CN115736007A - Litsea cubeba essential oil nanoparticles, preparation method thereof and application thereof in pepper preservation - Google Patents
Litsea cubeba essential oil nanoparticles, preparation method thereof and application thereof in pepper preservation Download PDFInfo
- Publication number
- CN115736007A CN115736007A CN202211548544.2A CN202211548544A CN115736007A CN 115736007 A CN115736007 A CN 115736007A CN 202211548544 A CN202211548544 A CN 202211548544A CN 115736007 A CN115736007 A CN 115736007A
- Authority
- CN
- China
- Prior art keywords
- essential oil
- litsea cubeba
- cubeba essential
- nanoparticles
- chitosan
- 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.)
- Pending
Links
- 239000000341 volatile oil Substances 0.000 title claims abstract description 146
- 240000002262 Litsea cubeba Species 0.000 title claims abstract description 129
- 235000012854 Litsea cubeba Nutrition 0.000 title claims abstract description 129
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 90
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 235000002566 Capsicum Nutrition 0.000 title abstract description 22
- 239000006002 Pepper Substances 0.000 title abstract description 20
- 235000016761 Piper aduncum Nutrition 0.000 title abstract description 20
- 235000017804 Piper guineense Nutrition 0.000 title abstract description 20
- 235000008184 Piper nigrum Nutrition 0.000 title abstract description 20
- 238000004321 preservation Methods 0.000 title description 15
- 244000203593 Piper nigrum Species 0.000 title 1
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 38
- 229920001661 Chitosan Polymers 0.000 claims abstract description 37
- 239000012071 phase Substances 0.000 claims abstract description 35
- 235000010489 acacia gum Nutrition 0.000 claims abstract description 34
- 239000001785 acacia senegal l. willd gum Substances 0.000 claims abstract description 34
- 239000000843 powder Substances 0.000 claims abstract description 31
- 239000000839 emulsion Substances 0.000 claims abstract description 25
- 239000003921 oil Substances 0.000 claims abstract description 20
- 240000008574 Capsicum frutescens Species 0.000 claims abstract description 10
- 239000008346 aqueous phase Substances 0.000 claims abstract description 10
- 235000002568 Capsicum frutescens Nutrition 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 46
- 239000000243 solution Substances 0.000 claims description 42
- 238000003756 stirring Methods 0.000 claims description 37
- 239000008367 deionised water Substances 0.000 claims description 21
- 229910021641 deionized water Inorganic materials 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 15
- 238000005119 centrifugation Methods 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 12
- 229920000136 polysorbate Polymers 0.000 claims description 11
- 239000006228 supernatant Substances 0.000 claims description 11
- 238000000108 ultra-filtration Methods 0.000 claims description 11
- 239000012153 distilled water Substances 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 9
- 238000009777 vacuum freeze-drying Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 9
- KEQXNNJHMWSZHK-UHFFFAOYSA-L 1,3,2,4$l^{2}-dioxathiaplumbetane 2,2-dioxide Chemical compound [Pb+2].[O-]S([O-])(=O)=O KEQXNNJHMWSZHK-UHFFFAOYSA-L 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 241000722363 Piper Species 0.000 abstract description 19
- 230000000694 effects Effects 0.000 abstract description 15
- 239000000463 material Substances 0.000 abstract description 5
- 230000003064 anti-oxidating effect Effects 0.000 abstract description 4
- 239000013543 active substance Substances 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 238000011282 treatment Methods 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 10
- OSVXSBDYLRYLIG-UHFFFAOYSA-N dioxidochlorine(.) Chemical compound O=Cl=O OSVXSBDYLRYLIG-UHFFFAOYSA-N 0.000 description 10
- 239000003755 preservative agent Substances 0.000 description 9
- 239000000126 substance Substances 0.000 description 8
- 235000013399 edible fruits Nutrition 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- 230000002335 preservative effect Effects 0.000 description 6
- 238000003860 storage Methods 0.000 description 6
- 238000012546 transfer Methods 0.000 description 6
- 239000004155 Chlorine dioxide Substances 0.000 description 5
- 235000019398 chlorine dioxide Nutrition 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 238000005538 encapsulation Methods 0.000 description 4
- 235000013305 food Nutrition 0.000 description 4
- 230000005855 radiation Effects 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 3
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000003958 fumigation Methods 0.000 description 3
- 238000000338 in vitro Methods 0.000 description 3
- 239000008055 phosphate buffer solution Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000007853 buffer solution Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000002595 cold damage Effects 0.000 description 2
- 238000004320 controlled atmosphere Methods 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000000813 microbial effect Effects 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 208000035240 Disease Resistance Diseases 0.000 description 1
- 241000758706 Piperaceae Species 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000003260 anti-sepsis Effects 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 239000001390 capsicum minimum Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005354 coacervation Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 235000012055 fruits and vegetables Nutrition 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 230000002503 metabolic effect Effects 0.000 description 1
- 239000003094 microcapsule Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 1
- 235000019796 monopotassium phosphate Nutrition 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 1
- IYDGMDWEHDFVQI-UHFFFAOYSA-N phosphoric acid;trioxotungsten Chemical compound O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.OP(O)(O)=O IYDGMDWEHDFVQI-UHFFFAOYSA-N 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229930000044 secondary metabolite Natural products 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 230000008685 targeting Effects 0.000 description 1
Images
Landscapes
- Medicinal Preparation (AREA)
Abstract
The invention discloses litsea cubeba essential oil nanoparticles, a preparation method thereof and application thereof in fresh keeping of hot pepper, and relates to the technical field of fresh keeping agents, wherein the litsea cubeba essential oil nanoparticles comprise the following raw materials: the gum comprises chitosan, arabic gum powder, an emulsifier and litsea cubeba essential oil, wherein the mass ratio of the chitosan to the Arabic gum powder is 1:5 to 1; the preparation method comprises the following steps: s1: preparing an aqueous phase solution; s2: preparing an oil phase; s3: preparing an emulsion; s4: preparing litsea cubeba essential oil nanoparticles; the litsea cubeba essential oil nanoparticles are used for keeping the pepper fresh; by adopting chitosan and Arabic gum as materials, the litsea cubeba essential oil is subjected to nano embedding, the stability of the litsea cubeba essential oil is improved, the release rate of active substances is controlled, and the active effects of the litsea cubeba essential oil such as bacteriostasis, antioxidation and the like can be effectively utilized.
Description
Technical Field
The invention relates to the technical field of preservatives, in particular to litsea cubeba essential oil nanoparticles, a preparation method thereof and application thereof in pepper preservation.
Background
The essential oil is used as a natural preservative, and the traditional application method is to directly coat and spray the essential oil on the surface of food or achieve the effect of antisepsis and preservation in a fumigation mode, wherein the fumigation method is the most common treatment mode because the fumigation method can not damage food and can keep the original flavor of the food. However, limitations based on the high volatility of essential oils, their susceptibility to decomposition by heat, their pronounced pungent odor, etc. limit their widespread use in the food industry. The litsea cubeba essential oil serving as a secondary metabolite has broad-spectrum antibacterial activity and obvious antioxidation, has a good development prospect in the field of fruit and vegetable preservation, and is a research hotspot of the current plant-derived preservative. The nano embedding technology is more stable than the microcapsule due to the specific nano size effect, has better biocompatibility, targeting property and slow release property, and can effectively reduce the sensitivity of bioactive substances. The litsea cubeba essential oil is subjected to nano embedding by adopting a complex coacervation method so as to increase the stability, reduce the volatilization loss of the essential oil and fully utilize the biological activity of the essential oil.
At present, the pepper preservation technology mainly adopts physical methods and chemical preservatives, but the defects of the preservation methods are continuously highlighted, for example, chemical preservatives are easy to have chemical reagent residues, so that the human body and the environment are damaged; the low-temperature storage has high energy consumption, and the cold damage of fruits is easily caused if the operation is improper; the controlled atmosphere storage investment is large, the requirement on the gas proportion is strict, and the stability is poor; the radiation fresh-keeping has very strict requirements on radiation use measurement and has higher operation difficulty; the common film-coating fresh-keeping method has the problems of easy microbial pollution, poor stability and the like due to the material problem; therefore, aiming at the current situation, the litsea cubeba essential oil nanoparticles, the preparation method thereof and the application thereof in pepper preservation are urgently needed to be developed so as to meet the actual use requirement.
Disclosure of Invention
In view of the above, the invention aims to overcome the defects in the prior art, and the main purpose of the invention is to provide litsea cubeba essential oil nanoparticles, a preparation method thereof and application thereof in pepper preservation.
In order to achieve the purpose, the invention adopts the following technical scheme:
the litsea cubeba essential oil nanoparticle comprises the following raw materials: the gum comprises chitosan, arabic gum powder, an emulsifier and litsea cubeba essential oil, wherein the mass ratio of the chitosan to the Arabic gum powder is 1:5 to 1.
The preparation method of the litsea cubeba essential oil nanoparticles comprises the following steps:
s1: preparing an aqueous phase solution: transferring an emulsifying agent to dissolve in deionized water, respectively weighing chitosan and Arabic gum powder, dissolving the weighed chitosan and Arabic gum powder in the deionized water added with the emulsifying agent, stirring at 60 ℃ until the chitosan and Arabic gum powder are completely dissolved, filtering by 0.45 mu m, and adjusting the pH of the solution to 4.0 to obtain an aqueous solution;
s2: preparing an oil phase: dissolving litsea cubeba essential oil in absolute ethyl alcohol, wherein the volume ratio of the mass of the litsea cubeba essential oil to the absolute ethyl alcohol is 1; continuously adding an emulsifier to obtain an oil phase;
s3: preparing an emulsion: slowly and dropwise adding the oil phase obtained in the step S2 into the water phase solution obtained in the step S1, and stirring at normal temperature at the stirring speed of: 800r/min, stirring for 30min to obtain milk white emulsion;
s4: preparing litsea cubeba essential oil nanoparticles: and (3) centrifuging the emulsion obtained in the step (S3) by using an ultrafiltration centrifugal tube, wherein the centrifugation speed is 12000r/min, the centrifugation time is 30min, discarding the supernatant, taking the lower layer, washing the particles by using distilled water, and carrying out vacuum freeze drying at-52 ℃ to obtain the litsea cubeba essential oil nanoparticles.
As a preferred embodiment: the volume ratio of the emulsifier to the deionized water in the S1 is 1.
As a preferred embodiment: the mass ratio of the chitosan to the Arabic gum powder weighed in the S1 is 1.
As a preferred embodiment: the ratio of the mass of the chitosan to the volume of the emulsifier in the S1 is 5.
As a preferred embodiment: the emulsifier is tween and span.
As a preferred embodiment: the volume ratio of the spit temperature to the span is 1
As a preferred embodiment: the volume ratio of the mass of the litsea cubeba essential oil to the absolute ethyl alcohol in the S2 is 1.
As a preferred embodiment: the volume ratio of the mass of the emulsifier in the S2 to the absolute ethyl alcohol is 1.
The litsea cubeba essential oil nanoparticles are applied to the preservation of hot peppers.
Compared with the prior art, the invention has obvious advantages and beneficial effects, and concretely, according to the technical scheme, the litsea cubeba essential oil is subjected to nano embedding by adopting the chitosan and the Arabic gum as materials, so that the stability of the litsea cubeba essential oil is improved, the release rate of active substances is controlled, and the active effects of bacteriostasis, antioxidation and the like of the litsea cubeba essential oil can be effectively utilized; the litsea cubeba essential oil is used as a raw material, and the nano embedded essential oil nanoparticles are used as a plant source preservative to be applied to the preservation of the hot pepper, so that the effect of preserving the hot pepper is good.
To more clearly illustrate the structural features and effects of the present invention, the following detailed description is given with reference to the accompanying drawings and specific embodiments.
Drawings
FIG. 1 is a schematic diagram showing the influence of the addition amount of Litsea cubeba essential oil on the nanoparticle embedding rate;
FIG. 2 is a transmission electron microscope image of the Litsea cubeba essential oil nanoparticles of the present invention;
FIG. 3 is a transmission electron micrograph of blank nanoparticles of the present invention;
FIG. 4 is a graph showing the in vitro release rate of Litsea cubeba essential oil nanoparticles and Litsea cubeba essential oil;
FIG. 5 is a graph showing the effect of different substances on the decay rate of peppers treated in accordance with the present invention.
The attached drawings indicate the following:
in the figure: CK1 is 1% chlorine dioxide treatment; CK2 is blank processing; CN is the blank nanoparticle treatment obtained in comparative example 1; EN is the treatment of the litsea cubeba essential oil nanoparticles obtained in the example 2; EO is litsea cubeba essential oil treatment in comparative example 2.
Detailed Description
As shown in fig. 1 to 5, the invention provides litsea cubeba essential oil nanoparticles, which comprise the following raw materials: the gum comprises chitosan, arabic gum powder, an emulsifying agent and litsea cubeba essential oil, wherein the mass ratio of the chitosan to the Arabic gum powder is 1:5 to 1.
The preparation method of the litsea cubeba essential oil nanoparticles comprises the following steps:
s1: preparing an aqueous phase solution: transferring an emulsifying agent to dissolve in deionized water, respectively weighing chitosan and Arabic gum powder, and dissolving the weighed chitosan and Arabic gum powder in the deionized water added with the emulsifying agent, wherein the volume ratio of the emulsifying agent to the deionized water is 1; the weight ratio of the chitosan to the Arabic gum powder is 1; the ratio of the mass of the chitosan to the volume of the emulsifier is 5; the emulsifier is tween and span, and the volume ratio of the tween to the span is 1; stirring at 60 deg.C until completely dissolved, filtering at 0.45 μm, and adjusting pH of the solution to 4.0 to obtain water phase solution;
s2: preparing an oil phase: dissolving litsea cubeba essential oil in absolute ethyl alcohol, wherein the volume ratio of the mass of the litsea cubeba essential oil to the absolute ethyl alcohol is (1); the optimal volume ratio of the mass of the litsea cubeba essential oil to the absolute ethyl alcohol is 1; continuously adding an emulsifier, wherein the volume ratio of the mass of the emulsifier to the absolute ethyl alcohol is 1; obtaining an oil phase;
s3: preparing an emulsion: slowly and dropwise adding the oil phase obtained in the step S2 into the water phase solution obtained in the step S1, and stirring at normal temperature at the stirring speed of: 800r/min, stirring for 30min to obtain milky emulsion;
s4: preparing litsea cubeba essential oil nanoparticles: and (3) centrifuging the emulsion obtained in the step (S3) by using an ultrafiltration centrifugal tube, wherein the centrifugation speed is 12000r/min, the centrifugation time is 30min, discarding the supernatant, taking the lower layer, washing the particles by using distilled water, and carrying out vacuum freeze drying at-52 ℃ to obtain the litsea cubeba essential oil nanoparticles.
The litsea cubeba essential oil nanoparticles are applied to preservation of hot peppers.
Example 1
A preparation method of litsea cubeba essential oil nanoparticles comprises the following steps:
s1: preparing an aqueous phase solution: respectively transferring 0.18mL of spitting temperature and 0.18mL of span by using a liquid transfer gun, dissolving in 180mL of deionized water, accurately weighing 0.1000g of chitosan and 0.3000g of Arabic gum powder by using an electronic analytical balance, and dissolving the weighed chitosan and Arabic gum powder in the deionized water added with an emulsifying agent; stirring at 60 deg.C to dissolve completely, filtering at 0.45 μm, and adjusting pH to 4.0 to obtain water phase solution;
s2: preparing an oil phase: accurately measuring 0.1000g of litsea cubeba essential oil by using an electronic analytical balance, and dissolving in 2ml of absolute ethyl alcohol; continuously adding 0.4000g of emulsifier (Tween and span in a mass ratio of 1);
s3: preparing an emulsion: slowly and dropwise adding the oil phase obtained in the step S2 into the water phase solution obtained in the step S1, and stirring at normal temperature at the stirring speed of: 800r/min, stirring for 30min to obtain milk white emulsion;
s4: preparing litsea cubeba essential oil nanoparticles: and (4) centrifuging the emulsion obtained in the step (S3) by using an ultrafiltration centrifugal tube at the centrifugal speed of 12000r/min for 30min, removing a supernatant, taking a lower layer, washing particles by using distilled water, and carrying out vacuum freeze drying at the temperature of-52 ℃ to obtain the litsea cubeba essential oil nanoparticles.
Example 2
A preparation method of Litsea cubeba essential oil nanoparticles comprises the following steps:
s1: preparing an aqueous phase solution: respectively transferring 0.18mL of spitting temperature and 0.18mL of span by using a liquid transfer gun, dissolving the span into 180mL of deionized water, accurately weighing 0.1000g of chitosan and 0.3000g of Arabic gum powder by using an electronic analytical balance, and dissolving the weighed chitosan and Arabic gum powder into the deionized water added with an emulsifying agent; stirring at 60 deg.C until completely dissolved, filtering at 0.45 μm, and adjusting pH of the solution to 4.0 to obtain water phase solution;
s2: preparing an oil phase: accurately measuring 0.2000g of litsea cubeba essential oil by using an electronic analytical balance, and dissolving in 2ml of absolute ethyl alcohol; continuously adding 0.4000g of emulsifier (Tween and span in a mass ratio of 1);
s3: preparing an emulsion: slowly and dropwise adding the oil phase obtained in the step S2 into the water phase solution obtained in the step S1, and stirring at normal temperature at the stirring speed of: 800r/min, stirring for 30min to obtain milky emulsion;
s4: preparing litsea cubeba essential oil nanoparticles: and (3) centrifuging the emulsion obtained in the step (S3) by using an ultrafiltration centrifugal tube, wherein the centrifugation speed is 12000r/min, the centrifugation time is 30min, discarding the supernatant, taking the lower layer, washing the particles by using distilled water, and carrying out vacuum freeze drying at-52 ℃ to obtain the litsea cubeba essential oil nanoparticles.
Example 3
A preparation method of Litsea cubeba essential oil nanoparticles comprises the following steps:
s1: preparing an aqueous phase solution: respectively transferring 0.18mL of spitting temperature and 0.18mL of span by using a liquid transfer gun, dissolving the span into 180mL of deionized water, accurately weighing 0.1000g of chitosan and 0.3000g of Arabic gum powder by using an electronic analytical balance, and dissolving the weighed chitosan and Arabic gum powder into the deionized water added with an emulsifying agent; stirring at 60 deg.C to dissolve completely, filtering at 0.45 μm, and adjusting pH to 4.0 to obtain water phase solution;
s2: preparing an oil phase: accurately measuring 0.3000g of litsea cubeba essential oil by using an electronic analytical balance, and dissolving the litsea cubeba essential oil in 2ml of absolute ethyl alcohol; continuously adding 0.4000g of emulsifier (Tween and span in a mass ratio of 1;
s3: preparing an emulsion: slowly and dropwise adding the oil phase obtained in the step S2 into the water phase solution obtained in the step S1, and stirring at normal temperature at the stirring speed of: 800r/min, stirring for 30min to obtain milk white emulsion;
s4: preparing litsea cubeba essential oil nanoparticles: and (3) centrifuging the emulsion obtained in the step (S3) by using an ultrafiltration centrifugal tube, wherein the centrifugation speed is 12000r/min, the centrifugation time is 30min, discarding the supernatant, taking the lower layer, washing the particles by using distilled water, and carrying out vacuum freeze drying at-52 ℃ to obtain the litsea cubeba essential oil nanoparticles.
Example 4
A preparation method of litsea cubeba essential oil nanoparticles comprises the following steps:
s1: preparing an aqueous phase solution: respectively transferring 0.18mL of spitting temperature and 0.18mL of span by using a liquid transfer gun, dissolving the span into 180mL of deionized water, accurately weighing 0.1000g of chitosan and 0.3000g of Arabic gum powder by using an electronic analytical balance, and dissolving the weighed chitosan and Arabic gum powder into the deionized water added with an emulsifying agent; stirring at 60 deg.C until completely dissolved, filtering at 0.45 μm, and adjusting pH of the solution to 4.0 to obtain water phase solution;
s2: preparing an oil phase: accurately measuring 0.4000g of litsea cubeba essential oil by using an electronic analytical balance, and dissolving the litsea cubeba essential oil in 2ml of absolute ethyl alcohol; continuously adding 0.4000g of emulsifier (Tween and span in a mass ratio of 1);
s3: preparing an emulsion: slowly and dropwise adding the oil phase obtained in the step S2 into the water phase solution obtained in the step S1, and stirring at normal temperature at the stirring speed of: 800r/min, stirring for 30min to obtain milk white emulsion;
s4: preparing litsea cubeba essential oil nanoparticles: and (4) centrifuging the emulsion obtained in the step (S3) by using an ultrafiltration centrifugal tube at the centrifugal speed of 12000r/min for 30min, removing a supernatant, taking a lower layer, washing particles by using distilled water, and carrying out vacuum freeze drying at the temperature of-52 ℃ to obtain the litsea cubeba essential oil nanoparticles.
Example 5
A preparation method of litsea cubeba essential oil nanoparticles comprises the following steps:
s1: preparing an aqueous phase solution: respectively transferring 0.18mL of spitting temperature and 0.18mL of span by using a liquid transfer gun, dissolving in 180mL of deionized water, accurately weighing 0.1000g of chitosan and 0.3000g of Arabic gum powder by using an electronic analytical balance, and dissolving the weighed chitosan and Arabic gum powder in the deionized water added with an emulsifying agent; stirring at 60 deg.C to dissolve completely, filtering at 0.45 μm, and adjusting pH to 4.0 to obtain water phase solution;
s2: preparing an oil phase: accurately measuring 0.5000g of litsea cubeba essential oil by using an electronic analytical balance, and dissolving in 2ml of absolute ethyl alcohol; continuously adding 0.4000g of emulsifier (Tween and span in a mass ratio of 1;
s3: preparing an emulsion: slowly and dropwise adding the oil phase obtained in the step S2 into the water phase solution obtained in the step S1, and stirring at normal temperature at the stirring speed of: 800r/min, stirring for 30min to obtain milk white emulsion;
s4: preparing litsea cubeba essential oil nanoparticles: and (3) centrifuging the emulsion obtained in the step (S3) by using an ultrafiltration centrifugal tube, wherein the centrifugation speed is 12000r/min, the centrifugation time is 30min, discarding the supernatant, taking the lower layer, washing the particles by using distilled water, and carrying out vacuum freeze drying at-52 ℃ to obtain the litsea cubeba essential oil nanoparticles.
Comparative example 1
A preparation method of blank nanoparticles without adding litsea cubeba essential oil comprises the following steps:
s1: preparing an aqueous phase solution: respectively transferring 0.18mL of spitting temperature and 0.18mL of span by using a liquid transfer gun, dissolving in 180mL of deionized water, accurately weighing 0.1000g of chitosan and 0.3000g of Arabic gum powder by using an electronic analytical balance, and dissolving the weighed chitosan and Arabic gum powder in the deionized water added with an emulsifying agent; stirring at 60 deg.C to dissolve completely, filtering at 0.45 μm, and adjusting pH to 4.0 to obtain water phase solution;
s2: adding 0.4000g of emulsifier (Tween and span in a mass ratio of 1);
s3: slowly and dropwise adding the alcoholic solution obtained in the step S2 into the aqueous solution obtained in the step S1, and stirring at normal temperature at the stirring speed of: 800r/min, stirring for 30min to obtain a mixed solution;
s4: preparing blank nanoparticles without adding litsea cubeba essential oil: and (3) centrifuging the mixed solution obtained in the step (S3) by using an ultrafiltration centrifugal tube, wherein the centrifugation speed is 12000r/min, the centrifugation time is 30min, discarding the supernatant, taking the lower layer, washing the particles by using distilled water, and carrying out vacuum freeze drying at-52 ℃ to obtain the blank nanoparticles without adding the litsea cubeba essential oil.
Comparative example 2
A preparation method of litsea cubeba essential oil solution comprises the following steps:
accurately measuring 0.4000g of litsea cubeba essential oil by using an electronic analytical balance, and dissolving the litsea cubeba essential oil in 2ml of absolute ethyl alcohol; and continuously adding 0.4000g of emulsifier (Tween and span in a mass ratio of 1).
Effect example 1
Determination test of embedding rate:
determining the embedding rate of the litsea cubeba essential oil nanoparticles by adopting an ultrafiltration centrifugal tube, placing the litsea cubeba essential oil nanoparticles obtained in the examples 1 to 5 into the ultrafiltration centrifugal tube, and centrifuging at high speed of 12000r/min at 4 ℃ for 30min; taking supernatant in the upper layer centrifugal tube, and measuring the content of free essential oil by using an ultraviolet spectrophotometer at the wavelength of 235 nm; the blank nanoparticles in comparative example 1 were used as a control, and the embedding rate (EE%) was calculated according to the standard curve of Litsea cubeba essential oil, and the result is shown in FIG. 1.
The embedding rate (EE%) is the percentage of the active ingredient embedded by the nanoparticles in the colloidal solution to the total mass when added into the system. The encapsulation rate is high, the free amount in the solution is small, and the loss is small.
And (4) analyzing results:
fig. 1 shows the change trend of the nanoparticle embedding rate when the content of litsea cubeba essential oil is increased, and it can be seen that when the content of the essential oil is continuously increased, the embedding rate is in a trend of increasing first and then decreasing. When the addition amount of the litsea cubeba essential oil is 0.1-0.2%, namely, when the litsea cubeba essential oil is used in the examples 1-2, the embedding rate is obviously increased; the addition amount of the litsea cubeba essential oil is the percentage of the mass of the added litsea cubeba essential oil in the mass of the total solution; when the addition amount of the litsea cubeba essential oil is between 0.2 and 0.4 percent, namely, the addition amounts of the litsea cubeba essential oil in examples 2 to 4 are equal, the ascending trend of the embedding rate becomes slow, and the peak value (77.34 percent) is reached at 0.4 percent; example 5 the encapsulation efficiency began to decrease, mainly because when too much essential oil was added to the solution, the nanoparticle encapsulation capacity was limited, excess essential oil was free in the solution, and the encapsulation efficiency began to decrease. Therefore, the condition for preparing the litsea cubeba essential oil nanoparticles in example 2 is selected by taking the addition of 0.2% of the litsea cubeba essential oil into consideration of the integration of the addition and the embedding rate of the litsea cubeba.
Effect example 2:
appearance morphology observation test:
respectively taking equal amounts of the litsea cubeba essential oil nanoparticles obtained in the example 2 and the blank nanoparticles obtained in the comparative example 1, carrying out ultrasonic dyeing for 5min, carrying out counterstaining by using phosphotungstic acid with the mass fraction of 2%, placing on a copper mesh, naturally drying, placing on a sample table, and observing the appearance of particles by using a transmission electron microscope; the transmission electron microscope picture of the litsea cubeba essential oil nanoparticles in example 2 is shown in figure 2, and the transmission electron microscope picture of the hollow white nanoparticles in comparative example 1 is shown in figure 3.
And (4) analyzing results:
fig. 2 and 3 show that: the prepared nanoparticles are uniformly dispersed, have no agglomeration phenomenon, and have the average particle size of below 200 nm; as can be seen by observing the blank nanoparticles and the litsea cubeba essential oil nanoparticles, the quantity of the litsea cubeba essential oil nanoparticles is reduced compared with that of the blank nanoparticles, the dispersibility is improved, but the particle size difference of the essential oil nanoparticles is larger, so that the particle size is increased and the particle size is nonuniform due to the fact that the essential oil enters the nanoparticles.
Effect example 3
Determination of the Slow Release Performance:
preparing a phosphate buffer solution, preparing a Phosphate Buffer Solution (PBS) with pH7.4: potassium dihydrogen phosphate (KH 2PO 4): 0.27g, disodium hydrogen phosphate (Na 2HPO 4): 1.42g, sodium chloride (NaCl): 8g and 0.2g of potassium chloride (KCl), the volume is fixed to 1L, the pH value is adjusted to 7.4, and the mixture is sterilized and stored at 4 ℃ for standby.
Centrifuging the litsea cubeba essential oil nanoparticles obtained in the example 2 and the litsea cubeba essential oil solution obtained in the comparative example 2 respectively, adding buffer solutions into the solutions respectively, stirring the solutions mildly at 37 ℃, taking out a certain volume of the solution after a period of time, centrifuging the solution at 235nm, measuring the light absorption value of a supernatant, and supplementing the solution with an equal volume of buffer solution. Repeating for 3 times, and taking an average value; the in vitro release rate curve of fructus Litseae essential oil nanoparticles and fructus Litseae essential oil is shown in figure 4.
Release Rate = (Total essential oil content-measured essential oil content)/Total essential oil content
And (4) analyzing results:
as shown in fig. 4, the in vitro release rate of the Litsea cubeba essential oil nanoparticles and the Litsea cubeba essential oil was measured at 37 ℃; the release rate of the free litsea cubeba essential oil is much faster than that of the embedded litsea cubeba essential oil nanoparticles, and the release rate of the free litsea cubeba essential oil is in a continuously rising trend and has a significant difference with the nanoparticles. Because the particle size of the nanoparticles is small, the specific surface area is large, and a large amount of litsea cubeba essential oil is attached to the surfaces of the nanoparticles, the litsea cubeba essential oil nanoparticles are in two stages in the release process, the first stage refers to 1-10 hours, the free litsea cubeba essential oil attached to the surfaces of the nanoparticles is quickly released, the release rate of the litsea cubeba essential oil is high, the second stage is 10-30 hours, the litsea cubeba essential oil in the nanoparticles starts to be slowly released, the release rate is slowly increased, the release rate is 61.17% after 30 hours, and the release rate is reduced by 26.16% compared with the release rate of the free litsea cubeba essential oil (87.33%).
Effect example 4
Determination of decay index test:
evaluation of rotting grade:
level 0: no rotting phenomenon
Stage 1: the rotten area accounts for 0-10% of the total fruit area.
And 2, stage: the rotten area accounts for 10-30% of the total fruit area.
And 3, level: the rotten area accounts for 30-50% of the total fruit area.
And 4, stage 4: the rotten area accounts for 50-100% of the total fruit area.
Selecting pepper stored for 30 days, and treating the pepper with 1% chlorine dioxide in the same amount; blank processing; treating the blank nanoparticles obtained in comparative example 1; treatment of the litsea cubeba essential oil nanoparticles obtained in example 2 and treatment of capsicum prepared by litsea cubeba essential oil in comparative example 2; the effect of different treatments on the rotting rate of pepper when stored for 30 days is shown in fig. 5.
And (4) analyzing results:
during the storage period of the pepper, the basic metabolic activity is still carried out, the nutrient substances in the body are continuously consumed, the disease resistance is weakened, in addition, the water content of the pepper is higher, the pepper is easy to be infected by pathogenic bacteria, and the aging and putrefaction speed is accelerated. FIG. 5 shows the effect of treatment with various substances on the rotting rate of pepper fruits at day 30 of storage. The rotting rate of the blank treatment reaches 66.93 percent and is obviously higher than that of other treatments, wherein the rotting rate of 1 percent of chlorine dioxide treated pepper is 27.70 percent at least, the rotting rate of litsea cubeba essential oil treated pepper is 46.13 percent, the rotting rate of the litsea cubeba essential oil treated pepper is 38.96 percent, and chlorine dioxide has certain harmfulness when being used as an antistaling agent due to the physicochemical property of chlorine dioxide; the rotten rate of the pepper treated by the litsea cubeba essential oil nano particles is obviously smaller than that of the pepper treated by the blank treatment group and the litsea cubeba essential oil. The litsea cubeba essential oil treatment can inhibit the rotting and deterioration speed of the hot pepper, and the inhibition effect is enhanced after the nano embedding.
In conclusion:
at present, the pepper preservation technology mainly adopts a physical method and a chemical preservative, but the defects of the preservation methods are continuously highlighted, for example, chemical preservative is easy to have chemical reagent residues to cause damage to human bodies and the environment; the low-temperature storage has high energy consumption, and the cold damage of fruits is easily caused if the operation is improper; the controlled atmosphere storage investment is large, the requirement on the gas proportion is strict, and the stability is poor; the radiation fresh-keeping has very strict requirements on radiation use measurement and has higher operation difficulty; the common film fresh-keeping method is easy to cause the problems of microbial pollution, poor stability and the like due to the material problem.
The litsea cubeba essential oil is embedded in a nanometer mode by adopting the chitosan and the Arabic gum as composite wall materials, so that the stability of the litsea cubeba essential oil is improved, the release rate of active substances is controlled, and the active effects of the litsea cubeba essential oil such as bacteriostasis, antioxidation and the like can be effectively utilized.
The litsea cubeba essential oil is used as a raw material, and the nano embedded essential oil nanoparticles are used as a plant source preservative to be applied to the preservation of the hot pepper, so that the effect of preserving the hot pepper is good.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the technical scope of the present invention, so that any minor modifications, equivalent changes and modifications made to the above embodiment according to the technical spirit of the present invention are within the technical scope of the present invention.
Claims (10)
1. A Litsea cubeba essential oil nanoparticle is characterized in that; the method comprises the following raw materials: the gum comprises chitosan, arabic gum powder, an emulsifier and litsea cubeba essential oil, wherein the mass ratio of the chitosan to the Arabic gum powder is 1:5 to 1.
2. A preparation method of the litsea cubeba essential oil nanoparticles as claimed in claim 1, which is characterized in that; the method comprises the following steps:
s1: preparing an aqueous phase solution: transferring an emulsifying agent to dissolve in deionized water, respectively weighing chitosan and Arabic gum powder, dissolving the weighed chitosan and Arabic gum powder in the deionized water added with the emulsifying agent, stirring at 60 ℃ until the chitosan and Arabic gum powder are completely dissolved, filtering by 0.45 mu m, and adjusting the pH of the solution to 4.0 to obtain an aqueous solution;
s2: preparing an oil phase: dissolving litsea cubeba essential oil in absolute ethyl alcohol, wherein the volume ratio of the mass of the litsea cubeba essential oil to the absolute ethyl alcohol is 1; continuously adding an emulsifier to obtain an oil phase;
s3: preparing an emulsion: slowly and dropwise adding the oil phase obtained in the step S2 into the water phase solution obtained in the step S1, and stirring at normal temperature at the stirring speed of: 800r/min, stirring for 30min to obtain milk white emulsion;
s4: preparing litsea cubeba essential oil nanoparticles: and (3) centrifuging the emulsion obtained in the step (S3) by using an ultrafiltration centrifugal tube, wherein the centrifugation speed is 12000r/min, the centrifugation time is 30min, discarding the supernatant, taking the lower layer, washing the particles by using distilled water, and carrying out vacuum freeze drying at-52 ℃ to obtain the litsea cubeba essential oil nanoparticles.
3. The preparation method of the Litsea cubeba essential oil nanoparticles according to claim 1, which is characterized in that; the volume ratio of the emulsifier to the deionized water in the S1 is 1.
4. The preparation method of the Litsea cubeba essential oil nanoparticles according to claim 1, which is characterized in that; the mass ratio of the chitosan to the Arabic gum powder weighed in the S1 is 1.
5. The preparation method of the Litsea cubeba essential oil nanoparticles according to claim 1, which is characterized in that; the ratio of the mass of the chitosan to the volume of the emulsifier in the S1 is 5.
6. The preparation method of the litsea cubeba essential oil nanoparticles according to claim 1, characterized in that; the emulsifier is tween and span.
7. The method for preparing the litsea cubeba essential oil nanoparticles according to claim 6, which is characterized in that; the volume ratio of the temperature and span added is 1.
8. The preparation method of the litsea cubeba essential oil nanoparticles according to claim 1, characterized in that; the volume ratio of the mass of the litsea cubeba essential oil to the absolute ethyl alcohol in the S2 is 1.
9. The preparation method of the litsea cubeba essential oil nanoparticles according to claim 1, characterized in that; the volume ratio of the mass of the emulsifier in the S2 to the absolute ethyl alcohol is 1.
10. The use of the Litsea cubeba essential oil nanoparticles according to claim 1, wherein the nanoparticle comprises a major component selected from the group consisting of; the litsea cubeba essential oil nanoparticles are used for keeping the freshness of the hot pepper.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211548544.2A CN115736007A (en) | 2022-12-05 | 2022-12-05 | Litsea cubeba essential oil nanoparticles, preparation method thereof and application thereof in pepper preservation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211548544.2A CN115736007A (en) | 2022-12-05 | 2022-12-05 | Litsea cubeba essential oil nanoparticles, preparation method thereof and application thereof in pepper preservation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115736007A true CN115736007A (en) | 2023-03-07 |
Family
ID=85343200
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211548544.2A Pending CN115736007A (en) | 2022-12-05 | 2022-12-05 | Litsea cubeba essential oil nanoparticles, preparation method thereof and application thereof in pepper preservation |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115736007A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103340195A (en) * | 2013-07-16 | 2013-10-09 | 东北林业大学 | Black pepper refined oil microcapsule taking chitosan and Arabic gum as wall materials and preparation method of black pepper refined oil microcapsule |
| CN107307403A (en) * | 2017-07-12 | 2017-11-03 | 日照职业技术学院 | A kind of astaxanthin micro and nano powders preparation |
| CN112544695A (en) * | 2020-10-16 | 2021-03-26 | 浙江杭化新材料科技有限公司 | Interlayer paper for fruit and vegetable fresh-keeping |
| CN113440479A (en) * | 2021-07-14 | 2021-09-28 | 南京师范大学 | Nano emulsion of plant essential oil and preparation method and application thereof |
-
2022
- 2022-12-05 CN CN202211548544.2A patent/CN115736007A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103340195A (en) * | 2013-07-16 | 2013-10-09 | 东北林业大学 | Black pepper refined oil microcapsule taking chitosan and Arabic gum as wall materials and preparation method of black pepper refined oil microcapsule |
| CN107307403A (en) * | 2017-07-12 | 2017-11-03 | 日照职业技术学院 | A kind of astaxanthin micro and nano powders preparation |
| CN112544695A (en) * | 2020-10-16 | 2021-03-26 | 浙江杭化新材料科技有限公司 | Interlayer paper for fruit and vegetable fresh-keeping |
| CN113440479A (en) * | 2021-07-14 | 2021-09-28 | 南京师范大学 | Nano emulsion of plant essential oil and preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| 付红军: "山苍子油的提取效果及其防腐保鲜研究", 《中国优秀博士学位论文全文数据库电子期刊》 * |
| 刘占东;李璐;全国芬;丁武;: "肉桂精油壳聚糖纳米粒在冷却肉保藏中的应用", 西北农林科技大学学报(自然科学版), no. 05, pages 194 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Deladino et al. | Encapsulation of natural antioxidants extracted from Ilex paraguariensis | |
| CN113397081B (en) | Preparation method of epsilon-polylysine-acacia nano-particles | |
| Uscategui et al. | Concentrates of sugarcane juice and whey protein: Study of a new powder product obtained by spray drying of their combinations | |
| CN110250263A (en) | A kind of method of fertile mandarin orange keeping-freshness storage | |
| Benitez et al. | Effect of gelatin on apple juice turbidity | |
| Soto‐Muñoz et al. | Starch‐based antifungal edible coatings to control sour rot caused by Geotrichum citri‐aurantii and maintain postharvest quality of ‘Fino’lemon | |
| CN115736007A (en) | Litsea cubeba essential oil nanoparticles, preparation method thereof and application thereof in pepper preservation | |
| Huie et al. | Microporous chitosan/polyvinyl alcohol based active packaging materials with integrated gas-transmission, radiation-cooling, anti-microbial, and ultraviolet shielding features | |
| Prommajak et al. | Optimizing tannin precipitation in cashew apple juice | |
| CN114600953A (en) | Preservative, preparation method thereof, preservative film solution and application thereof | |
| CN106387030B (en) | A kind of preparation method of sliver sea lettuce polysaccharide-chitosan compounding essential oil lotion | |
| CN109730318A (en) | It is a kind of improve fraise glycosides stability composition and its application | |
| Songkro et al. | Microencapsulation of citronella oil for mosquito repellent: Preparation and evaluation of release characteristics. | |
| Liu et al. | Preparation and application of chlorine dioxide gas slow-release fresh-keeping card based on polylactic acid | |
| CN110403919A (en) | A kind of preparation method of rouge radish thionin capsule of nano | |
| CN107604752B (en) | Preparation method of chromogenic antibacterial sucrose packaging paper | |
| Cuevas-Glory et al. | Spray drying and process optimization of sour orange juice | |
| Corrêa et al. | Spray drying of coffee leaf extract | |
| CN109090220B (en) | Preservative and fresh-keeping liquid and application thereof in preservative and fresh-keeping of citrus fruits | |
| CN110279122A (en) | A method of high-protein nutrient stick cohesion is improved by addition phospholipid capsule bubble | |
| CN111758771A (en) | Microcapsule for inhibiting potato germination and preparation method and application thereof | |
| Ziaolhagh | Effects of some salts on the shelf life of Shahrood Sorkh-e-Fakhri table grapes stored in cold storage. | |
| EP0085589B1 (en) | Processes for the preparation of fresh stabilised cell suspensions for pharmaceutical, cosmetic and alimentary use | |
| CN108708218A (en) | A kind of food fresh keeping tectorial paper and preparation method thereof | |
| CN108835238A (en) | A kind of fruits and vegetables nanometer fresh-keeping agent and preparation method thereof |
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 |