CN109317066A - A kind of nutmeg essential oil microcapsules and its preparation method and application - Google Patents
A kind of nutmeg essential oil microcapsules and its preparation method and application Download PDFInfo
- Publication number
- CN109317066A CN109317066A CN201710647284.7A CN201710647284A CN109317066A CN 109317066 A CN109317066 A CN 109317066A CN 201710647284 A CN201710647284 A CN 201710647284A CN 109317066 A CN109317066 A CN 109317066A
- Authority
- CN
- China
- Prior art keywords
- essential oil
- microcapsules
- inulin
- nutmeg
- preparation
- 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
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
- B01J13/043—Drying and spraying
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/5005—Wall or coating material
- A61K9/5021—Organic macromolecular compounds
- A61K9/5036—Polysaccharides, e.g. gums, alginate; Cyclodextrin
-
- 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
Landscapes
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Alternative & Traditional Medicine (AREA)
- Wood Science & Technology (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Medical Informatics (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Dispersion Chemistry (AREA)
- Medicinal Preparation (AREA)
- Cosmetics (AREA)
- General Preparation And Processing Of Foods (AREA)
Abstract
The present invention relates to microcapsules technology field, a kind of nutmeg essential oil microcapsules and its preparation method and application are disclosed.Nutmeg essential oil microcapsules of the present invention include starch octenyl succinate anhydride, inulin and nutmeg essential oil.The present invention selects unconventional inulin to prepare nutmeg essential oil microcapsules as one of wall material and starch octenyl succinate anhydride, so that the microcapsules have good thermal stability and higher encapsulation rate and essential oil retention rate；The distinctive fluid-bed drying technique of this fit on, can be further improved the mobility of product, is the particle size distribution range that product has smaller particle and concentration, improves the utilization rate of product.
Description
Technical field
The present invention relates to microcapsules technology fields, and in particular to a kind of nutmeg essential oil microcapsules and preparation method thereof and answers
With.
Background technique
Nutmeg is the drying kernel of myristicaceae plant nutmeg (MyristicafragransHoutt), and clinic is common
In deficiency-cold in spleen and stomach, endless diarrhea, abdominal distention, deficiency of food vomiting.Nutmeg mainly contains essential oil (8%~15%) and fat oil
(25%~46%), as a kind of natural perfume material widely used in the world and China's GB2760-2014 " food additives
Use standard " regulation allow using flavorant, nutmeg essential oil and oleoresin are mainly used for bread, biscuit, cake, potato
In piece, curry powder, sauce etc., and application range is growing, and dosage also increases year by year.In addition to this, nutmeg essential oil exists
Antioxidation, removing free radical, food additives etc. have also had shown that certain application prospect.But nutmeg essential oil is steady
Qualitative poor, irritant smell, poorly water-soluble meets light, the oxidizable decomposition of heat, to seriously affect myristic effect.
In order to improve the utilization rate and stability of nutmeg essential oil, microcapsules technology is answered extensively as common technology
With.Solid-state or liquid are wrapped up using natural or synthesis high molecular material (being referred to as capsule material or wall material) as cyst membrane by micro-capsule system
Drug (becoming capsule core material or core material) forms spherical or spherical tiny capsules.If drug is dissolved and (or) is highly dispersed at
In high molecular material, matrix type particle is formed, then referred to as microballoon.The partial size of micro-capsule and microballoon belongs to micro- between 1-250 microns
Meter level scope, and it is referred to as particle (particle of the partial size within the scope of 10nm-100nm is then known as nanoparticle, belongs to colloid scope).
Microcapsules technology isolates core material with external environment, can resist the effect of oxygen, light；It can protect volatility
Substance covers the bad smell of some core materials；Change physical property (including color, shape, density, the dispersibility of core material
Can), chemical property etc., convenient for storage and use, and the selection of microcapsule wall material has vital shadow to these performances height
It rings.
About the patent of " essential oil " and " microcapsules ", there are reports at present.It is " a kind of anti-containing myristica oil microcapsule
Bacterial type PVC wallpaper body paper and preparation method thereof (CN201410672406.4) " with wild chrysanthemum water extract, polycarboxylate water-reducer,
Polyhexamethylene guanide, mace oil, needle float chemical wood pulp, broad-leaved eucalyptus pulp, polyamine epichlorohydrin resin, 600- entirely
800 mesh calcium carbonate crystal whiskers, Arabic gum, polyethylene glycol, white carbon black, 800-1250 mesh environmental-friendly pigment etc. are that raw material prepares nutmeg
Oil microcapsule wallpaper；" a kind of method (CN201110289961.5) using ultrasonic wave preparation myristica oil microcapsule " is with β-ring
Dextrin is wall material, by ultrasound, is freeze-dried to obtain myristica oil microcapsule；A kind of " essential oil microcapsules and preparation method thereof
(CN201610969058.6) " using maltodextrin and/or malt syrup, whey protein isolate and/or soybean protein isolate as wall
Material prepares essential oil microcapsules, and embedding rate is greater than 90%；A kind of " essential oil microcapsules and preparation method thereof
(CN201510158355.8) " lemon grass (Cymbopogon citratus) essential oil microcapsules, oil content are prepared under the conditions of starvation with wall material and emulsifier
Up to 10% or more, yield is 60% or more；" a kind of production method (CN201410017305.3) of Fructus Hippophae polysaccharide microcapsules "
Fructus Hippophae polysaccharide, embedding rate 88.63% are embedded using octenyl succinate sodium and beta-cyclodextrin；A kind of " Compositional type microcapsules
Wall material and its application (CN201310319279.5) in flavouring essence for tobacco microcapsules " is with starch octenylsuccinate, wheat
Bud dextrin, soybean protein isolate, Arabic gum, casein sodium, sucrose, sodium alginate, xanthan gum, is grown sturdily at sodium carboxymethyl starch
The compounding wall material such as mould polysaccharide prepares microcapsules, and product sensory is functional, has stronger practicability.
Above-mentioned existing microcapsules technology has generallyd use more wall material and auxiliary material, though these substances can by core material at
Function microencapsulation, but final product is on partial size, mobility, encapsulation rate and essential oil retention rate that there are still deficiencies.In addition, existing
In microencapsulation spray drying be most common granulating technique, but this kind of method equally have to the quality of the said goods it is unfavorable
It influences.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of nutmeg essential oil microcapsules, so that the microcapsules have
Good thermal stability, and encapsulation rate with higher and essential oil retention rate；
Another object of the present invention is that provide a kind of nutmeg essential oil microcapsules so that the microcapsules have compared with
Good mobility；
Another object of the present invention is that provide a kind of nutmeg essential oil microcapsules so that the microcapsules have compared with
The particle size distribution range of small partial size and concentration；
Another object of the present invention is that providing the preparation method of above-mentioned nutmeg essential oil microcapsules and described micro-
Related application of the capsule in drug and/or food.
For achieving the above object, the invention provides the following technical scheme:
A kind of nutmeg essential oil microcapsules, including starch octenyl succinate anhydride, inulin and nutmeg essential oil.
The present invention is using starch octenyl succinate anhydride and inulin as the microcapsules of wall material preparation nutmeg essential oil, compared to normal
The wall material type of rule, can significantly improve nutmeg essential oil encapsulation rate and retention rate.
Preferably, the mass ratio of the starch octenyl succinate anhydride and inulin is (1-2): 1；Of the invention specific real
It applies in mode, the mass ratio of the starch octenyl succinate anhydride and inulin is 1.5:1 or 1:1, wherein the 1.5:1 also includes
The ratio of 1.5:1, such as 14.5:9.7 and 18.5:12.3 are nearly equal to according to the principle that rounds up；In addition, of the present invention
Mass ratio can be embodied in the form of any mass unit, such as g, kg, mg, jin, kilogram, parts by weight, more specifically, can refer to
Following situation:
(1) starch octenyl succinate anhydride 16.2g, inulin 10.8g, the two mass ratio are 1.5:1；
(2) starch octenyl succinate anhydride 10g, inulin 10g or starch octenyl succinate anhydride 11.5g, inulin 11.5g,
The two mass ratio is 1:1；
(3) starch octenyl succinate anhydride 14.5g, inulin 9.7g or starch octenyl succinate anhydride 18.5g, inulin
12.3g, the two mass ratio are approximately equal to 1.5:1.
Preferably, the quality of the nutmeg essential oil is the 20- of starch octenyl succinate anhydride and inulin gross mass
50%；In a specific embodiment, the quality of the nutmeg essential oil can choose as starch octenyl succinate anhydride and inulin
29.6% (being also possible to 8/27) of gross mass, 50%, 45% (being also possible to 10.9/24.2), 29.9% (are also possible to 9.2/
Or 30% 30.8).
It is compared to common starch octenyl succinate anhydride and maltodextrin, encapsulation rate of the invention can reach 95%
More than, it can reach 99.4%, and essential oil retention rate can reach 85% or so 75% or more；And conventional wall
The encapsulation rate that material type reaches is only 92% or so, and essential oil retention rate is only 65% or so.Meanwhile the microcapsules have well
Thermal stability.
Based on above-mentioned excellent technical effect, the invention proposes the microcapsules in preparing food and/or drug
Using.According to the purposes of nutmeg essential oil, purposes of the microcapsules of the present invention in food and/or drug is selected from as addition
Agent, as fragrance, as antioxidant content, as removing one or more of free based component.
Meanwhile the present invention also provides the preparation method of the microcapsules, the preparation method usually first prepares lotion, then
It is granulated with spray drying process or fluid-bed drying, obtains microcapsules.
It is as follows with the processing step that spray drying process is granulated:
Step 1 takes starch octenyl succinate anhydride, inulin and nutmeg essential oil, and shearing, homogeneous obtain uniform lotion；
Step 2, emulsion spray seasoning are granulated, and obtain nutmeg essential oil microcapsules.
Wherein, the condition of the spray drying can carry out according to normal conditions, be in the specific embodiment of the invention: spray
Mist pressure 0.3MPa, 170 DEG C of inlet air temperature, 60 DEG C of leaving air temp, charging rate 16mL/min；Or atomisation pressure 0.3MPa,
185 DEG C of inlet air temperature, leaving air temp is 108 DEG C, feed rate 32mL/min.
It is as follows with the processing step that fluid-bed drying is granulated:
Step 1 takes starch octenyl succinate anhydride, part inulin and nutmeg essential oil, and shearing, homogeneous obtain uniform
Lotion；
Step 2, lotion are to be granulated material to carry out fluid-bed drying granulation with remaining inulin, obtain the micro- glue of nutmeg essential oil
Capsule.
In the technique being granulated with fluid-bed drying, the spray drying process being routinely granulated is replaced with fluidized drying by the present invention
Method, and the inulin of one of wall material is divided into two parts, a part is used as the preparation of lotion, and a part is made as fluid-bed drying
The granulation material of grain is removed compared to the general way that wall material is all used as to preparation lotion by microcapsules prepared by the method for the present invention
On the basis of having the above-mentioned high encapsulation rate referred to and a high essential oil retention rate, it is also equipped with preferable mobility and has smaller
Partial size and concentration particle size distribution range.
Preferably, the part inulin (referring to the inulin for being used to prepare lotion) is the 20-30% of inulin gross mass；Having
In body embodiment, the part inulin is the 24-26% of inulin gross mass, more specifically can be 25%, 24.74% (
Can be 2.4/9.7), 25.20% (being also possible to 3.1/12.3) or 25.12% (being also possible to 2.9/11.5).
Preferably, the step 1 for the technique being granulated with fluid-bed drying are as follows:
Starch octenyl succinate anhydride is taken to be dissolved in water, part inulin is added under 40-60 DEG C of magnetic agitation in 300-500rpm,
After completely dissolution, it is cooled to room temperature, essential oil, high speed shear 30-90s, 30-80mbar homogeneous 2-4 under 6000-15000rpm is added
A circulation obtains uniform lotion.Wherein, the revolving speed of the magnetic agitation can be 300rpm, 400rpm or 500rpm, the magnetic
The temperature of power stirring can be 40 DEG C, 50 DEG C or 60 DEG C；The revolving speed of the high speed shear can be 6000rpm, 8000rpm or
The time of 10000rpm, the high speed shear can be 30s, 60s or 80s；The pressure of the homogeneous can be 30mbar,
40mbar, 50mbar or 60mbar, the recurring number of the homogeneous can be 2,3 or 4 circulations；
In addition, can obtain mobility under conditions of the present invention following fluid-bed drying and partial size is more preferably micro-
Capsule:
Atomizing pressure 1.8bar, 100~120 DEG C of inlet air temperature, 45~55 DEG C of leaving air temp, 10~20mL/ of charging rate
min.Wherein, inlet air temperature can be 100 DEG C, 110 DEG C, 115 DEG C or 120 DEG C, the leaving air temp can be 45 DEG C, 50 DEG C or
55 DEG C, the charging rate can be 14mL/min, 15mL/min, 16mL/min or 18mL/min.
From the above technical scheme, the present invention selects unconventional inulin to form sediment as one of wall material and ocentyl succinic
Powder ester prepares nutmeg essential oil microcapsules, so that the microcapsules have good thermal stability and higher encapsulation rate
With essential oil retention rate；The distinctive fluid-bed drying technique of this fit on, can be further improved the mobility of product, be that product has
The particle size distribution range of smaller particle and concentration improves the utilization rate of product.
Detailed description of the invention
Fig. 1 show the scanning electron microscope (SEM) photograph of 1 microcapsules of embodiment；
Fig. 2 show the line chart that former essential oil places 12h mass change in 40 DEG C of baking ovens；
Fig. 3 show the line chart that 1 essential oil of embodiment places 12h mass change in 40 DEG C of baking ovens；
Fig. 4, which is shown in 40 DEG C of baking ovens of former essential oil, places 12 hours column diagrams of constituent content variation later；Wherein, cylindricality A
Indicate 0h constituent content cylindricality, cylindricality B indicates 12h constituent content cylindricality, and 1-14 corresponds to 1 component of table；
Fig. 5, which is shown in embodiment 1 microencapsulation essential oil, 40 DEG C of baking ovens, places 12 hours column diagrams of constituent content variation later；
Wherein, cylindricality A indicates 0h constituent content cylindricality, and cylindricality B indicates 12h constituent content cylindricality, and 1-14 corresponds to 1 each component of table；
Fig. 6 show starch octenyl succinate anhydride/maltodextrin preparation nutmeg essential oil microcapsules scanning electron microscope (SEM) photograph.
Specific embodiment
The invention discloses a kind of nutmeg essential oil microcapsules and its preparation method and application, those skilled in the art can be with
Present disclosure is used for reference, realization of process parameters is suitably modified.In particular, it should be pointed out that all similar substitutions and modifications are to ability
It is it will be apparent that they are considered as being included in the present invention for field technique personnel.Microcapsules of the present invention and its preparation
Methods and applications are described by embodiment, and related personnel can obviously not depart from the content of present invention, spirit and model
Enclose it is interior method described herein and application are modified or appropriate changes and combinations, carry out implementation and application the technology of the present invention.
If not otherwise specified, nutmeg essential oil employed in the specific embodiment of the invention and each wall material raw material are all made of
In addition to due difference, remaining is consistent for the raw material of identical source and quality, preparation process and experimental condition.
Just a kind of nutmeg essential oil microcapsules provided by the present invention and its preparation method and application are done furtherly below
It is bright.
Embodiment 1: nutmeg essential oil microcapsules of the present invention are prepared
1) selection of raw material: choosing starch octenyl succinate anhydride 16.2g, inulin 10.8g, nutmeg essential oil 8.0g, standby
With；
2) preparation of lotion: taking starch octenyl succinate anhydride to be dissolved in water, and inulin 2.7g is added under magnetic agitation, sufficiently molten
Xie Hou is cooled to room temperature, and essential oil is added, high speed shear, homogeneous obtain uniform lotion；
The condition of the magnetic agitation is: 300rpm, 50 DEG C；
The condition of the high speed shear is: 10000rpm, 60s；
The condition of the homogeneous is: 60mbar, 2 circulations；
3) prepared by microcapsules: lotion fluid-bed drying is granulated, and charging rate appropriate is arranged, and keeps feeding temperature and outlet air
Temperature is added residue 8.1g inulin as material is granulated, obtains nutmeg essential oil microcapsules；
The condition of the fluid-bed drying is: atomizing pressure 1.8bar, 100 DEG C of inlet air temperature, 45 DEG C of leaving air temp, into
Expect speed 14mL/min；
It is 99.4% that the microcapsule embedded rate of nutmeg essential oil, which is made, and essential oil retention rate is 85.2%, through scanning electron microscopic observation,
Surface compact is regular circle, inviscid, and partial size is 1-4 μm, sees Fig. 1.
Embodiment 2: nutmeg essential oil microcapsules of the present invention are prepared
1) selection of raw material: choosing starch octenyl succinate anhydride 10g, inulin 10g, nutmeg essential oil 10g, spare；
2) preparation of lotion: taking starch octenyl succinate anhydride to be dissolved in water, and inulin 2.5g is added under magnetic agitation, sufficiently molten
Xie Hou is cooled to room temperature, and essential oil is added, high speed shear, homogeneous obtain uniform lotion；
The condition of the magnetic agitation is: 500rpm, 60 DEG C；
The condition of the high speed shear is: 8000rpm, 80s；
The condition of the homogeneous is: 40mbar, 3 circulations；
3) prepared by microcapsules: lotion fluid-bed drying is granulated, and charging rate appropriate is arranged, and keeps feeding temperature and outlet air
Temperature is added residue 7.5g inulin as material is granulated, obtains nutmeg essential oil microcapsules；
The condition of the fluid-bed drying is: atomizing pressure 1.8bar, 110 DEG C of inlet air temperature, 50 DEG C of leaving air temp, into
Expect speed 18mL/min；
It is 98.6% that the microcapsule embedded rate of nutmeg essential oil, which is made, and essential oil retention rate is 80.4%, through scanning electron microscopic observation,
Surface compact is regular circle, inviscid, and partial size is 1-4 μm.
Embodiment 3: nutmeg essential oil microcapsules of the present invention are prepared
1) selection of raw material: choosing starch octenyl succinate anhydride 14.5g, inulin 9.7g, nutmeg essential oil 10.9g, standby
With；
2) preparation of lotion: taking starch octenyl succinate anhydride to be dissolved in water, and inulin 2.4g is added under magnetic agitation, sufficiently molten
Xie Hou is cooled to room temperature, and essential oil is added, high speed shear, homogeneous obtain uniform lotion；
The condition of the magnetic agitation is: 300rpm, 40 DEG C；
The condition of the high speed shear is: 10000rpm, 30s；
The condition of the homogeneous is: 60mbar, 2 circulations；
3) prepared by microcapsules: lotion fluid-bed drying is granulated, and charging rate appropriate is arranged, and keeps feeding temperature and outlet air
Temperature is added residue 7.3g inulin as material is granulated, obtains nutmeg essential oil microcapsules；
The condition of the fluid-bed drying is: atomizing pressure 1.8bar, 115 DEG C of inlet air temperature, 55 DEG C of leaving air temp, into
Expect speed 16mL/min；
It is 97.0% that the microcapsule embedded rate of nutmeg essential oil, which is made, and essential oil retention rate is 78.1%, through scanning electron microscopic observation,
Surface compact is regular circle, inviscid, and partial size is 1-4 μm.
Embodiment 4: nutmeg essential oil microcapsules of the present invention are prepared
1) selection of raw material: choosing starch octenyl succinate anhydride 18.5g, inulin 12.3g, nutmeg essential oil 9.2g, standby
With；
2) preparation of lotion: taking starch octenyl succinate anhydride to be dissolved in water, and inulin 3.1g is added under magnetic agitation, sufficiently molten
Xie Hou is cooled to room temperature, and essential oil is added, high speed shear, homogeneous obtain uniform lotion；
The condition of the magnetic agitation is: 500rpm, 50 DEG C；
The condition of the high speed shear is: 6000rpm, 80s；
The condition of the homogeneous is: 30mbar, 3 circulations；
3) prepared by microcapsules: lotion fluid-bed drying is granulated, and charging rate appropriate is arranged, and keeps feeding temperature and outlet air
Temperature is added residue 9.2g inulin as material is granulated, obtains nutmeg essential oil microcapsules；
The condition of the fluid-bed drying is: atomizing pressure 1.8bar, 100 DEG C of inlet air temperature, 50 DEG C of leaving air temp, into
Expect speed 15mL/min；
It is 97.2% that the microcapsule embedded rate of nutmeg essential oil, which is made, and essential oil retention rate is 77.8%, through scanning electron microscopic observation,
Surface compact is regular circle, inviscid, and partial size is 1-4 μm.
Embodiment 5: nutmeg essential oil microcapsules of the present invention are prepared
1) selection of raw material: choosing starch octenyl succinate anhydride 11.5g, inulin 11.5g, nutmeg essential oil 6.9g, standby
With；
2) preparation of lotion: taking starch octenyl succinate anhydride to be dissolved in water, and inulin 2.9g is added under magnetic agitation, sufficiently molten
Xie Hou is cooled to room temperature, and essential oil is added, high speed shear, homogeneous obtain uniform lotion；
The condition of the magnetic agitation is: 500rpm, 60 DEG C；
The condition of the high speed shear is: 8000rpm, 60s；
The condition of the homogeneous is: 50mbar, 2 circulations；
3) prepared by microcapsules: lotion fluid-bed drying is granulated, and charging rate appropriate is arranged, and keeps feeding temperature and outlet air
Temperature is added residue 8.6g inulin as material is granulated, obtains nutmeg essential oil microcapsules；
The condition of the fluid-bed drying is: atomizing pressure 1.8bar, 120 DEG C of inlet air temperature, 55 DEG C of leaving air temp, into
Expect speed 16mL/min；
It is 95.4% that the microcapsule embedded rate of nutmeg essential oil, which is made, and essential oil retention rate is 80.3%, through scanning electron microscopic observation,
Surface compact is regular circle, inviscid, and partial size is 1-4 μm.
Embodiment 6: nutmeg essential oil microcapsules of the present invention are prepared
1) selection of raw material: choosing starch octenyl succinate anhydride 15.3g, inulin 7.7g, nutmeg essential oil 6.9g, standby
With；
2) preparation of lotion: taking starch octenyl succinate anhydride to be dissolved in water, and inulin 7.7g is added under magnetic agitation, sufficiently molten
Xie Hou is cooled to room temperature, and essential oil is added, high speed shear, homogeneous obtain uniform lotion；
The condition of the magnetic agitation is: 500rpm, 40 DEG C；
The condition of the high speed shear is: 8000rpm, 60s；
The condition of the homogeneous is: 50mbar, 2 circulations；
3) prepared by microcapsules: lotion is routinely spray-dried, and obtains nutmeg essential oil microcapsules；
The condition being routinely spray-dried is: atomisation pressure 0.3MPa, 170 DEG C of inlet air temperature, 60 DEG C of leaving air temp,
Charging rate 16mL/min.
It is 96.0% that the microcapsule embedded rate of nutmeg essential oil, which is made, and essential oil retention rate is 77.7%.But microscapsule powder is viscous
Degree is big, particle slightly conglomeration, carr index 36.55%, poor (mobility of particle ratio when carr index is less than 25% of powder flowbility
Preferably).
Embodiment 7: nutmeg essential oil microencapsulation fore-and-aft stability compares
Former essential oil and 1 microencapsulation essential oil of embodiment are placed in progress constant temperature storage, every 2h in 40 DEG C of electric heating bellows to take
Sample measurement, measures its thermal stability with constant weight method, the results are shown in Table 1-3 and Fig. 2-5.
The former essential oil composition of table 1 and its relative amount (%)
The former essential oil of table 2 places the component measured after 12h and its relative amount (%) in 40 DEG C of baking ovens
3 microencapsulation essential oil of table places the component measured after 12h and its relative amount (%) in 40 DEG C of baking ovens
Table 1-3 and Fig. 2-5 display, from the point of view of the variation of gross mass and each component, quality is kept to originally after former essential oil 2 hours
60% after 2 hours hereinafter, volatilize slow.Australene almost all is volatilized after 12 hours, and australene loss is obvious after microencapsulation
It reduces.Obviously essential oil progress microencapsulation rear stability is significantly improved.
Embodiment 8: the nutmeg essential oil microencapsulation rate of other techniques and the statistics of essential oil retention rate
1) starch octenyl succinate anhydride 18.5g, maltodextrin 12.3g, nutmeg essential oil the selection of raw material: are chosen
9.2g, it is spare；
2) preparation of lotion: taking starch octenyl succinate anhydride to be dissolved in water, and inulin 3.1g is added under magnetic agitation, sufficiently molten
Xie Hou is cooled to room temperature, and essential oil is added, high speed shear, homogeneous obtain uniform lotion；
The condition of the magnetic agitation is: 500rpm, 50 DEG C；
The condition of the high speed shear is: 6000rpm, 80s；
The condition of the homogeneous is: 30mbar, 3 circulations；
3) prepared by microcapsules: lotion fluid-bed drying is granulated, and charging rate appropriate is arranged, and keeps feeding temperature and outlet air
Temperature is added residue 9.2g maltodextrin as material is granulated, obtains nutmeg essential oil microcapsules；
The condition of the fluid-bed drying is: atomizing pressure 1.8bar, 100 DEG C of inlet air temperature, 50 DEG C of leaving air temp, into
Expect speed 15mL/min；
It is 92.2% that the microcapsule embedded rate of nutmeg essential oil, which is made, and essential oil retention rate is 65.8%.
The control technique and 4 technique of the embodiment of the present invention that can be seen that the present embodiment according to above-mentioned process conditions are only in wall
Material type is different, and high as the microencapsulated rate of wall material using starch octenyl succinate anhydride and inulin, essential oil retention rate is high, and produces
Product have the healthcare function of inulin.
Embodiment 9: the nutmeg essential oil micro-capsule mobility and micromeritis Characteristic Contrast of different process
The process ration of embodiment 6 spray drying process and fluid-bed drying be granulated and the difference of inulin usage mode under
Mobility, it was demonstrated that can be improved the mobility of microcapsules under fluidized drying process conditions of the present invention.On this basis,
The present embodiment further provides for the mobility and micromeritis feature of control technique and present invention process contrast product.
1, comparative example technique
Wall material: nutmeg essential oil=1:4, starch Sodium Octenyl Succinate in wall material: maltodextrin=10g:10g
Wall material is added in ultrapure water, heating stirring dissolves at 90 DEG C, obtains wall material aqueous solution；The wherein compound wall materials
Aqueous solution mass concentration is 10%；
Nutmeg essential oil is added in above-mentioned wall material aqueous solution, with the speed high speed shear 2min of 20000r/min, obtains
Colostric fluid；Wherein, the compound wall materials and the mass ratio of nutmeg essential oil are 1:4；By obtained colostric fluid with high pressure 300Bar,
Temperature 60 C, obtains the whole lotion of stable homogeneous homogeneous 1 time；
Whole emulsion spray after above-mentioned homogeneous is dried to obtain nutmeg essential oil micro-capsule powder (scanning electron microscope (SEM) photograph is shown in Fig. 6),
Atomisation pressure 0.3MPa when spray drying treatment, inlet air temperature are 185 DEG C, and leaving air temp is 108 DEG C, and feed rate is
32mL/min。
2, the measurement of carr index:
Take certain mass m (10g) sample, be placed in 100mL graduated cylinder, after gently striking off read volume V0, oscillation graduated cylinder until
Powder volume no longer changes, and reading volume is Vf, duplicate measurements three times, calculate heap density D0With tap density Df, then:
D0=m/V0Df=m/Vf
Carr index (Carr index)=(Df-D0)/Df× 100%
3, determination of moisture:
It is measured according to GB50093-2010 " measurement of moisture in food " method.Clean aluminum capsule is taken, 105 DEG C of bakings are placed in
In case, tiltedly lid branch heats 1h in box side, and taking-up is placed in drier, cooling 0.5h.It weighs, it is of poor quality to front and back to repeat drying
No more than 2mg, as aluminum capsule constant weight m3。
2g~5g sample (being accurate to 0.0001g) is weighed, is put into this aluminum capsule, weight m is closed1, sample thickness is no more than
5mm, for example loose sample, thickness are no more than 10mm, cover, and after precision weighing, set in 101 DEG C~105 DEG C drying boxes, bottle cap is oblique
Branch covers taking-up behind bottle side, dry 2h~4h, weighs after being put into drier cooling 0.5h.Then place into 101 DEG C~
Dry 1h or so, takes out in 105 DEG C of drying boxes, weighs again after being put into drier cooling 0.5h.And it repeats above operation to preceding
It is of poor quality twice afterwards to be no more than 2mg, as constant weight m2.Then moisture content are as follows:
X=(m1-m2)/(m1-m3)×100
X --- the content of moisture in sample, unit are gram every hectogram (g/100g)；
m1--- the quality of aluminum capsule and sample, unit are gram (g)；
m2--- the quality after aluminum capsule and samples dried, unit are gram (g)；
m3--- the quality of aluminum capsule, unit are gram (g).
When moisture content >=1g/100g, calculated result retains three effective digitals；When moisture content < 1g/100g, as a result
Retain two effective digitals.
4, the measurement (funnel method) at angle of repose:
The culture dish that a diameter is 6cm is put in bottom, and funnel is fixed on iron stand, makes the distance between funnel and culture dish
For 10cm, powder 10g is weighed, powder is fallen above funnel, is gradually accumulated in culture dish after funnel buffers, forms cone
Body.Until obtaining highest cone, a height of h of the cone and radius r of conical bottom circle is measured.Find out angle of repose
α is averaged in triplicate.Calculation formula are as follows:
Tan α=h/r
5, result
The powder characteristics of 4 nutmeg essential oil microencapsulated powder of table
From the powder characteristics of essential oil microencapsulation product it can be seen that powder modest viscosity obtained by present invention process, particle are equal
It is even, average grain diameter less than 4 μm, moisture content is held at 3% or so substantially.Powder carr index and angle of repose more preferably, are easier to
Molding, mobility are more preferable.
And the essential oil microencapsulation product of comparative example technique, powder viscosity are larger, particle is finer and smoother, at the same average grain diameter also compared with
Height, between 3-6 μm, powder carr index and angle of repose are obviously poor, and not easily molded, mobility is poor.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of nutmeg essential oil microcapsules, which is characterized in that including starch octenyl succinate anhydride, inulin and nutmeg essence
Oil.
2. microcapsules according to claim 1, which is characterized in that the mass ratio of the starch octenyl succinate anhydride and inulin
For (1-2): 1.
3. microcapsules according to claim 1, which is characterized in that the quality of the nutmeg essential oil is that ocentyl succinic forms sediment
The 20-50% of powder ester and inulin gross mass.
4. microcapsules described in claim 1-3 any one are preparing the application in food and/or drug.
5. applying according to claim 4, which is characterized in that purposes of the microcapsules in food and/or drug is selected from
As additive, as fragrance, as antioxidant content, as removing one or more of free based component.
6. the preparation method of microcapsules described in claim 1 characterized by comprising
Step 1 takes starch octenyl succinate anhydride, part inulin and nutmeg essential oil, and shearing, homogeneous obtain uniform lotion；
Step 2, lotion are to be granulated material to carry out fluid-bed drying granulation with remaining inulin, obtain nutmeg essential oil microcapsules.
7. preparation method according to claim 6, which is characterized in that step 1 are as follows:
Starch octenyl succinate anhydride is taken to be dissolved in water, part inulin is added under 40-60 DEG C of magnetic agitation, sufficiently in 300-500rpm
It after dissolution, is cooled to room temperature, essential oil is added, high speed shear 30-90s, 30-80mbar homogeneous 2-4 is followed under 6000-15000rpm
Ring obtains uniform lotion.
8. preparation method described according to claim 6 or 7, which is characterized in that the part inulin is the 20- of inulin gross mass
30%.
9. preparation method according to claim 6, which is characterized in that the condition of the fluid-bed drying is as follows:
Atomizing pressure 1.8bar, 100~120 DEG C of inlet air temperature, 45~55 DEG C of leaving air temp, 10~20mL/min of charging rate.
10. the preparation method of microcapsules described in claim 1 characterized by comprising
Step 1 takes starch octenyl succinate anhydride, inulin and nutmeg essential oil, and shearing, homogeneous obtain uniform lotion；
Step 2, emulsion spray seasoning are granulated, and obtain nutmeg essential oil microcapsules.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710647284.7A CN109317066B (en) | 2017-08-01 | 2017-08-01 | Myristica fragrans essential oil microcapsule and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710647284.7A CN109317066B (en) | 2017-08-01 | 2017-08-01 | Myristica fragrans essential oil microcapsule and preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109317066A true CN109317066A (en) | 2019-02-12 |
| CN109317066B CN109317066B (en) | 2021-04-27 |
Family
ID=65245834
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710647284.7A Active CN109317066B (en) | 2017-08-01 | 2017-08-01 | Myristica fragrans essential oil microcapsule and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109317066B (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN113016864A (en) * | 2021-04-20 | 2021-06-25 | 甘肃农业大学 | Preparation method of dried meat 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 |
| CN113730299A (en) * | 2021-08-06 | 2021-12-03 | 广州市芳香时代进出口有限公司 | Preparation process of essential oil microcapsule containing essential oil |
| CN114869847A (en) * | 2022-03-31 | 2022-08-09 | 中国热带农业科学院分析测试中心 | Amomum katsumadai essential oil microemulsion and preparation method thereof |
| CN116492944A (en) * | 2023-06-21 | 2023-07-28 | 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 |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102349584A (en) * | 2011-09-22 | 2012-02-15 | 徐州工程学院 | Method for preparing myristica oil microcapsule by utilizing ultrasonic waves |
| US20140066357A1 (en) * | 2012-08-30 | 2014-03-06 | P. H. Glatfelter Company | Heat-stable microencapsulated fragrance oils |
| CN103861537A (en) * | 2014-03-20 | 2014-06-18 | 中国热带农业科学院农产品加工研究所 | Preparation method of essential oil microcapsule |
| WO2015019307A1 (en) * | 2013-08-07 | 2015-02-12 | University Of Saskatchewan | Microcapsules containing probiotics and methods of making same |
| CN105343723A (en) * | 2015-12-15 | 2016-02-24 | 广西大海阳光药业有限公司 | Preparation method of Juyuan cough relieving micro-capsule |
| CN105996040A (en) * | 2016-05-20 | 2016-10-12 | 福建师范大学 | Microcapsule powder and preparation method thereof |
| CN106343577A (en) * | 2015-07-09 | 2017-01-25 | 北京宝得瑞食品有限公司 | Water-soluble sea buckthron oil microcapsules with high oil carrying capacity and preparation method thereof |
| CN106690154A (en) * | 2016-11-22 | 2017-05-24 | 张海生 | Processing method of red jujube polyphenol microcapsule food |
| WO2017127641A1 (en) * | 2016-01-20 | 2017-07-27 | Flurry Powders | Encapsulation of lipophilic ingredients in dispersible spray dried powders suitable for inhalation |
-
2017
- 2017-08-01 CN CN201710647284.7A patent/CN109317066B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102349584A (en) * | 2011-09-22 | 2012-02-15 | 徐州工程学院 | Method for preparing myristica oil microcapsule by utilizing ultrasonic waves |
| US20140066357A1 (en) * | 2012-08-30 | 2014-03-06 | P. H. Glatfelter Company | Heat-stable microencapsulated fragrance oils |
| WO2015019307A1 (en) * | 2013-08-07 | 2015-02-12 | University Of Saskatchewan | Microcapsules containing probiotics and methods of making same |
| CN103861537A (en) * | 2014-03-20 | 2014-06-18 | 中国热带农业科学院农产品加工研究所 | Preparation method of essential oil microcapsule |
| CN106343577A (en) * | 2015-07-09 | 2017-01-25 | 北京宝得瑞食品有限公司 | Water-soluble sea buckthron oil microcapsules with high oil carrying capacity and preparation method thereof |
| CN105343723A (en) * | 2015-12-15 | 2016-02-24 | 广西大海阳光药业有限公司 | Preparation method of Juyuan cough relieving micro-capsule |
| WO2017127641A1 (en) * | 2016-01-20 | 2017-07-27 | Flurry Powders | Encapsulation of lipophilic ingredients in dispersible spray dried powders suitable for inhalation |
| CN105996040A (en) * | 2016-05-20 | 2016-10-12 | 福建师范大学 | Microcapsule powder and preparation method thereof |
| CN106690154A (en) * | 2016-11-22 | 2017-05-24 | 张海生 | Processing method of red jujube polyphenol microcapsule food |
Non-Patent Citations (1)
| Title |
|---|
| 缪晓平等: "肉豆蔻油树脂的提取及微胶囊化的研究", 《中国调味品》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN113016864A (en) * | 2021-04-20 | 2021-06-25 | 甘肃农业大学 | Preparation method of dried meat preservative |
| 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 |
| CN113730299A (en) * | 2021-08-06 | 2021-12-03 | 广州市芳香时代进出口有限公司 | Preparation process of essential oil microcapsule containing essential oil |
| 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 |
| CN114869847A (en) * | 2022-03-31 | 2022-08-09 | 中国热带农业科学院分析测试中心 | Amomum katsumadai essential oil microemulsion and preparation method thereof |
| CN116492944A (en) * | 2023-06-21 | 2023-07-28 | 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 |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109317066B (en) | 2021-04-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109317066A (en) | A kind of nutmeg essential oil microcapsules and its preparation method and application | |
| Yang et al. | Development and evaluation of novel microcapsules containing poppy-seed oil using complex coacervation | |
| Shen et al. | Preparation and characterization of clove essential oil loaded nanoemulsion and pickering emulsion activated pullulan-gelatin based edible film | |
| Devi et al. | Encapsulation of active ingredients in polysaccharide–protein complex coacervates | |
| Kumar et al. | Evaluation of chitosan as a wall material for microencapsulation of squalene by spray drying: Characterization and oxidative stability studies | |
| Kaushik et al. | Microencapsulation of flaxseed oil in flaxseed protein and flaxseed gum complex coacervates | |
| JP5439366B2 (en) | Cellulose powder excellent in segregation preventing effect and composition thereof | |
| Zhou et al. | Preparation of walnut oil microcapsules employing soybean protein isolate and maltodextrin with enhanced oxidation stability of walnut oil | |
| Chawla et al. | Synthesis, characterization and cellular mineral absorption of nanoemulsions of Rhododendron arboreum flower extracts stabilized with gum arabic | |
| Choi et al. | Spray-dried conjugated linoleic acid encapsulated with Maillard reaction products of whey proteins and maltodextrin | |
| JP5734436B2 (en) | High-performance cellulose composite | |
| JP5757698B2 (en) | Organic-inorganic composite particles and method for producing the same, dispersion containing the particles, and cosmetics containing the particles | |
| Zhao et al. | Measurement of particle diameter of Lactobacillus acidophilus microcapsule by spray drying and analysis on its microstructure | |
| XIE et al. | Study on the morphology, particle size and thermal properties of vitamin A microencapsulated by starch octenylsucciniate | |
| CN109219357A (en) | food additive | |
| Binsi et al. | Structural, functional and in vitro digestion characteristics of spray dried fish roe powder stabilised with gum arabic | |
| JP2006045491A (en) | Functional material, method for producing functional material, functional member and environment modification apparatus using the functional material | |
| Bordón et al. | Formulation, spray-drying and physicochemical characterization of functional powders loaded with chia seed oil and prepared by complex coacervation | |
| CN102613298B (en) | Glycerol monolaurate microcapsule as well as preparation method and application of glycerol monolaurate microcapsule | |
| Chen et al. | Physicochemical properties and storage stability of microencapsulated DHA-rich oil with different wall materials | |
| JP2013053086A (en) | Microcapsule containing oil and fat and method for producing the same | |
| CN107455492A (en) | A kind of method that nano-silicon dioxide modified microcapsule wall material prepares microcapsules | |
| Chen et al. | Quinoa protein isolate-gum Arabic coacervates cross-linked with sodium tripolyphosphate: Characterization, environmental stability, and Sichuan pepper essential oil microencapsulation | |
| Marinopoulou et al. | Production of spray-dried starch molecular inclusion complexes on an industrial scale | |
| Arshad et al. | Native and modified Sorghum starches as wall materials in microencapsulation of nutmeg oleoresin |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |