CN109317066B - Myristica fragrans essential oil microcapsule and preparation method and application thereof - Google Patents
Myristica fragrans essential oil microcapsule and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to the technical field of microcapsules and discloses a nutmeg essential oil microcapsule as well as a preparation method and application thereof. The nutmeg essential oil microcapsule comprises starch octenyl succinate, inulin and nutmeg essential oil. According to the invention, unconventional inulin is selected as one of wall materials to be matched with octenyl succinic acid starch ester to prepare the myristica fragrans essential oil microcapsule, so that the microcapsule has good thermal stability and higher encapsulation rate and essential oil retention rate; in addition, the special fluidized drying process is matched, so that the flowability of the product can be further improved, the product has smaller particle size and concentrated particle size distribution range, and the utilization rate of the product is improved.
Description
Technical Field
The invention relates to the technical field of microcapsules, and particularly relates to a nutmeg essential oil microcapsule as well as a preparation method and application thereof.
Background
Myristica fragrans Houtt (Myristica fragrans Houtt) is dry kernel of Myristica fragrans Houtt, and is clinically used for treating deficiency-cold of spleen and stomach, chronic diarrhea, abdominal pain, anorexia and emesis. Nutmeg mainly contains 8-15% of essential oil and 25-46% of fatty oil, is used as a natural spice which is widely applied internationally and is also an edible spice which is allowed to be used in the stipulation of GB2760-2014 food additive use standard in China, and the nutmeg essential oil and the oleoresin are mainly used in bread, biscuits, cakes, potato chips, curry powder, sauce and the like, and the application range is gradually expanded, and the using amount is also increased year by year. In addition, the nutmeg essential oil has shown a certain application prospect in the aspects of antioxidation, free radical removal, food additives and the like. However, nutmeg essential oil has poor stability, pungent odor, poor water solubility, and is easily oxidized and decomposed by light and heat, thereby seriously affecting the efficacy of nutmeg.
In order to improve the utilization rate and stability of nutmeg essential oil, the microcapsule technology is widely used as a commonly used technology. The microcapsule is a spherical or spheroidal microcapsule formed by wrapping a solid or liquid drug (to be a core material or a core material) by using a natural or synthetic polymer material (collectively referred to as a capsule material or a wall material) as a capsule membrane. If the drug is dissolved and/or highly dispersed in the polymer material to form skeleton-type microparticles, the microspheres are called. The diameter of the microcapsule and microsphere is 1-250 μm, and belongs to micrometer range, or microparticle (the particle diameter of 10-100 nm is called nanoparticle, and belongs to colloid range).
The microcapsule technology isolates the core material from the external environment and can resist the action of oxygen and light; volatile substances can be protected, and the bad smell of some core materials can be shielded; the physical properties (including color, shape, density and dispersion performance), chemical properties and the like of the core material are changed, so that the storage and the use are convenient, and the selection of the microcapsule wall material has a crucial influence on the performance.
There are some reports on "essential oils" and "microcapsules". "an antibacterial PVC wallpaper base paper containing nutmeg oil microcapsule and preparation method thereof (CN 201410672406.4)" uses wild chrysanthemum flower water extract, polycarboxylic acid water reducing agent, polyhexamethylene guanidine, nutmeg oil, coniferous full bleaching chemical wood pulp, broadleaf eucalyptus wood pulp, polyamide epichlorohydrin resin, 600-plus 800-mesh calcium carbonate whisker, Arabic gum, polyethylene glycol, white carbon black, 800-plus 1250-mesh environment-friendly pigment and the like as raw materials to prepare nutmeg oil microcapsule wallpaper; "a method for preparing nutmeg oil microcapsule (CN201110289961.5) by using ultrasonic wave" uses beta-cyclodextrin as wall material, and obtains nutmeg oil microcapsule by ultrasonic wave, freeze drying; "an essential oil microcapsule and its preparation method (CN 201610969058.6)" uses maltodextrin and/or maltose syrup, whey protein isolate and/or soy protein isolate as wall material to prepare essential oil microcapsule, the embedding rate is greater than 90%; an essential oil microcapsule and a preparation method thereof (CN201510158355.8) uses wall materials and an emulsifier to prepare the lemongrass essential oil microcapsule under the condition of oxygen isolation, the oil content can reach more than 10 percent, and the yield is more than 60 percent; "a method for producing sea buckthorn polysaccharide microcapsule (CN 201410017305.3)" uses sodium octenyl succinate and beta-cyclodextrin to embed sea buckthorn polysaccharide, the embedding rate is 88.63%; a composite microcapsule wall material and application thereof in essence microcapsules for cigarettes (CN201310319279.5) are prepared by compounding wall materials such as octenyl succinate starch, maltodextrin, sodium carboxymethyl starch, isolated soy protein, Arabic gum, sodium caseinate, sucrose, sodium alginate, xanthan gum, pullulan and the like, and the microcapsule has good sensory property and stronger practicability.
The existing microcapsule technology generally adopts more wall materials and auxiliary materials, and although the materials can successfully microencapsulate the core material, the final product still has defects in particle size, fluidity, encapsulation efficiency and essential oil retention rate. Furthermore, spray drying is the most common granulation technique in the prior art microencapsulation technique, but this method also has a negative effect on the quality of the product.
Disclosure of Invention
In view of the above, the present invention aims to provide a myristica fragrans essential oil microcapsule, which has good thermal stability, and has high encapsulation efficiency and essential oil retention rate;
another object of the present invention is to provide a myristica fragrans essential oil microcapsule, which allows the microcapsule to have better fluidity;
another object of the present invention is to provide a nutmeg essential oil microcapsule, which has a small particle size and a concentrated particle size distribution range;
another object of the present invention is to provide a preparation method of the above nutmeg essential oil microcapsule and related applications of the microcapsule in medicines and/or foods.
In order to achieve the above purpose, the invention provides the following technical scheme:
a microcapsule containing semen Myristicae essential oil comprises starch octenyl succinate, inulin and semen Myristicae essential oil.
Compared with the conventional wall material type, the microcapsule for preparing the nutmeg essential oil by using the starch octenyl succinate and the inulin as the wall materials can obviously improve the encapsulation rate and retention rate of the nutmeg essential oil.
Preferably, the mass ratio of the starch octenyl succinate ester to the inulin is (1-2) to 1; in a particular embodiment of the invention, the mass ratio of starch octenyl succinate and inulin is 1.5:1 or 1:1, wherein said 1.5:1 also comprises a ratio approximately equal to 1.5:1 according to the rounding principle, such as 14.5:9.7 and 18.5: 12.3; in addition, the mass ratio of the present invention can be embodied in any unit of mass, such as g, kg, mg, jin, kg, parts by weight, and the like, and more specifically, the following can be referred to:
(1) 16.2g of starch octenyl succinate and 10.8g of inulin, wherein the mass ratio of the two is 1.5: 1;
(2) 10g of starch octenyl succinate, 10g of inulin or 11.5g of starch octenyl succinate and 11.5g of inulin, wherein the mass ratio of the two is 1: 1;
(3) 14.5g of starch octenyl succinate, 9.7g of inulin or 18.5g of starch octenyl succinate and 12.3g of inulin, wherein the mass ratio of the two is approximately equal to 1.5: 1.
Preferably, the mass of the nutmeg essential oil is 20-50% of the total mass of the starch octenyl succinate and the inulin; in specific embodiments, the mass of the nutmeg essential oil can be selected to be 29.6% (also 8/27), 50%, 45% (also 10.9/24.2), 29.9% (also 9.2/30.8), or 30% of the total mass of octenyl starch succinate and inulin.
Compared with common starch octenyl succinate and maltodextrin, the encapsulation rate of the invention can reach more than 95 percent and can reach 99.4 percent to the maximum, and the retention rate of the essential oil is more than 75 percent and can reach about 85 percent to the maximum; the encapsulation rate of the conventional wall material type is only about 92%, and the retention rate of the essential oil is only about 65%. Meanwhile, the microcapsule has good thermal stability.
Based on the excellent technical effects, the invention provides the application of the microcapsule in preparing food and/or medicines. According to the application of the nutmeg essential oil, the application of the microcapsule in food and/or medicine is selected from one or more of additives, perfumes, antioxidant ingredients and free radical scavenging ingredients.
Meanwhile, the invention also provides a preparation method of the microcapsule, wherein the preparation method generally comprises the steps of firstly preparing the emulsion, and then granulating by a spray drying method or a boiling drying method to obtain the microcapsule.
The process steps of granulation by a spray drying method are as follows:
and 2, granulating by using an emulsion spray drying method to obtain the nutmeg essential oil microcapsule.
Wherein the spray drying conditions can be carried out according to conventional conditions, and in the specific embodiment of the invention, the spray drying conditions are as follows: the spraying pressure is 0.3MPa, the air inlet temperature is 170 ℃, the air outlet temperature is 60 ℃, and the feeding speed is 16 mL/min; or the spraying pressure is 0.3MPa, the air inlet temperature is 185 ℃, the air outlet temperature is 108 ℃, and the feeding flow is 32 mL/min.
The process steps of granulating by a boiling drying method are as follows:
and 2, granulating the emulsion by using the residual inulin as a granulating material through a boiling drying method to obtain the nutmeg essential oil microcapsule.
In the process of granulation by a boiling drying method, the spray drying method of conventional granulation is replaced by the boiling drying method, inulin of one wall material is divided into two parts, one part is used for preparing emulsion, and the other part is used as a granulating material of the boiling drying method.
Preferably, the part of inulin (referred to as inulin for preparing the emulsion) is 20-30% of the total mass of the inulin; in a particular embodiment, the portion of inulin is from 24 to 26% of the total mass of inulin, more particularly 25%, 24.74% (also 2.4/9.7), 25.20% (also 3.1/12.3) or 25.12% (also 2.9/11.5).
Preferably, step 1 of the process of granulation by the fluidized drying method is as follows:
dissolving starch octenylsuccinate in water, adding part of inulin under magnetic stirring at 300-500rpm and 40-60 ℃, cooling to room temperature after full dissolution, adding essential oil, and homogenizing at 6000-15000rpm for 2-4 cycles with high-speed shearing for 30-90s and 30-80mbar to obtain uniform emulsion. Wherein the rotation speed of the magnetic stirring can be 300rpm, 400rpm or 500rpm, and the temperature of the magnetic stirring can be 40 ℃, 50 ℃ or 60 ℃; the high-speed shearing rotating speed can be 6000rpm, 8000rpm or 10000rpm, and the high-speed shearing time can be 30s, 60s or 80 s; the homogenising pressure may be 30mbar, 40mbar, 50mbar or 60mbar and the number of homogenising cycles may be 2, 3 or 4 cycles;
in addition, under the conditions of the boiling drying method of the invention, microcapsules with better fluidity and particle size can be obtained:
the atomization pressure is 1.8bar, the air inlet temperature is 100-120 ℃, the air outlet temperature is 45-55 ℃, and the feeding speed is 10-20 mL/min. Wherein the air inlet temperature can be 100 ℃, 110 ℃, 115 ℃ or 120 ℃, the air outlet temperature can be 45 ℃, 50 ℃ or 55 ℃, and the feeding speed can be 14mL/min, 15mL/min, 16mL/min or 18 mL/min.
According to the technical scheme, unconventional inulin is selected as one of the wall materials to be matched with starch octenyl succinate to prepare the nutmeg essential oil microcapsule, so that the microcapsule has good thermal stability and high encapsulation rate and essential oil retention rate; in addition, the special fluidized drying process is matched, so that the flowability of the product can be further improved, the product has smaller particle size and concentrated particle size distribution range, and the utilization rate of the product is improved.
Drawings
FIG. 1 is a scanning electron micrograph of a microcapsule according to example 1;
FIG. 2 is a line graph showing the change of the mass of the original essential oil after being placed in an oven at 40 ℃ for 12 hours;
FIG. 3 is a line graph showing the change in mass of the essential oil of example 1 when placed in an oven at 40 ℃ for 12 hours;
FIG. 4 is a bar graph showing the change of the content of components after the essential oil is left in an oven at 40 ℃ for 12 hours; wherein bar A represents the 0h component content bar, bar B represents the 12h component content bar, 1-14 correspond to Table 1 components;
FIG. 5 is a bar graph showing the change in the content of components after the microencapsulated essential oil of example 1 is left in an oven at 40 ℃ for 12 hours; wherein bar A represents the 0h component content bar, bar B represents the 12h component content bar, 1-14 correspond to the components of Table 1;
fig. 6 shows a scanning electron microscope image of octenyl succinic acid starch ester/maltodextrin for preparing nutmeg essential oil microcapsule.
Detailed Description
The invention discloses a nutmeg essential oil microcapsule and a preparation method and application thereof, and a person skilled in the art can realize the microcapsule by properly improving process parameters by referring to the content. It is expressly intended that all such similar substitutes and modifications which would be obvious to one skilled in the art are deemed to be included in the invention. While the microcapsules of the present invention and methods of making and using the same have been described in terms of examples, it will be apparent to those of ordinary skill in the art that the techniques of the present invention may be practiced and used with modification, or with appropriate modification, and combinations of the methods and uses described herein without departing from the spirit, scope, and concept of the invention.
Unless otherwise specified, the nutmeg essential oil and the wall material raw materials used in the embodiments of the present invention all use raw materials with the same source and quality, and the preparation process and the test conditions are consistent except for the differences.
The nutmeg essential oil microcapsule provided by the invention, the preparation method and the application thereof are further explained below.
Example 1: preparing the nutmeg essential oil microcapsule
1) Selecting raw materials: selecting 16.2g of octenyl succinic acid starch ester, 10.8g of inulin and 8.0g of nutmeg essential oil for later use;
2) preparation of the emulsion: dissolving starch octenylsuccinate in water, adding 2.7g of inulin under magnetic stirring, fully dissolving, cooling to room temperature, adding essential oil, shearing at high speed, and homogenizing to obtain uniform emulsion;
the magnetic stirring condition is 300rpm and 50 ℃;
the high-speed shearing conditions are as follows: 10000rpm,60 s;
the homogenization conditions are as follows: 60mbar,2 cycles;
3) preparing microcapsules: granulating by an emulsion fluidized drying method, setting a proper feeding speed, keeping the feeding temperature and the air outlet temperature, and adding the residual 8.1g of inulin as a granulating material to obtain nutmeg essential oil microcapsules;
the conditions of the boiling drying method are as follows: the atomization pressure is 1.8bar, the air inlet temperature is 100 ℃, the air outlet temperature is 45 ℃, and the feeding speed is 14 mL/min;
the embedding rate of the prepared nutmeg essential oil microcapsule is 99.4%, the retention rate of the essential oil is 85.2%, and the nutmeg essential oil microcapsule has a compact surface, is regular and round and has no viscosity and a particle size of 1-4 μm as shown in figure 1 through observation of a scanning electron microscope.
Example 2: preparing the nutmeg essential oil microcapsule
1) Selecting raw materials: selecting 10g of octenyl succinic acid starch ester, 10g of inulin and 10g of nutmeg essential oil for later use;
2) preparation of the emulsion: dissolving starch octenylsuccinate in water, adding 2.5g of inulin under magnetic stirring, fully dissolving, cooling to room temperature, adding essential oil, shearing at high speed, and homogenizing to obtain uniform emulsion;
the magnetic stirring condition is 500rpm and 60 ℃;
the high-speed shearing conditions are as follows: 8000rpm,80 s;
the homogenization conditions are as follows: 40mbar,3 cycles;
3) preparing microcapsules: granulating by an emulsion fluidized drying method, setting a proper feeding speed, keeping the feeding temperature and the air outlet temperature, and adding the rest 7.5g of inulin as a granulating material to obtain nutmeg essential oil microcapsules;
the conditions of the boiling drying method are as follows: the atomization pressure is 1.8bar, the air inlet temperature is 110 ℃, the air outlet temperature is 50 ℃, and the feeding speed is 18 mL/min;
the embedding rate of the prepared nutmeg essential oil microcapsule is 98.6%, the retention rate of the essential oil is 80.4%, and the nutmeg essential oil microcapsule has a compact surface, is regular and round and has no viscosity and a particle size of 1-4 microns through the observation of a scanning electron microscope.
Example 3: preparing the nutmeg essential oil microcapsule
1) Selecting raw materials: selecting 14.5g of octenyl succinic acid starch ester, 9.7g of inulin and 10.9g of nutmeg essential oil for later use;
2) preparation of the emulsion: dissolving starch octenylsuccinate in water, adding 2.4g of inulin under magnetic stirring, fully dissolving, cooling to room temperature, adding essential oil, shearing at high speed, and homogenizing to obtain uniform emulsion;
the magnetic stirring condition is 300rpm and 40 ℃;
the high-speed shearing conditions are as follows: 10000rpm,30 s;
the homogenization conditions are as follows: 60mbar,2 cycles;
3) preparing microcapsules: granulating by an emulsion fluidized drying method, setting a proper feeding speed, keeping the feeding temperature and the air outlet temperature, and adding the rest 7.3g of inulin as a granulating material to obtain nutmeg essential oil microcapsules;
the conditions of the boiling drying method are as follows: the atomization pressure is 1.8bar, the air inlet temperature is 115 ℃, the air outlet temperature is 55 ℃, and the feeding speed is 16 mL/min;
the embedding rate of the prepared nutmeg essential oil microcapsule is 97.0%, the retention rate of the essential oil is 78.1%, and the nutmeg essential oil microcapsule has a compact surface, is regular and round and has no viscosity and a particle size of 1-4 microns through the observation of a scanning electron microscope.
Example 4: preparing the nutmeg essential oil microcapsule
1) Selecting raw materials: selecting 18.5g of octenyl succinic acid starch ester, 12.3g of inulin and 9.2g of nutmeg essential oil for later use;
2) preparation of the emulsion: dissolving starch octenylsuccinate in water, adding 3.1g of inulin under magnetic stirring, fully dissolving, cooling to room temperature, adding essential oil, shearing at high speed, and homogenizing to obtain uniform emulsion;
the magnetic stirring condition is 500rpm and 50 ℃;
the high-speed shearing conditions are as follows: 6000rpm,80 s;
the homogenization conditions are as follows: 30mbar,3 cycles;
3) preparing microcapsules: granulating by an emulsion fluidized drying method, setting a proper feeding speed, keeping the feeding temperature and the air outlet temperature, and adding the rest 9.2g of inulin as a granulating material to obtain nutmeg essential oil microcapsules;
the conditions of the boiling drying method are as follows: the atomization pressure is 1.8bar, the air inlet temperature is 100 ℃, the air outlet temperature is 50 ℃, and the feeding speed is 15 mL/min;
the embedding rate of the prepared nutmeg essential oil microcapsule is 97.2%, the retention rate of the essential oil is 77.8%, and the nutmeg essential oil microcapsule has a compact surface, is regular and round and has no viscosity and a particle size of 1-4 microns through the observation of a scanning electron microscope.
Example 5: preparing the nutmeg essential oil microcapsule
1) Selecting raw materials: selecting 11.5g of octenyl succinic acid starch ester, 11.5g of inulin and 6.9g of nutmeg essential oil for later use;
2) preparation of the emulsion: dissolving starch octenylsuccinate in water, adding 2.9g of inulin under magnetic stirring, fully dissolving, cooling to room temperature, adding essential oil, shearing at high speed, and homogenizing to obtain uniform emulsion;
the magnetic stirring condition is 500rpm and 60 ℃;
the high-speed shearing conditions are as follows: 8000rpm,60 s;
the homogenization conditions are as follows: 50mbar,2 cycles;
3) preparing microcapsules: granulating by an emulsion fluidized drying method, setting a proper feeding speed, keeping the feeding temperature and the air outlet temperature, and adding the residual 8.6g of inulin as a granulating material to obtain nutmeg essential oil microcapsules;
the conditions of the boiling drying method are as follows: the atomization pressure is 1.8bar, the air inlet temperature is 120 ℃, the air outlet temperature is 55 ℃, and the feeding speed is 16 mL/min;
the embedding rate of the prepared nutmeg essential oil microcapsule is 95.4%, the retention rate of the essential oil is 80.3%, and the nutmeg essential oil microcapsule has a compact surface, is regular and round and has no viscosity and a particle size of 1-4 microns through the observation of a scanning electron microscope.
Example 6: preparing the nutmeg essential oil microcapsule
1) Selecting raw materials: selecting 15.3g of octenyl succinic acid starch ester, 7.7g of inulin and 6.9g of nutmeg essential oil for later use;
2) preparation of the emulsion: dissolving starch octenylsuccinate in water, adding 7.7g of inulin under magnetic stirring, fully dissolving, cooling to room temperature, adding essential oil, shearing at high speed, and homogenizing to obtain uniform emulsion;
the magnetic stirring condition is 500rpm and 40 ℃;
the high-speed shearing conditions are as follows: 8000rpm,60 s;
the homogenization conditions are as follows: 50mbar,2 cycles;
3) preparing microcapsules: carrying out conventional spray drying on the emulsion to obtain nutmeg essential oil microcapsules;
the conditions of the conventional spray drying are as follows: the spraying pressure is 0.3MPa, the air inlet temperature is 170 ℃, the air outlet temperature is 60 ℃, and the feeding speed is 16 mL/min.
The embedding rate of the prepared nutmeg essential oil microcapsule is 96.0 percent, and the retention rate of the essential oil is 77.7 percent. However, the microcapsules had a powder with a high viscosity and slightly agglomerated particles, a Carl index of 36.55%, and poor powder flowability (the particles were more flowable when the Carl index was less than 25%).
Example 7: comparison of stability before and after microencapsulation of nutmeg essential oil
The original essential oil and the microencapsulated essential oil of example 1 were stored at a constant temperature in an electric heating blower at 40 ℃, sampled every 2 hours for measurement, and measured for thermal stability by a constant weight method, and the results are shown in tables 1 to 3 and fig. 2 to 5.
Table 1 original essential oil composition and relative content (%)
TABLE 2 composition and relative content (%)
Table 3 components and their relative contents (%) -of microencapsulated essential oils measured after 12h in an oven at 40 ℃
Tables 1 to 3 and FIGS. 2 to 5 show that the original essential oil was reduced in mass to 60% or less after 2 hours and slowly volatilized after 2 hours, from the change of the total mass and the components. After 12 hours, the alpha-pinene almost completely volatilizes, and the loss of the alpha-pinene after microencapsulation is obviously reduced. It is clear that the stability of the essential oil is significantly improved after microencapsulation.
Example 8: statistics of encapsulation and retention of essential oils for nutmeg essential oil for other processes
1) Selecting raw materials: selecting 18.5g of octenyl succinic acid starch ester, 12.3g of maltodextrin and 9.2g of nutmeg essential oil for later use;
2) preparation of the emulsion: dissolving starch octenylsuccinate in water, adding 3.1g of maltodextrin under magnetic stirring, fully dissolving, cooling to room temperature, adding essential oil, shearing at high speed, and homogenizing to obtain uniform emulsion;
the magnetic stirring condition is 500rpm and 50 ℃;
the high-speed shearing conditions are as follows: 6000rpm,80 s;
the homogenization conditions are as follows: 30mbar,3 cycles;
3) preparing microcapsules: granulating by an emulsion fluidized drying method, setting a proper feeding speed, keeping the feeding temperature and the air outlet temperature, and adding the rest 9.2g of maltodextrin as a granulating material to obtain nutmeg essential oil microcapsules;
the conditions of the boiling drying method are as follows: the atomization pressure is 1.8bar, the air inlet temperature is 100 ℃, the air outlet temperature is 50 ℃, and the feeding speed is 15 mL/min;
the embedding rate of the prepared nutmeg essential oil microcapsule is 92.2 percent, and the retention rate of the essential oil is 65.8 percent.
According to the process conditions, the comparison process of the embodiment is different from the process of the embodiment 4 only in the types of wall materials, the microcapsule encapsulation rate taking the starch octenyl succinate and the inulin as the wall materials is high, the retention rate of essential oil is high, and the product has the health-care function of the inulin.
Example 9: comparison of fluidity and powder characteristics of nutmeg essential oil microcapsules of different processes
The process of example 6 compares the fluidity of spray drying, granulation by the fluidized drying method and the difference between the use modes of inulin, and proves that the fluidity of the microcapsules can be improved under the fluidized drying process conditions of the invention. On the basis, the embodiment further provides the flowability and the powder characteristics of the product compared with the comparison process and the process of the invention.
1. Comparative example Process
Wall material: nutmeg essential oil 1:4, starch sodium octenyl succinate in wall material: maltodextrin 10 g: 10g
Adding the wall material into ultrapure water, heating and stirring at 90 ℃ to dissolve the wall material to obtain a wall material aqueous solution; wherein the mass concentration of the composite wall material aqueous solution is 10 percent;
adding semen Myristicae essential oil into the wall material water solution, and shearing at a high speed of 20000r/min for 2min to obtain primary emulsion; wherein the mass ratio of the composite wall material to the nutmeg essential oil is 1: 4; homogenizing the obtained primary emulsion at 60 deg.C under high pressure of 300Bar for 1 time to obtain uniform and stable final emulsion;
and (3) spray-drying the homogenized final emulsion to obtain nutmeg essential oil microcapsule powder (shown in a scanning electron microscope figure 6), wherein the spray pressure during spray-drying treatment is 0.3MPa, the air inlet temperature is 185 ℃, the air outlet temperature is 108 ℃, and the feed flow is 32 mL/min.
2. Determination of the Carr index:
taking a sample with a certain mass m (10g), placing the sample in a 100mL measuring cylinder, slightly scraping, reading the volume V0, oscillating the measuring cylinder until the volume of the powder does not change, and reading the volume VfThe measurement was repeated three times to calculate the bulk density D0And tap density DfAnd then:
D0＝m/V0Df＝m/Vf
carr index (Carr index) ═ Df-D0)/Df×100％
3. And (3) moisture determination:
the measurement is carried out according to the method of GB50093-2010 determination of moisture in food. Placing a small clean aluminum box in a 105 ℃ oven, supporting the box edge with an inclined cover, heating for 1h, taking out, placing in a dryer, and cooling for 0.5 h. Weighing, and repeatedly drying until the mass difference between the front and the back is not more than 2mg, namely the constant weight m of the aluminum small box3。
Weighing 2 g-5 g of sample (accurate to 0.0001g), placing into the aluminum capsule, and weighing m1And if the thickness of the sample is not more than 5mm, if the sample is loose, the thickness is not more than 10mm, the sample is covered, the sample is precisely weighed, the sample is placed in a drying box at the temperature of 101-105 ℃, a bottle cover is obliquely supported at the edge of the bottle, the sample is taken out after being dried for 2-4 h, and the sample is placed in a dryer and cooled for 0.5h and then weighed. Then the mixture is put into a drying oven with the temperature of 101-105 ℃ for drying for about 1h, taken out and put into a dryer for cooling for 0.5h, and then weighed. Repeating the above steps until the mass difference between the two times is not more than 2mg, thus obtaining the constant weight m2. The moisture content is then:
X＝(m1-m2)/(m1-m3)×100
x-moisture content in the sample in grams per hundred grams (g/100 g);
m1the mass of the aluminum capsule and the sample in grams (g);
m2the mass of the aluminum capsule and the sample after drying is given in grams (g);
m3the mass of the aluminum capsule in grams (g).
When the water content is more than or equal to 1g/100g, three effective digits are reserved in the calculation result; at a moisture content of < 1g/100g, two significant figures are retained.
4. Measurement of angle of repose (funnel method):
a diameter is 6 cm's culture dish is put to the bottom, and the funnel is fixed on the iron stand platform, makes the distance between funnel and the culture dish be 10cm, weighs powder 10g, falls the powder from the funnel top, piles up in the culture dish after the buffering of funnel gradually, forms the cone. Until the highest cone is obtained, the height of the cone is measured as h, and the radius of the cone base circle r. The angle of repose α was determined, and the average was obtained by repeating the procedure three times. The calculation formula is as follows:
tanα＝h/r
5. results
TABLE 4 powder Properties of microencapsulated nutmeg essential oil powder
The powder characteristics of the essential oil microencapsulated product can be seen as follows: the powder obtained by the process of the invention has moderate viscosity, uniform particles, average particle size of less than 4 mu m and water content basically kept about 3 percent. The powder has better Karl index and repose angle, is easier to form and has better fluidity.
The essential oil microencapsulated product prepared by the comparative example process has the advantages of high powder viscosity, fine particles, high average particle size of 3-6 mu m, obviously poor powder Carl index and angle of repose, difficulty in forming and poor flowability.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (7)
1. The nutmeg essential oil microcapsule is characterized by consisting of starch octenyl succinate, inulin and nutmeg essential oil, wherein the mass ratio of the starch octenyl succinate to the inulin is (1-2):1, and the mass of the nutmeg essential oil is 20-50% of the total mass of the starch octenyl succinate and the inulin;
the microcapsule is prepared according to the following steps:
step 1, taking octenyl succinic acid starch ester, partial inulin and nutmeg essential oil, shearing and homogenizing to obtain uniform emulsion;
and 2, granulating the emulsion by using the residual inulin as a granulating material through a boiling drying method to obtain the nutmeg essential oil microcapsule.
2. Use of microcapsules according to claim 1 for the preparation of a food and/or pharmaceutical product.
3. Use according to claim 2, wherein the microcapsules are used in food and/or pharmaceutical products selected from one or more of as an additive, as a fragrance, as an antioxidant ingredient, as a free radical scavenging ingredient.
4. A process for the preparation of microcapsules according to claim 1, comprising:
step 1, taking octenyl succinic acid starch ester, partial inulin and nutmeg essential oil, shearing and homogenizing to obtain uniform emulsion;
and 2, granulating the emulsion by using the residual inulin as a granulating material through a boiling drying method to obtain the nutmeg essential oil microcapsule.
5. The method according to claim 4, wherein the step 1 is:
dissolving starch octenylsuccinate in water, adding part of inulin under magnetic stirring at 300-500rpm and 40-60 ℃, cooling to room temperature after full dissolution, adding essential oil, and homogenizing at 6000-15000rpm for 2-4 cycles with high-speed shearing for 30-90s and 30-80mbar to obtain uniform emulsion.
6. The production method according to claim 4 or 5, wherein the partial inulin accounts for 20 to 30% of the total mass of the inulin.
7. The preparation method according to claim 4, wherein the conditions of the fluidized drying method are as follows:
the atomization pressure is 1.8bar, the air inlet temperature is 100-120 ℃, the air outlet temperature is 45-55 ℃, and the feeding speed is 10-20 mL/min.
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| CN111990475A (en) * | 2020-07-31 | 2020-11-27 | 中国科学院天津工业生物技术研究所 | Lycium seed oil microcapsule rich in lycium erythrophyll and preparation method thereof |
| CN113016864B (en) * | 2021-04-20 | 2023-11-28 | 甘肃农业大学 | Preparation method of jerky preservative |
| CN113171737A (en) * | 2021-04-26 | 2021-07-27 | 深圳市真味生物科技有限公司 | Melon essence microcapsule and melon-flavored electronic atomized liquid |
| CN113730299B (en) * | 2021-08-06 | 2023-06-02 | 广州市芳香时代进出口有限公司 | Preparation process of essential oil microcapsule containing essential oil |
| CN114869847B (en) * | 2022-03-31 | 2023-07-28 | 中国热带农业科学院分析测试中心 | Semen katsumadai essential oil microemulsion and preparation method thereof |
| CN116492944B (en) * | 2023-06-21 | 2023-09-29 | 云南省农业科学院农产品加工研究所 | Microcapsule wall material and preparation method and application thereof |
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