CN112450417A - Clausena lansium volatile oil microcapsule powder and preparation method thereof - Google Patents
Clausena lansium volatile oil microcapsule powder and preparation method thereof Download PDFInfo
- Publication number
- CN112450417A CN112450417A CN202011266408.5A CN202011266408A CN112450417A CN 112450417 A CN112450417 A CN 112450417A CN 202011266408 A CN202011266408 A CN 202011266408A CN 112450417 A CN112450417 A CN 112450417A
- Authority
- CN
- China
- Prior art keywords
- volatile oil
- clausena lansium
- microcapsule powder
- parts
- oil microcapsule
- 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.)
- Granted
Links
- 244000089795 Clausena lansium Species 0.000 title claims abstract description 84
- 235000008738 Clausena lansium Nutrition 0.000 title claims abstract description 84
- 239000000341 volatile oil Substances 0.000 title claims abstract description 81
- 239000003094 microcapsule Substances 0.000 title claims abstract description 69
- 239000000843 powder Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims description 26
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- GUOCOOQWZHQBJI-UHFFFAOYSA-N 4-oct-7-enoxy-4-oxobutanoic acid Chemical compound OC(=O)CCC(=O)OCCCCCCC=C GUOCOOQWZHQBJI-UHFFFAOYSA-N 0.000 claims description 15
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Images
Classifications
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- A—HUMAN NECESSITIES
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- 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
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/10—Natural spices, flavouring agents or condiments; Extracts thereof
- A23L27/12—Natural spices, flavouring agents or condiments; Extracts thereof from fruit, e.g. essential oils
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/70—Fixation, conservation, or encapsulation of flavouring agents
- A23L27/72—Encapsulation
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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Abstract
The invention discloses clausena lansium volatile oil microcapsule powder, and relates to the field of essence and spice. The clausena lansium volatile oil microcapsule powder comprises the following components in parts by weight: 30-50 parts of clausena lansium volatile oil, 50-70 parts of wall material, 0.5-3 parts of emulsifier and 0.05-0.5 part of antioxidant. The clausena lansium volatile oil microcapsule powder provided by the invention has the advantages that the glass transition temperature is more than 80 ℃, and the heat resistance, the embedding rate and the storage resistance are good.
Description
Technical Field
The invention relates to the field of essence and flavor, in particular to clausena lansium volatile oil microcapsule powder and a preparation method thereof.
Background
The wampee is a characteristic fruit in south China, is rich in vitamin C, sugar, organic acid and pectin, can be used as a medicine for both pericarp and kernel, and has the effects of promoting digestion, reducing phlegm and regulating qi. The clausena lansium is popular with consumers due to the special aroma of fruits and fruit peels, and the special aroma mainly comprises volatile oil components. The preparation of microcapsules by utilizing a spray drying technology is a common method, the quality of the microcapsules is evaluated by taking the embedding rate, the heat resistance, the fluidity and the slow release property as indexes in the prior art, and the quality of the microcapsules is not evaluated by comprehensive indexes.
Glass transition temperature TgWhen the temperature of the liquid drops is lower than the vitrification temperature of the capsule wall, the microcapsule wall becomes a glass state and does not form a semi-permeable membrane, and the microcapsule wall becomes a hard shell, which often occurs in the constant-speed drying stage of the liquid drops, the diffusion speed of most of water in the liquid drops is higher than the evaporation speed, so that the microcapsule wall can be rapidly dehydrated, the vitrification temperature is rapidly increased, the surface temperature of the liquid drops is lower than the vitrification temperature of the capsule wall, and the capsule wall becomes a glass state; when the temperature of the liquid drops is higher than the viscous flow temperature, the material is in a fluid state and can be adhered to the tower wall of the spraying tower during operation, and the microcapsule effect can be changed due to the influence of high temperature on part of dried particles. Glass transition temperature T of the productgThe heat resistance, the storage stability, the embedding rate and the like of the microcapsule product are directly influenced. Most microcapsule products on the market generally have a glass transition temperature below 70 ℃.
Disclosure of Invention
Based on the above, the invention aims to overcome the defects of the prior art and provide the clausena lansium volatile oil microcapsule powder which has the glass transition temperature of more than 80 ℃ and has good heat resistance, embedding rate and storage stability.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: the clausena lansium volatile oil microcapsule powder comprises the following components in parts by weight: 30-50 parts of clausena lansium volatile oil, 50-70 parts of wall material, 0.5-3 parts of emulsifier and 0.05-0.5 part of antioxidant.
Preferably, the clausena lansium volatile oil microcapsule powder comprises the following components in parts by weight: 35-45 parts of clausena lansium volatile oil, 55-65 parts of wall material, 1-2 parts of emulsifier and 0.1-0.3 part of antioxidant.
Preferably, the clausena lansium volatile oil microcapsule powder comprises the following components in parts by weight: 38 parts of clausena lansium volatile oil, 60 parts of wall material, 1.8 parts of emulsifier and 0.2 part of antioxidant.
Preferably, the preparation method of the clausena lansium volatile oil comprises the following steps: pulverizing dried Clausena lansium (lour.) Szecht or Clausena lansium pericarp, and extracting with supercritical carbon dioxide to obtain Clausena lansium volatile oil.
Preferably, the supercritical carbon dioxide extraction process is: the extraction pressure is 20-30MPa, the extraction temperature is 35-60 ℃, the extraction time is 1-4h, the pressure of a separation chamber 1 is 6-12MPa, and the temperature is 40-60 ℃; the pressure of the separation 2 chamber is 5-10MPa, and the temperature is 30-45 ℃.
The invention extracts the volatile oil of the Chinese wampee fruit or Chinese wampee peel by using the supercritical carbon dioxide extraction technology, the extraction temperature is low, the Chinese wampee peel fragrance component is retained to a great extent, the extraction yield is high, and the fragrance of the extracted volatile oil is good.
Preferably, the clausena lansium volatile oil microcapsule powder is at least one of the following (a) to (c):
(a) the wall material is a compound of sodium starch octenyl succinate, Arabic gum and maltodextrin, wherein the weight ratio of the sodium starch octenyl succinate to the Arabic gum to the maltodextrin is as follows: sodium starch octenylsuccinate: gum arabic: maltodextrin ═ (3-6): (1-4): (2-5);
(b) the emulsifier is a compound of sodium caseinate and monoglyceride stearate, wherein the weight ratio of the sodium caseinate to the monoglyceride stearate is as follows: sodium caseinate: mono-glycerol stearate ═ 10-20: (1-3);
(c) the antioxidant is at least one of rosemary extract, mixed tocopherol, ascorbyl palmitate, tea polyphenol and phytic acid.
The invention screens 20 wall materials of sodium starch octenyl succinate, oxidized starch, porous starch, beta-cyclodextrin, gelatin, Arabic gum, xanthan gum, carrageenan, pectin, flaxseed gum, chitosan, soy protein isolate, lactalbumin, sodium alginate, maltose syrup, maltodextrin, maltitol, erythritol, sucrose and fructo-oligosaccharide to influence the vitrification temperature of the wampee volatile oil microcapsule powder, wherein the sodium starch octenyl succinate, the Arabic gum and the maltodextrin are good in compound emulsibility and film forming property, and the formed wampee volatile oil is high in glass temperature of the microcapsule powder, high in product yield, good in heat resistance, good in storage resistance and high in embedding rate. Finally, the compounded octenyl succinic acid starch sodium, Arabic gum and maltodextrin are selected as the wall material of the invention.
The invention improves the glass transition temperature of the clausena lansium volatile oil microcapsule powder by selecting proper emulsifier and antioxidant, thereby improving the heat resistance stability and storage stability of the product.
Preferably, the weight ratio of the starch sodium octenyl succinate, the Arabic gum and the maltodextrin is as follows: sodium starch octenylsuccinate: gum arabic: maltodextrin 4: 3: 3; the weight ratio of the sodium caseinate to the monoglyceride stearate is as follows: sodium caseinate: monoglyceride stearate ═ 14: 2.
in addition, the invention also provides a preparation method of the clausena lansium volatile oil microcapsule powder, which comprises the following steps:
(1) preparing an aqueous phase: adding 50-70 ℃ water into the wall material, stirring and dissolving to obtain a water phase A, wherein the mass concentration of the solid of the water phase A is 40-50%;
(2) preparing an oil phase: mixing emulsifier, antioxidant and cortex Phellodendri volatile oil at 40-60 deg.C to obtain oil phase B;
(3) emulsification: adding the oil phase B obtained in the step (2) into the water phase A obtained in the step (1), and stirring to obtain a crude emulsion;
(4) homogenizing and spray drying: and (4) homogenizing the coarse emulsion obtained in the step (3), preserving the temperature of the homogenized solution, and performing spray drying to obtain the clausena lansium volatile oil microcapsule powder.
Preferably, in the step (1), the stirring time is 20-30 min; in the step (3), the stirring speed is 10000-30000rpm, and the stirring time is 20-40 min.
In general microcapsule preparation process, in order to control the viscosity of the feed liquid to be too high, the mass concentration of the solid is generally below 40%. The invention improves the solid mass concentration of wall material solution to 40-50%, reduces water content, quickly evaporates water in the spraying process, quickly forms the microcapsule powder structure of the wampee volatile oil, and improves the vitrification temperature.
Preferably, in the step (4), the homogenizing pressure is 20-40MPa, the homogenizing times are 2-3 times, and the heat preservation temperature is 50-60 ℃; the air inlet temperature of the spray drying is 160-180 ℃, and the air outlet temperature of the spray drying is 80-85 ℃.
The invention keeps the temperature of the feed liquid at 50-60 ℃ during spraying, so that the feed liquid system has a higher glass transition temperature starting point at the beginning of spraying, and the invention is beneficial to shortening the time of passing through viscous state and high elastic state.
The spray drying process is the key for influencing the formation and performance of the microcapsule, and the invention improves the drying efficiency by controlling the spray drying inlet air temperature of 160-180 ℃, accelerates the formation of the microcapsule, and simultaneously controls the outlet air temperature of 80-85 ℃, thereby reducing the influence of the microcapsule on high temperature.
Preferably, the glass transition temperature of the clausena lansium volatile oil microcapsule powder is more than 80 ℃.
Compared with the prior art, the invention has the beneficial effects that: (1) the product embedding rate of the invention reaches up to 99.7 percent, the glass transition temperature reaches up to 91.9 ℃, the fragrance retention rate of the product is up to 98.2 percent when the product is heated at 80 ℃ for 30min, the fragrance retention rate of the product is up to 90.6 percent when the product is placed at 40 ℃ and RH75 percent for 3 months, and the product has good heat-resistant stability and storage stability, and is beneficial to the storage, transportation, wide processing and application of the clausena lansium volatile oil microcapsule powder. (2) The preparation method provided by the invention has the advantages of low cost, simple process flow, strong operability, high microcapsule yield, no pollution and good repeatability, and can realize large-scale industrial continuous production.
Drawings
FIG. 1 is a GC-MS total ion current chromatogram of supercritical carbon dioxide extraction of Clausena lansium volatile oil.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to the accompanying drawings and specific embodiments.
Examples 1-6 are provided herein, and the components and parts by weight of specific examples 1-6 are selected as shown in tables 1 and 2:
TABLE 1 selection of parts by weight of specific examples 1-6
TABLE 2 selection of Components for specific examples 1-6
Example 1
Example the preparation method of the clausena lansium volatile oil microcapsule powder described in example 1, after weighing the components according to tables 1 and 2, comprises the following steps:
(1) preparing an aqueous phase: adding water with the temperature of 70 ℃ into the wall material, stirring for dissolving, wherein the stirring time is 30min, and obtaining the water phase A with the solid content and the mass concentration of 50%;
(2) preparing an oil phase: mixing emulsifier, antioxidant and Clausena lansium volatile oil at 60 deg.C to obtain oil phase B;
(3) emulsification: adding the oil phase B obtained in the step (2) into the water phase A obtained in the step (1), and stirring at the speed of 30000rpm for 40min to obtain a crude emulsion;
(4) homogenizing and spray drying: homogenizing the crude emulsion obtained in the step (3) for 3 times under the homogenizing pressure of 30MPa, and keeping the temperature of the homogenized solution at 60 ℃, spray-drying at the air inlet temperature of 180 ℃ and at the air outlet temperature of 85 ℃ to obtain the clausena lansium volatile oil microcapsule powder.
Example 2
Example the preparation method of the clausena lansium volatile oil microcapsule powder described in example 2, after weighing the components according to tables 1 and 2, comprises the following steps:
(1) preparing an aqueous phase: adding water with the temperature of 60 ℃ into the wall material, stirring for dissolving, wherein the stirring time is 30min, and obtaining the water phase A with the solid content and the mass concentration of 40%;
(2) preparing an oil phase: mixing emulsifier, antioxidant and Clausena lansium volatile oil at 40 deg.C to obtain oil phase B;
(3) emulsification: adding the oil phase B obtained in the step (2) into the water phase A obtained in the step (1), and stirring at the stirring speed of 10000rpm for 20min to obtain a crude emulsion;
(4) homogenizing and spray drying: homogenizing the crude emulsion obtained in the step (3) at a homogenizing pressure of 20MPa for 2 times, preserving the temperature of the homogenized solution at 50 ℃, and performing spray drying at an inlet air temperature of 160 ℃ and an outlet air temperature of 80 ℃ to obtain the clausena lansium volatile oil microcapsule powder.
Example 3
Example the preparation method of the clausena lansium volatile oil microcapsule powder described in example 3, after weighing the components according to tables 1 and 2, comprises the following steps:
(1) preparing an aqueous phase: adding 65 ℃ water into the wall material, stirring for dissolving, wherein the stirring time is 30min, and obtaining the water phase A with the solid content mass concentration of 45%;
(2) preparing an oil phase: mixing emulsifier, antioxidant and Clausena lansium volatile oil at 50 deg.C to obtain oil phase B;
(3) emulsification: adding the oil phase B obtained in the step (2) into the water phase A obtained in the step (1), and stirring at the stirring speed of 10000rpm for 20min to obtain a crude emulsion;
(4) homogenizing and spray drying: homogenizing the crude emulsion obtained in the step (3) at 25MPa for 2 times, keeping the temperature of the homogenized solution at 60 ℃, spray-drying at 165 ℃ for air inlet, and 80 ℃ for air outlet.
Example 4
Example the preparation method of the clausena lansium volatile oil microcapsule powder described in example 4, after weighing the components according to tables 1 and 2, comprises the following steps:
(1) preparing an aqueous phase: adding water with the temperature of 70 ℃ into the wall material, stirring for dissolving, wherein the stirring time is 20min, and obtaining the water phase A with the solid content and the mass concentration of 40%;
(2) preparing an oil phase: mixing emulsifier, antioxidant and Clausena lansium volatile oil at 50 deg.C to obtain oil phase B;
(3) emulsification: adding the oil phase B obtained in the step (2) into the water phase A obtained in the step (1), and stirring at the speed of 20000rpm for 30min to obtain a crude emulsion;
(4) homogenizing and spray drying: homogenizing the crude emulsion obtained in the step (3) at the homogenizing pressure of 40MPa for 2 times, preserving the temperature of the homogenized solution at 55 ℃, and performing spray drying at the inlet air temperature of 170 ℃ and the outlet air temperature of 85 ℃ to obtain the clausena lansium volatile oil microcapsule powder.
Example 5
Example the preparation method of the clausena lansium volatile oil microcapsule powder described in example 5, after weighing the components according to tables 1 and 2, comprises the following steps:
(1) preparing an aqueous phase: adding water with the temperature of 50 ℃ into the wall material, stirring for dissolving, wherein the stirring time is 30min, and obtaining the water phase A with the solid content and the mass concentration of 45%;
(2) preparing an oil phase: mixing emulsifier, antioxidant and Clausena lansium volatile oil at 55 deg.C to obtain oil phase B;
(3) emulsification: adding the oil phase B obtained in the step (2) into the water phase A obtained in the step (1), and stirring at the speed of 15000rpm for 35min to obtain a crude emulsion;
(4) homogenizing and spray drying: homogenizing the crude emulsion obtained in the step (3) at 25MPa for 2 times, keeping the temperature of the homogenized solution at 55 ℃, spray-drying at 165 ℃ for air inlet and 80 ℃ for air outlet, and thus obtaining the clausena lansium volatile oil microcapsule powder.
Example 6
Example the preparation method of the clausena lansium volatile oil microcapsule powder described in example 6, after weighing the components according to tables 1 and 2, comprises the following steps:
(1) preparing an aqueous phase: adding 65 ℃ water into the wall material, stirring for dissolving, wherein the stirring time is 25min, and obtaining the water phase A with the solid content mass concentration of 43%;
(2) preparing an oil phase: mixing emulsifier, antioxidant and Clausena lansium volatile oil at 60 deg.C to obtain oil phase B;
(3) emulsification: adding the oil phase B obtained in the step (2) into the water phase A obtained in the step (1), and stirring at the speed of 20000rpm for 30min to obtain a crude emulsion;
(4) homogenizing and spray drying: homogenizing the crude emulsion obtained in the step (3) at the homogenizing pressure of 30MPa for 2 times, preserving the temperature of the homogenized solution at 60 ℃, and performing spray drying at the inlet air temperature of 175 ℃ and the outlet air temperature of 80 ℃ to obtain the clausena lansium volatile oil microcapsule powder.
Meanwhile, comparative examples 1 to 9 are provided in the present application, and the comparative examples 1 to 9 are specifically as follows:
the wall material of comparative example 1 is 45 parts by weight, and the selection of the components of the wall material, the selection of the rest components, the selection of the parts by weight and the preparation method are completely the same as those of example 3;
the wall material of comparative example 2 is a combination of whey protein isolate, gelatin and maltose syrup, in a ratio of 4: 3: 3, the selection of the rest components and the parts by weight and the preparation method are completely the same as the embodiment 3;
the wall material of the comparative example 3 is the compound of the soybean protein isolate, the beta-cyclodextrin and the sucrose, and the proportion is 4: 3: 3, the selection of the rest components and the parts by weight and the preparation method are completely the same as the embodiment 3;
the emulsifier of comparative example 4 is 0.4 part by weight, and the rest components, parts by weight selection and preparation method are completely the same as those of example 3;
the wall material of comparative example 5 was a blend of sodium starch octenyl succinate and maltodextrin, wherein the ratio of sodium starch octenyl succinate: maltodextrin ═ 6: 4, the selection of the rest components and the parts by weight and the preparation method are completely the same as the embodiment 3;
the wall material of comparative example 6 was a combination of sodium starch octenyl succinate, gum arabic and maltodextrin, wherein the ratio of sodium starch octenyl succinate: gum arabic: maltodextrin ═ 2: 5: 1, the selection of the rest components and the parts by weight and the preparation method are completely the same as the example 3;
in the preparation method of comparative example 7, when the spray drying is performed in the step (4), the inlet air temperature of the spray drying is 190 ℃, the outlet air temperature of the spray drying is 90 ℃, and the selection of the other components and the parts by weight and the preparation method are completely the same as those of the example 3;
in the preparation method of the comparative example 8, the homogeneous liquid in the step (4) is not subjected to heat preservation, and the selection of the rest components, the selection of the parts by weight and the preparation method are completely the same as those of the example 3;
in the production method of comparative example 9, the mass concentration of the solid matter obtained in step (1) was 35%, and the selection of the remaining components, the selection of the parts by weight, and the production method were completely the same as those of example 3.
Test example 1 gas chromatography-mass spectrometry for identifying volatile oil component of Clausena lansium
Sample pretreatment: adding 100mg of a sample into 10ml of n-hexane for ultrasonic dissolution;
GC-MS chromatographic conditions: a chromatographic column: TG-5MSSIL (30m, 0.25mm, 0.25 μm); ion source temperature: 300 ℃; ionization energy: 70 eV; transmission line temperature: 300 ℃; an ionization source (EI); the scanning mode is as follows: full Scan (35-450); sample inlet temperature: 250 ℃; split mode, split ratio: 50; flow rate of carrier gas: 1 ml/min;
temperature programming: maintaining at 70 deg.C for 2min, heating to 280 deg.C at 3 deg.C/min, and maintaining for 10 min.
Profiling from FIG. 1Known as supercritical CO2The main components of the extracted clausena lansium volatile oil are alpha-cis-bergamotene (the relative content is 42.18%), D-germacrene (the relative content is 12.38%), trans-beta-farnesene (the relative content is 5.60%) beta-phellandrene (the relative content is 5.32%), and the results in figure 1 show that the most main component of the supercritical extracted clausena lansium volatile oil is alpha-cis-bergamotene.
Test example 2 Performance test of Clausena lansium volatile oil microcapsule powder
1. Determination of the yield
The yield is equal to the yield of the clausena lansium volatile oil microcapsule powder/raw material input amount multiplied by 100 percent
2. Determination of the glass transition temperature Tg
Weighing 5 + -0.2 mg of clausena lansium volatile oil microcapsule powder, and placing in an aluminum box with an empty aluminum box as reference. The scanning temperature range is 20-150 ℃, the heating rate is 5 ℃/min, and the glass transition temperature Tg is measured by a Differential Scanning Calorimeter (DSC).
3. Determination of embedding Rate
The method for measuring the embedding rate refers to the comparative analysis of the preparation of vanilla essential oil microcapsules by cinnabar plum, etc. (cinnabar, Zhangjun, Xufei, Tianjian character, Chuzhong, 4 physical methods [ J ] food science, 2017,38(21):106 + 111.).
The surface oil is extracted with petroleum ether and the total oil is extracted with alkaline ether.
4. Measurement of aroma Retention and peroxide value
Aroma retention rate measuring method: from the results of fig. 1, it can be known that the main component of the supercritical extracted wampee volatile oil is alpha-cis-bergamotene, and the retention rate of the alpha-cis-bergamotene in the storage of the wampee volatile oil microcapsule powder is monitored by using HPLC;
determination method of peroxide number: reference is made to the method of ZHANG et al (ZHANG Y, TAN C, ABBAS S, et al. modified SPI improvees the experimental properties and oxidative stability of fish oil microcapsules [ J ]. Food Hydrocolloids,2015,51: 108-;
stability tests at elevated temperature (80 ℃) and at accelerated conditions (40 ℃, RH 75%) were carried out separately
Stability test procedure at high temperature (80 ℃): and (3) placing the clausena lansium volatile oil microcapsule powder in an oven at the temperature of 80 ℃ for high-temperature test, and taking out after 30min to measure the aroma retention rate and the peroxide value.
Procedure for stability testing under accelerated conditions (40 ℃, RH 75%): the clausena lansium volatile oil microcapsule powder is placed in a constant temperature and humidity box with the temperature of 40 ℃ and RH 75% for testing, and the fragrance retention rate and the peroxide value are monitored for 3 months.
The results of the performance test of the clausena lansium volatile oil microcapsule powder are as follows: the test results are shown in table 1:
TABLE 1 EXAMPLES 1-6 clausena lansium volatile oil microcapsule powder Performance test results
TABLE 2 comparative examples 1-9 clausena lansium volatile oil microcapsule powder Performance test results
The test results in table 1 show that the Chinese wampee volatile oil microcapsule powder has a high glass transition temperature Tg (as high as 91.9 ℃), an embedding rate of over 95%, a fragrance retention rate of 98.2% after 30min treatment at 80 ℃, a fragrance retention rate of over 85% after 3 months of acceleration at 40 ℃ of RH 75%, a small peroxide change, good thermal stability and good storage stability. The clausena lansium volatile oil microcapsule powder of the comparative example, which is not limited by the conditions of the invention, has a very low glass transition temperature of 41.9 ℃ at the lowest and a low embedding rate, and has a low fragrance retention rate of 41.7 percent after being treated at 80 ℃ for 30min, a low fragrance retention rate of 26.8 percent after being accelerated at 40 ℃ of RH75 percent for 3 months.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The clausena lansium volatile oil microcapsule powder is characterized by comprising the following components in parts by weight: 30-50 parts of clausena lansium volatile oil, 50-70 parts of wall material, 0.5-3 parts of emulsifier and 0.05-0.5 part of antioxidant.
2. The clausena lansium volatile oil microcapsule powder according to claim 1, which comprises the following components in parts by weight: 35-45 parts of clausena lansium volatile oil, 55-65 parts of wall material, 1-2 parts of emulsifier and 0.1-0.3 part of antioxidant.
3. The clausena lansium volatile oil microcapsule powder according to claim 2, which comprises the following components in parts by weight: 38 parts of clausena lansium volatile oil, 60 parts of wall material, 1.8 parts of emulsifier and 0.2 part of antioxidant.
4. The clausena lansium volatile oil microcapsule powder according to any one of claims 1 to 3, wherein the preparation method of the clausena lansium volatile oil comprises the following steps: pulverizing dried Clausena lansium (lour.) Szecht or Clausena lansium pericarp, and extracting with supercritical carbon dioxide to obtain Clausena lansium volatile oil.
5. The clausena lansium volatile oil microcapsule powder according to any one of claims 1 to 3, wherein at least one of the following (a) to (c):
(a) the wall material is a compound of sodium starch octenyl succinate, Arabic gum and maltodextrin, wherein the weight ratio of the sodium starch octenyl succinate to the Arabic gum to the maltodextrin is as follows: sodium starch octenylsuccinate: gum arabic: maltodextrin ═ (3-6): (1-4): (2-5);
(b) the emulsifier is a compound of sodium caseinate and monoglyceride stearate, wherein the weight ratio of the sodium caseinate to the monoglyceride stearate is as follows: sodium caseinate: mono-glycerol stearate ═ 10-20: (1-3);
(c) the antioxidant is at least one of rosemary extract, mixed tocopherol, ascorbyl palmitate, tea polyphenol and phytic acid.
6. The clausena lansium volatile oil microcapsule powder according to claim 5, wherein the weight ratio of the sodium starch octenyl succinate, the gum arabic and the maltodextrin is as follows: sodium starch octenylsuccinate: gum arabic: maltodextrin 4: 3: 3; the weight ratio of the sodium caseinate to the monoglyceride stearate is as follows: sodium caseinate: monoglyceride stearate ═ 14: 2.
7. a method for preparing the clausena lansium volatile oil microcapsule powder according to any one of claims 1 to 6, which comprises the following steps:
(1) preparing an aqueous phase: adding 50-70 ℃ water into the wall material, stirring and dissolving to obtain a water phase A, wherein the mass concentration of the solid of the water phase A is 40-50%;
(2) preparing an oil phase: mixing emulsifier, antioxidant and cortex Phellodendri volatile oil at 40-60 deg.C to obtain oil phase B;
(3) emulsification: adding the oil phase B obtained in the step (2) into the water phase A obtained in the step (1), and stirring to obtain a crude emulsion;
(4) homogenizing and spray drying: and (4) homogenizing the coarse emulsion obtained in the step (3), preserving the temperature of the homogenized solution, and performing spray drying to obtain the clausena lansium volatile oil microcapsule powder.
8. The method for preparing the clausena lansium volatile oil microcapsule powder according to claim 7, wherein in the step (1), the stirring time is 20-30 min; in the step (3), the stirring speed is 10000-30000rpm, and the stirring time is 20-40 min.
9. The method for preparing the clausena lansium volatile oil microcapsule powder according to claim 7, wherein in the step (4), the homogenizing pressure is 20-40MPa, the homogenizing times are 2-3 times, and the temperature is 50-60 ℃; the air inlet temperature of the spray drying is 160-180 ℃, and the air outlet temperature of the spray drying is 80-85 ℃.
10. The clausena lansium volatile oil microcapsule powder according to any one of claims 1 to 3, wherein the glass transition temperature of the clausena lansium volatile oil microcapsule powder is 80 ℃ or higher.
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| CN114868922A (en) * | 2022-05-23 | 2022-08-09 | 新疆农垦科学院 | Pumpkin seed oil microcapsule and preparation method thereof |
| CN115337880A (en) * | 2022-07-15 | 2022-11-15 | 纽斯葆广赛（广东）生物科技股份有限公司 | Pumpkin seed oil microcapsule and preparation method and application thereof |
| CN115399465A (en) * | 2022-07-15 | 2022-11-29 | 可菲生物科技有限公司 | Preparation method of clausena lansium-flavored microcapsule powder essence |
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| CN114868922B (en) * | 2022-05-23 | 2023-08-18 | 新疆农垦科学院 | Pumpkin seed oil microcapsule and preparation method thereof |
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| CN115399465A (en) * | 2022-07-15 | 2022-11-29 | 可菲生物科技有限公司 | Preparation method of clausena lansium-flavored microcapsule powder essence |
| CN115337880B (en) * | 2022-07-15 | 2024-06-04 | 纽斯葆广赛（广东）生物科技股份有限公司 | Pumpkin seed oil microcapsule and preparation method and application thereof |
| CN115812939A (en) * | 2022-12-29 | 2023-03-21 | 晨光生物科技集团股份有限公司 | Zanthoxylum oil microcapsule and preparation method thereof |
| CN115812939B (en) * | 2022-12-29 | 2024-04-26 | 晨光生物科技集团股份有限公司 | Zanthoxylum oil microcapsule and preparation method thereof |
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