitamin D, etc. The vitamin A and the vitamin D in the cod liver oil can improve the visual system of a human body and promote bone growth respectively, and are important natural vitamins which are needed to be frequently supplemented by the human body, especially children. Therefore, cod liver oil is commonly used to supplement vitamins a and D required for the body in daily life.
Cod liver oil is poorly soluble in water and has a particular fishy smell, which presents difficulties for its direct consumption and application in formula foods. In addition, polyunsaturated fatty acids contained in cod liver oil are easily oxidized, resulting in an increase in peroxide value, rancidity, and vitamins are also easily oxidized, reducing their food safety and commercial value. People often improve the fishy smell and the problem of easy oxidation of cod liver oil by adding a flavoring agent, an antioxidant and the like, but the flavoring agent and the antioxidant are usually chemical substances, so that the problem of food and medicine safety is easily brought.
At present, the common processing method is to process cod liver oil into products such as concentrated cod liver oil preparation, cod liver oil capsule and the like, but the products need to be taken frequently, and a plurality of places still exist in the aspect of product characteristics to be improved. Most prominently, the problem of fishy smell and extremely easy oxidation of the product still cannot be well solved, and the shelf life, the safety and the edible mouthfeel of the commodity are affected, so that the commodity value is affected.
Disclosure of Invention
Based on the technical problems in the background technology, the invention provides a cod liver oil microcapsule and a preparation method thereof, and the cod liver oil microcapsule has good oxidation resistance; single component, no additive such as corrigent, antioxidant, etc.; no fishy smell, good water solubility and high embedding rate.
The invention provides a cod liver oil microcapsule, which comprises the following raw materials in parts by weight: 10-12 parts of cod liver oil, 15-18 parts of a capsule wall material and 70-75 parts of water, wherein the capsule wall material is a combination of acacia, carboxymethyl cellulose, chitosan and konjac glucomannan.
The water is purified water or the like; the raw materials are all subjected to sterilization treatment.
Preferably, the weight ratio of the acacia, the carboxymethyl cellulose, the chitosan and the konjak glucomannan is 2:2.5:0.6-0.7:0.3-0.4.
The invention also provides a preparation method of the cod liver oil microcapsule, which comprises the following steps:
s1, dissolving acacia, carboxymethyl cellulose, konjak glucomannan and chitosan in an acetic acid aqueous solution to obtain a solution A;
s2, uniformly mixing the cod liver oil with the solution A, performing ultrasonic emulsification to obtain an emulsion, standing, freezing again, and finally performing vacuum freeze drying to obtain the cod liver oil microcapsule.
Preferably, in S2, the power of the phacoemulsification is 300-500W.
Preferably, in S2, the time of phacoemulsification is 15-25min.
Preferably, in S2, the mixture is left to stand for 30 to 50 minutes.
Preferably, in S2, the freezing is performed for 8-12 hours.
Preferably, in S2, the temperature of the vacuum freeze-drying is-15 to-20℃for 1.5 to 2.5 days.
Preferably, in S1, the volume fraction of acetic acid in the aqueous acetic acid solution is 0.2-0.4%.
The preparation method is completed in a 10 ten thousand-grade clean area.
The beneficial effects are that:
1. the invention selects the Arabic gum and the carboxymethyl cellulose to have negative charges, the chitosan has positive charges and has electrostatic interaction, and the two components are matched with each other in a proper proportion, so that the emulsion has good stability, and the problem of uneven grain diameter of the microcapsule prepared by the later freeze drying is avoided; in addition, due to the existence of electrostatic interaction, the uniformity of a formed film can be improved, the surface smoothness of microcapsule particles can be improved, the oxygen permeability can be reduced, the oxidation resistance of the microcapsule can be improved, and the embedding rate can be improved;
2. the konjac glucomannan and the carboxymethyl cellulose are matched with each other in a proper proportion, so that the water solubility of the microcapsule can be improved; the embedding rate of cod liver oil can be improved by the mutual matching of konjak glucomannan, arabic gum, carboxymethyl cellulose and chitosan, so that the oxidation resistance can be further improved;
3. the proper ultrasonic process is selected, so that the emulsion with tiny liquid drops (oil-in-water) and uniform size can be obtained while the oxidation is kept low, and the embedding rate can be improved by the proper freeze-drying process; the active ingredient of the invention is only cod liver oil, and does not contain other additives; in addition, the invention can realize targeted absorption of small intestine and improve bioavailability.
Detailed Description
The technical scheme of the invention is described in detail through specific embodiments.
Examples 1 to 8
In order to select a proper capsule wall material, the following experiments were performed to compare the properties of the microcapsules obtained by different ratios of the capsule wall materials. The specific formulation is shown in table 1.
Table 1 formulations of examples 1-8
The preparation methods of the above examples 1 to 8 are the same, and specifically include the following steps:
s1, weighing purified water according to weight, and adding acetic acid to prepare an acetic acid aqueous solution with the volume fraction of 0.3%; then adding the capsule wall material according to the weight, and stirring until the capsule wall material is dissolved to obtain solution A;
s2, weighing cod liver oil according to weight, adding the cod liver oil into the solution A, stirring and coarse mixing, then placing the mixture into an ultrasonic instrument, adjusting the power to 400W, performing ultrasonic emulsification for 25min to obtain emulsion, taking out the emulsion, standing for 40min, freezing at-5 ℃ for 12h, and finally performing vacuum freeze drying at-20 ℃ for 2 days to obtain the cod liver oil microcapsule.
Experiment 1
The cod liver oil microcapsules prepared in examples 1 to 8 were each examined, and the results are shown in Table 2.
1. The detection method of the microcapsule embedding rate comprises the following steps:
a. surface oil: accurately weighing M (2-5 g) microcapsules into a dried conical flask, adding 30ml of petroleum ether with the boiling range of 30-60 ℃, carrying out shaking extraction for 5min, filtering with filter paper, washing the conical flask and the filter paper with 10ml of petroleum ether, collecting the obtained filtrate in a conical flask (M1) with constant dry weight, evaporating the filtrate in a water bath with the temperature of 60 ℃, and then transferring the filtrate into a blast drying oven to be dried with the temperature of 60 ℃ until the weight is constant (M2). 3 replicates were run and the test data was an average of 3.
Surface oil= (M2-M1)/mx100%; wherein M is microcapsule mass (g), M1 is cone mass (g), and M2 is cone and grease mass (g) after drying.
b. Total oil: accurately weighing 2g of microcapsules in a 50ml large test tube, adding 8ml of water to fully dissolve the microcapsules, adding 10ml of concentrated hydrochloric acid, placing the microcapsules in a 80 ℃ water bath for 1h, and shaking or stirring the microcapsules once every 10 min; taking out the test tube, adding 10ml of 95% ethanol, mixing, cooling, transferring into a 100ml measuring cylinder with a plug, adding 30ml of diethyl ether, adding the plug, shaking for 1min, standing for 10min, opening the plug, and flushing the plug and the wall of the measuring cylinder with 20ml of petroleum ether-diethyl ether equivalent mixed solution; sucking out the supernatant liquid in a conical flask with constant dry weight (M1) when the upper liquid is clear; adding 10ml of diethyl ether into a measuring cylinder with a plug, shaking, standing, sucking the diethyl ether on the upper layer, and placing into an original conical flask; the conical flask was evaporated to dryness on a water bath and dried to constant weight (M2) in an oven at 105.+ -. 1 ℃.3 replicates were run and the test data was an average of 3.
Total oil= (M2-M1)/2×100%; wherein M1 is the mass (g) of the conical flask, and M2 is the mass (g) of the dried conical flask and grease;
embedding rate= (1-surface oil/total oil) ×100%.
2. The solubility of the microcapsules was measured as: dissolving 5g microcapsule in 100ml beaker with 50ml distilled water (25-30deg.C), centrifuging at 4500r/min for 10min, removing supernatant, adding 50ml water, stirring for dissolving, centrifuging for 10min, removing supernatant, washing precipitate with small amount of water into weighing bottle (M1), steaming to remove water, transferring to 105deg.C, and oven drying to constant weight (M2).
Solubility = 1- (M2-M1)/(1-B)/mx100%; wherein M is the mass (g) of the microcapsule, M1 is the mass (g) of the weighing bottle, M2 is the mass (g) of the weighing bottle and insoluble matter, and B is the moisture content (%) of the microcapsule, wherein the moisture of the microcapsule is measured by a direct drying method of GB/T5009.3-2003.
TABLE 2 detection results
As can be seen from Table 2, the microcapsules prepared in examples 6 and 7 were excellent in the embedding rate, solubility and water content.
Experiment 2
The cod liver oil crude oil, the microcapsules prepared in example 6 and example 7 were stored in an incubator at 60.+ -. 1 ℃ for 8 days, and the peroxide value was measured every 2 days, and the results are shown in Table 3.
The detection method of the peroxide value of the microcapsule comprises the following steps:
a. extraction of grease: 15g of microcapsule is taken and placed in a 100ml beaker, 50ml of water (45-50 ℃) is added, stirring is carried out until the microcapsule is completely dispersed and dissolved, the microcapsule is transferred to a 250ml separating funnel, 50ml of ethanol is added and uniformly shaken, 30ml of diethyl ether is added, 30s of petroleum ether is added, grease is extracted, standing and layering are carried out, the lower water phase is discarded, the upper layer is clarified, the microcapsule is transferred to a 250ml conical flask with a plug, and 5g of anhydrous sodium sulfate is added, and the microcapsule is shaken for 1min to remove water; the ether phase from which water has been removed is filtered with a quick filter paper in a weighed 250ml iodophor bottle, and the iodophor bottle is placed in a water bath at 60 ℃ in a fume hood and evaporated to dryness to obtain the grease.
b. Measurement of peroxide value: the peroxide value of the microcapsule was measured with reference to GB/T5009.37-2003 "measurement of peroxide value of animal and vegetable fats & oils".
TABLE 3 detection results
As can be seen from Table 3, the cod liver oil microcapsules prepared in examples 6 and 7 have good oxidation resistance and good stability.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.

Claims (4)

1. The cod liver oil microcapsule is characterized by comprising the following raw materials in parts by weight: 10-12 parts of cod liver oil, 15-18 parts of a capsule wall material and 70-75 parts of water, wherein the capsule wall material is a combination of acacia, carboxymethyl cellulose, chitosan and konjac glucomannan;
the weight ratio of the acacia to the carboxymethyl cellulose to the chitosan to the konjac glucomannan is 2:2.5:0.6-0.7:0.3-0.4;
the preparation method of the cod liver oil microcapsule comprises the following steps:
s1, dissolving acacia, carboxymethyl cellulose, konjak glucomannan and chitosan in an acetic acid aqueous solution to obtain a solution A;
s2, uniformly mixing cod liver oil with the solution A, performing ultrasonic emulsification to obtain an emulsion, standing, freezing again, and finally performing vacuum freeze drying to obtain a cod liver oil microcapsule;
in S2, the power of ultrasonic emulsification is 300-500W;
in S2, the time of ultrasonic emulsification is 15-25min;
in S2, standing for 30-50min;
in S2, freezing for 8-12h.
2. A process for preparing cod liver oil microcapsules as claimed in claim 1 comprising the steps of:
s1, dissolving acacia, carboxymethyl cellulose, konjak glucomannan and chitosan in an acetic acid aqueous solution to obtain a solution A;
s2, uniformly mixing the cod liver oil with the solution A, performing ultrasonic emulsification to obtain an emulsion, standing, freezing again, and finally performing vacuum freeze drying to obtain the cod liver oil microcapsule.
3. The method for preparing cod liver oil microcapsules according to claim 2, wherein in S2, the temperature of vacuum freeze-drying is-15 to-20 ℃ for 1.5 to 2.5 days.
4. The method for preparing cod liver oil microcapsules according to claim 2, wherein in S1, the volume fraction of acetic acid in the aqueous acetic acid solution is 0.2 to 0.4%.
CN202110779352.1A 2021-07-09 2021-07-09 Cod liver oil microcapsule and preparation method thereof Active CN113575954B (en)

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Citations (4)

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CN105505580A (en) * 2015-12-14 2016-04-20 长江大学 Microcapsule and preparation method thereof
CN110025638A (en) * 2019-03-29 2019-07-19 华中科技大学 Chitosan-sodium carboxymethylcellulose LBL self-assembly probiotics micro-capsule and its preparation
CN112544975A (en) * 2020-12-10 2021-03-26 山东省科学院生物研究所 Method for producing fish oil microcapsules by using konjac glucomannan aerogel

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CN102293266A (en) * 2011-08-18 2011-12-28 中国海洋大学 Method for preparing antioxidant fish oil microcapsule
CN105505580A (en) * 2015-12-14 2016-04-20 长江大学 Microcapsule and preparation method thereof
CN110025638A (en) * 2019-03-29 2019-07-19 华中科技大学 Chitosan-sodium carboxymethylcellulose LBL self-assembly probiotics micro-capsule and its preparation
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