CN112220017A - Preparation method of propolis volatile oil nano complex by taking silk fibroin as wall material - Google Patents
Preparation method of propolis volatile oil nano complex by taking silk fibroin as wall material Download PDFInfo
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- CN112220017A CN112220017A CN202010990358.9A CN202010990358A CN112220017A CN 112220017 A CN112220017 A CN 112220017A CN 202010990358 A CN202010990358 A CN 202010990358A CN 112220017 A CN112220017 A CN 112220017A
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- 229940069949 propolis Drugs 0.000 title claims abstract description 138
- 239000000341 volatile oil Substances 0.000 title claims abstract description 118
- 241000241413 Propolis Species 0.000 title claims abstract description 109
- 108010022355 Fibroins Proteins 0.000 title claims abstract description 31
- 239000000463 material Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002114 nanocomposite Substances 0.000 claims abstract description 34
- 238000002474 experimental method Methods 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 27
- 239000000126 substance Substances 0.000 claims abstract description 10
- 238000012360 testing method Methods 0.000 claims abstract description 4
- IPZIYGAXCZTOMH-UHFFFAOYSA-N alpha-eudesmol Natural products CC1=CCCC2CCC(CC12)C(C)(C)O IPZIYGAXCZTOMH-UHFFFAOYSA-N 0.000 claims description 18
- WWULHQLTPGKDAM-UHFFFAOYSA-N gamma-eudesmol Natural products CC(C)C1CC(O)C2(C)CCCC(=C2C1)C WWULHQLTPGKDAM-UHFFFAOYSA-N 0.000 claims description 18
- 239000003814 drug Substances 0.000 claims description 15
- 238000005538 encapsulation Methods 0.000 claims description 13
- 229940079593 drug Drugs 0.000 claims description 12
- 238000011068 loading method Methods 0.000 claims description 12
- 230000008859 change Effects 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 238000005070 sampling Methods 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 9
- WEEGYLXZBRQIMU-UHFFFAOYSA-N Eucalyptol Chemical compound C1CC2CCC1(C)OC2(C)C WEEGYLXZBRQIMU-UHFFFAOYSA-N 0.000 claims description 6
- 229930007050 cineol Natural products 0.000 claims description 6
- 229960005233 cineole Drugs 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- 238000011156 evaluation Methods 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 238000001694 spray drying Methods 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 238000013112 stability test Methods 0.000 claims description 4
- CTKXFMQHOOWWEB-UHFFFAOYSA-N Ethylene oxide/propylene oxide copolymer Chemical compound CCCOC(C)COCCO CTKXFMQHOOWWEB-UHFFFAOYSA-N 0.000 claims description 3
- 230000001804 emulsifying effect Effects 0.000 claims description 3
- 238000005286 illumination Methods 0.000 claims description 3
- 230000001678 irradiating effect Effects 0.000 claims description 3
- 229920001993 poloxamer 188 Polymers 0.000 claims description 3
- 229940044519 poloxamer 188 Drugs 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 3
- 230000001954 sterilising effect Effects 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 230000004071 biological effect Effects 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 15
- 238000000605 extraction Methods 0.000 description 7
- 238000012545 processing Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 235000013871 bee wax Nutrition 0.000 description 2
- 239000012166 beeswax Substances 0.000 description 2
- 235000013599 spices Nutrition 0.000 description 2
- 150000003505 terpenes Chemical class 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 235000008708 Morus alba Nutrition 0.000 description 1
- 240000000249 Morus alba Species 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 150000007824 aliphatic compounds Chemical class 0.000 description 1
- 230000003260 anti-sepsis Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000006286 aqueous extract Substances 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229940079919 digestives enzyme preparation Drugs 0.000 description 1
- 239000008157 edible vegetable oil Substances 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 235000021190 leftovers Nutrition 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000000874 microwave-assisted extraction Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000004854 plant resin Substances 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 210000003079 salivary gland Anatomy 0.000 description 1
- 230000028327 secretion Effects 0.000 description 1
- 229930004725 sesquiterpene Natural products 0.000 description 1
- 150000004354 sesquiterpene derivatives Chemical class 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
- 239000011345 viscous material Substances 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L21/00—Marmalades, jams, jellies or the like; Products from apiculture; Preparation or treatment thereof
- A23L21/20—Products from apiculture, e.g. royal jelly or pollen; Substitutes therefor
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
- A23P10/00—Shaping or working of foodstuffs characterised by the products
- A23P10/30—Encapsulation of particles, e.g. foodstuff additives
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K35/00—Medicinal preparations containing materials or reaction products thereof with undetermined constitution
- A61K35/56—Materials from animals other than mammals
- A61K35/63—Arthropods
- A61K35/64—Insects, e.g. bees, wasps or fleas
- A61K35/644—Beeswax; Propolis; Royal jelly; Honey
-
- 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
- A61K9/51—Nanocapsules; Nanoparticles
- A61K9/5107—Excipients; Inactive ingredients
- A61K9/513—Organic macromolecular compounds; Dendrimers
- A61K9/5169—Proteins, e.g. albumin, gelatin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P1/00—Drugs for disorders of the alimentary tract or the digestive system
- A61P1/16—Drugs for disorders of the alimentary tract or the digestive system for liver or gallbladder disorders, e.g. hepatoprotective agents, cholagogues, litholytics
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P29/00—Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID]
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/04—Antibacterial agents
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P35/00—Antineoplastic agents
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P39/00—General protective or antinoxious agents
- A61P39/06—Free radical scavengers or antioxidants
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y5/00—Nanobiotechnology or nanomedicine, e.g. protein engineering or drug delivery
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- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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Abstract
The invention belongs to the technical field of propolis volatile oil, and discloses a preparation method of a propolis volatile oil nano complex by taking silk fibroin as a wall material, which comprises the following steps: firstly, preparing a natural nano complex of silk fibroin-propolis volatile oil; secondly, orthogonal test; thirdly, detecting the physical and chemical properties of the natural nano complex of the silk fibroin-propolis volatile oil; and fourthly, performing stability experiment on the natural nano complex of the silk fibroin-propolis volatile oil. According to the scheme, the natural silk fibroin is used as a wall material to embed the propolis volatile oil, the natural nano-composite technology is optimized, the physical and chemical properties of the natural nano-composite product are detected, and the stability of the natural nano-composite product is considered, so that the stable and reliable preparation technology of the propolis volatile oil natural nano-composite with the silk fibroin as the wall material is obtained, the propolis volatile oil natural nano-composite product with high safety and natural environmental protection is developed, and the method has important significance for maintaining the original characteristics and fully exerting the biological activity of the propolis volatile oil.
Description
Technical Field
The invention relates to the technical field of propolis volatile oil, in particular to a preparation method of a propolis volatile oil nano-complex taking silk fibroin as a wall material.
Background
Propolis is a viscous substance obtained by collecting plant resin from bee (Apisme llifera), mixing with salivary gland secretion, beeswax, pollen, etc., and has pungent and fragrant taste. The propolis has complex components, is composed of about 55% of resin and resina arborescens, about 30% of beeswax, 10% of aromatic volatile oil and 5% of pollen and sundries, and has multiple biological activities of protecting liver, resisting tumor, inhibiting bacteria, resisting inflammation, resisting oxidation and the like. The volatile oil is one of important biological active components in the propolis, is a main source of special fragrance of the propolis, and is beneficial to the propolis to play the effects of antisepsis, bacteriostasis, insect expelling and the like in a honeycomb. Researches show that the propolis volatile oil is very complex in chemical components and mainly comprises terpenoids, aliphatic compounds, aromatic compounds and the like.
The existing propolis products are mainly capsules, tablets or tinctures prepared from aqueous extracts or alcohol extracts of propolis, non-volatile components in the propolis are utilized, and volatile oil serving as an important component of the biological activity of the propolis is not fully utilized. In recent years, with the analysis of the components of the propolis volatile oil, the optimization of the extraction method and the research on biological activity, the propolis volatile oil gradually becomes a research and development hotspot of propolis products.
The domestic and foreign researches on the propolis volatile oil mainly focus on the component analysis and extraction method of the propolis volatile oil: the extraction method of propolis volatile oil mainly comprises steam steamingDistillation extraction method, ultrasonic and microwave assisted extraction method, and supercritical CO2Extraction methods, and the like. The extraction yield of the propolis volatile oil extracted by different methods is different from 1 percent to 15 percent; the identification of chemical components in the propolis volatile oil shows that the propolis volatile oil contains a large amount of terpenes, sesquiterpenes and derivatives thereof with biological activity.
Because the propolis volatile oil is unstable in a strong acid or strong alkaline medium, is easy to discolor, is easy to oxidize in the air and is very easy to volatilize, the application of the propolis volatile oil is limited to a certain extent by the characteristics. The natural nano-composite of the propolis volatile oil can well protect the propolis volatile oil from external adverse factors (such as light, oxygen, temperature and humidity) so as to protect the original characteristics of the propolis volatile oil and more fully exert the biological effect of the propolis volatile oil.
The natural nano-composite can make the substance obtain one special function or simultaneously obtain multiple functions, and has multiple applications in the aspects of preserving spices and spices, improving the quality of edible oil and fat, maintaining the activity of enzyme preparations and the like. At present, the influence factors of the application of the natural nano-composite technology in the food industry are mainly related to the high cost, the safety performance of wall materials, equipment and methods, so that the application of the economical, safe and high-performance wall materials, the improvement of the natural nano-composite technology method, the development of new products and the like are new directions of the technical research.
Disclosure of Invention
Technical problem to be solved
1. Technical problem to be solved
Aiming at the problems in the prior art, the invention aims to provide a preparation method of a propolis volatile oil nano complex taking silk fibroin as a wall material, and solves the problems.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme:
the preparation method of the propolis volatile oil nano complex with silk fibroin as a wall material comprises the following steps:
firstly, preparing a natural nano complex of silk fibroin-propolis volatile oil:
(1) measuring a certain concentration of silk fibroin solution in a beaker with the volume of 100mL to 500mL, adding a certain amount of propolis volatile oil in the beaker, emulsifying the solution for 2min at the speed of 10000r/min by using a high-speed homogenizer, and then stirring for 5min at a constant speed in a magnetic stirrer;
(2) carrying out spray drying on the uniformly stirred solution by using a high-speed spray dryer at the conditions of the inlet temperature of 190 ℃ and the outlet temperature of 80 ℃ at the sample introduction speed of 15mL/min, and sealing a sample to be tested after the spray drying is finished;
II, orthogonal test:
on the basis of a preliminary experiment and a single-factor experiment, the optimal combination of the core-wall ratio, the temperature and the time in the process of preparing the natural nano complex is determined by an orthogonal experiment, and the experiment is carried out by taking the comprehensive evaluation value of the natural nano complex as a survey index, wherein the comprehensive evaluation value is that the yield of the inclusion compound is multiplied by 30 percent and the embedding rate of the propolis volatile oil is multiplied by 70 percent.
Thirdly, detecting the physical and chemical properties of the natural nano complex of the silk fibroin-propolis volatile oil:
the quality of the silk fibroin-propolis volatile oil natural nano complex is evaluated by detecting the physicochemical properties of the propolis volatile oil natural nano complex product, such as appearance, embedding rate, yield, solubility, water content, propolis volatile oil content determination, drug loading rate and encapsulation rate determination, particle size determination and the like;
fourthly, a stability experiment of the natural nano complex of the silk fibroin-propolis volatile oil:
the influence of the stability of the natural nano-composite product of illumination, oxygen and humidity is inspected, so that the optimized formula and the reasonable natural nano-composite of the silk fibroin-propolis volatile oil and the process flow are obtained.
Preferably, the method for measuring the content of the silk fibroin-propolis volatile oil natural nano complex propolis volatile oil comprises the following steps: selecting characteristic component cineol in propolis volatile oil, and determining the content of cineol in the original medicine and the inclusion compound by GC.
Preferably, the method for measuring the drug loading and the encapsulation efficiency comprises the following steps: measuring the content of eudesmol in the propolis volatile oil to measure the propolis drug loading rate and the encapsulation rate, wherein the drug loading rate (%) is (the total input amount of the propolis volatile oil-the volatile oil amount of the propolis free in the solution/the total silk fibroin protein amount) × 100%, and the encapsulation rate (%) is (the total input amount of the propolis volatile oil (calculated by eudesmol) -the volatile oil amount of the propolis free in the solution)/the total input amount of the propolis volatile oil (calculated by eudesmol) × 100%.
Preferably, the method for measuring the particle size is as follows: taking appropriate amount of the natural nanometer complex of silk fibroin-propolis volatile oil, dispersing with 0.3% poloxamer 188 solution to make the final concentration of the natural nanometer complex of propolis volatile oil 0.1mg/mL, vortex oscillating for 10min, and determining particle size with Zeta potential analyzer.
Preferably, the silk fibroin-propolis volatile oil natural nano complex stability experiment comprises a light stability experiment, a heat stability experiment and a high humidity stability experiment.
Preferably, the light stability test is as follows: weighing the clathrate and the mixture, sealing, sterilizing at 100 deg.C for 30 min, irradiating under 220V300W incandescent lamp for 12d, sampling at 0, 4, 8, and 12 days, and determining eudesmol content change.
Preferably, the thermal stability test is: weighing the clathrate and the mixture, standing at 40 deg.C, 60 deg.C and 80 deg.C for 12 days, sampling at 0, 4, 8 and 12 days, and measuring eudesmol content change.
Preferably, the high humidity stability test is as follows: weighing appropriate amount of clathrate and mixture, standing at room temperature for 12 days under relative humidity of 75% and 95%, respectively, sampling at 0, 4, 8, and 12 days, and determining eudesmol content change.
(III) advantageous effects
Compared with the prior art, the invention provides a preparation method of the propolis volatile oil nano complex by taking silk fibroin as a wall material, which has the following beneficial effects:
(1) according to the scheme, natural silk fibroin with excellent biodegradability and biocompatibility is used as a wall material to embed the propolis volatile oil, a natural nano-composite preparation process is optimized, the physical and chemical properties of a natural nano-composite product are detected, the stability of the natural nano-composite product is considered, so that a stable and reliable preparation process of the propolis volatile oil natural nano-composite with the silk fibroin as the wall material is obtained, the propolis volatile oil in propolis processing residues is developed and utilized, a high-safety, natural and environment-friendly propolis volatile oil natural nano-composite product is developed, and the important significance is achieved for maintaining the original characteristics of the propolis volatile oil and fully exerting the biological activity.
(2) The fibroin, as a natural protein, has good biodegradability, biocompatibility and outstanding mechanical strength, so that the silk fibroin is used for preparing a micro-encapsulation system, the propolis volatile oil is encapsulated and embedded, the storage characteristic and the absorption availability of the propolis volatile oil are further improved, and an attractive novel approach is provided for deep processing and comprehensive utilization of propolis
(2) The propolis volatile oil is widely existed in leftovers of products of alcohol extraction propolis and water extraction propolis, and the fibroin can also be obtained in large quantity by utilizing processing scraps of mulberry silk, so that the utilization of the propolis volatile oil not only can be used as beneficial supplement of the existing propolis product, but also is an entry point of deep processing of the propolis, and theoretical basis and experimental basis are provided for improving the additional value of the propolis volatile oil product and comprehensively utilizing propolis resources.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The preparation method of the propolis volatile oil nano complex with silk fibroin as a wall material comprises the following steps:
firstly, preparing a natural nano complex of silk fibroin-propolis volatile oil:
(1) measuring a certain concentration of silk fibroin solution in a beaker with the volume of 100mL to 500mL, adding a certain amount of propolis volatile oil in the beaker, emulsifying the solution for 2min at the speed of 10000r/min by using a high-speed homogenizer, and then stirring for 5min at a constant speed in a magnetic stirrer;
(2) carrying out spray drying on the uniformly stirred solution by using a high-speed spray dryer at the conditions of the inlet temperature of 190 ℃ and the outlet temperature of 80 ℃ at the sample introduction speed of 15mL/min, and sealing a sample to be tested after the spray drying is finished;
II, orthogonal test:
on the basis of a preliminary experiment and a single-factor experiment, the optimal combination of the core-wall ratio, the temperature and the time in the process of preparing the natural nano complex is determined by an orthogonal experiment, and the experiment is carried out by taking the comprehensive evaluation value of the natural nano complex as a survey index, wherein the comprehensive evaluation value is that the yield of the inclusion compound is multiplied by 30 percent and the embedding rate of the propolis volatile oil is multiplied by 70 percent.
Thirdly, detecting the physical and chemical properties of the natural nano complex of the silk fibroin-propolis volatile oil:
the quality of the silk fibroin-propolis volatile oil natural nano complex is evaluated by detecting the physicochemical properties of the propolis volatile oil natural nano complex product, such as appearance, embedding rate, yield, solubility, water content, propolis volatile oil content determination, drug loading rate and encapsulation rate determination, particle size determination and the like;
fourthly, a stability experiment of the natural nano complex of the silk fibroin-propolis volatile oil:
the influence of the stability of the natural nano-composite product of illumination, oxygen and humidity is inspected, so that the optimized formula and the reasonable natural nano-composite of the silk fibroin-propolis volatile oil and the process flow are obtained.
Further, the method for measuring the content of the silk fibroin-propolis volatile oil natural nano complex propolis volatile oil comprises the following steps: selecting characteristic component cineol in propolis volatile oil, and determining the content of cineol in the original medicine and the inclusion compound by GC.
Further, the method for measuring the drug loading rate and the encapsulation efficiency comprises the following steps: the propolis drug loading and encapsulation rate are measured by measuring the eudesmol content in the propolis volatile oil, wherein the drug loading rate (%) is (total input amount of the propolis volatile oil-propolis volatile oil amount free in a solution/total silk fibroin protein amount) multiplied by 100%, and the encapsulation rate (%) is (total input amount of the propolis volatile oil (calculated by eudesmol) -propolis volatile oil amount free in the solution)/total input amount of the propolis volatile oil (calculated by eudesmol) multiplied by 100%.
Further, the particle size measurement method comprises the following steps: taking appropriate amount of the natural nanometer complex of silk fibroin-propolis volatile oil, dispersing with 0.3% poloxamer 188 solution to make the final concentration of the natural nanometer complex of propolis volatile oil 0.1mg/mL, vortex oscillating for 10min, and determining particle size with Zeta potential analyzer.
Further, the stability experiments of the silk fibroin-propolis volatile oil natural nano complex comprise a light stability experiment, a heat stability experiment and a high humidity stability experiment.
Further, the light stability experiment was: weighing the clathrate and the mixture, sealing, sterilizing at 100 deg.C for 30 min, irradiating under 220V300W incandescent lamp for 12d, sampling at 0, 4, 8, and 12 days, and determining eudesmol content change.
Further, the thermal stability experiment was: weighing the clathrate and the mixture, standing at 40 deg.C, 60 deg.C and 80 deg.C for 12 days, sampling at 0, 4, 8 and 12 days, and measuring eudesmol content change.
Further, the high humidity stability experiment was: weighing appropriate amount of clathrate and mixture, standing at room temperature for 12 days under relative humidity of 75% and 95%, respectively, sampling at 0, 4, 8, and 12 days, and determining eudesmol content change.
In summary, the following steps: according to the scheme, natural silk fibroin with good biodegradability and biocompatibility is used as a wall material to embed the propolis volatile oil, the natural nano-composite preparation process is optimized, the physical and chemical properties of the natural nano-composite product are detected, the stability of the natural nano-composite product is inspected, and therefore the stable and reliable preparation process of the propolis volatile oil natural nano-composite with the silk fibroin as the wall material is obtained.
The foregoing is only a preferred embodiment of the present invention; the scope of the invention is not limited thereto. Any person skilled in the art should be able to cover the technical scope of the present invention by equivalent or modified solutions and modifications within the technical scope of the present invention.
Claims (8)
1. The preparation method of the propolis volatile oil nano complex taking silk fibroin as a wall material is characterized by comprising the following steps: the method comprises the following steps:
firstly, preparing a natural nano complex of silk fibroin-propolis volatile oil:
(1) measuring a certain concentration of silk fibroin solution in a beaker with the volume of 100mL to 500mL, adding a certain amount of propolis volatile oil in the beaker, emulsifying the solution for 2min at the speed of 10000r/min by using a high-speed homogenizer, and then stirring for 5min at a constant speed in a magnetic stirrer;
(2) carrying out spray drying on the uniformly stirred solution by using a high-speed spray dryer at the conditions of the inlet temperature of 190 ℃ and the outlet temperature of 80 ℃ at the sample introduction speed of 15mL/min, and sealing a sample to be tested after the spray drying is finished;
II, orthogonal test:
on the basis of a preliminary experiment and a single-factor experiment, the optimal combination of the core-wall ratio, the temperature and the time in the process of preparing the natural nano complex is determined by an orthogonal experiment, and the experiment is carried out by taking the comprehensive evaluation value of the natural nano complex as a survey index, wherein the comprehensive evaluation value is that the yield of the inclusion compound is multiplied by 30 percent and the embedding rate of the propolis volatile oil is multiplied by 70 percent.
Thirdly, detecting the physical and chemical properties of the natural nano complex of the silk fibroin-propolis volatile oil:
the quality of the silk fibroin-propolis volatile oil natural nano complex is evaluated by detecting the physicochemical properties of the propolis volatile oil natural nano complex product, such as appearance, embedding rate, yield, solubility, water content, propolis volatile oil content determination, drug loading rate and encapsulation rate determination, particle size determination and the like;
fourthly, a stability experiment of the natural nano complex of the silk fibroin-propolis volatile oil:
the influence of the stability of the natural nano-composite product of illumination, oxygen and humidity is inspected, so that the optimized formula and the reasonable natural nano-composite of the silk fibroin-propolis volatile oil and the process flow are obtained.
2. The method for preparing the propolis volatile oil nanocomposite taking silk fibroin as a wall material as claimed in claim 1, which is characterized in that: the method for measuring the content of the silk fibroin-propolis volatile oil natural nano complex propolis volatile oil comprises the following steps: selecting characteristic component cineol in propolis volatile oil, and determining the content of cineol in the original medicine and the inclusion compound by GC.
3. The method for preparing the propolis volatile oil nanocomposite taking silk fibroin as a wall material as claimed in claim 1, which is characterized in that: the method for measuring the drug loading rate and the encapsulation efficiency comprises the following steps: measuring the content of eudesmol in the propolis volatile oil to measure the propolis drug loading rate and the encapsulation rate, wherein the drug loading rate (%) is (the total input amount of the propolis volatile oil-the volatile oil amount of the propolis free in the solution/the total silk fibroin protein amount) × 100%, and the encapsulation rate (%) is (the total input amount of the propolis volatile oil (calculated by eudesmol) -the volatile oil amount of the propolis free in the solution)/the total input amount of the propolis volatile oil (calculated by eudesmol) × 100%.
4. The method for preparing the propolis volatile oil nanocomposite taking silk fibroin as a wall material as claimed in claim 1, which is characterized in that: the particle size measuring method comprises the following steps: taking appropriate amount of the natural nanometer complex of silk fibroin-propolis volatile oil, dispersing with 0.3% poloxamer 188 solution to make the final concentration of the natural nanometer complex of propolis volatile oil 0.1mg/mL, vortex oscillating for 10min, and determining particle size with Zeta potential analyzer.
5. The method for preparing the propolis volatile oil nanocomposite taking silk fibroin as a wall material as claimed in claim 1, which is characterized in that: the silk fibroin-propolis volatile oil natural nano complex stability experiment comprises a light stability experiment, a heat stability experiment and a high humidity stability experiment.
6. The method for preparing the propolis volatile oil nanocomposite taking silk fibroin as a wall material as claimed in claim 5, wherein the propolis volatile oil nanocomposite comprises the following steps: the photostability experiment was: weighing the clathrate and the mixture, sealing, sterilizing at 100 deg.C for 30 min, irradiating under 220V300W incandescent lamp for 12d, sampling at 0, 4, 8, and 12 days, and determining eudesmol content change.
7. The method for preparing the propolis volatile oil nanocomposite taking silk fibroin as a wall material as claimed in claim 5, wherein the propolis volatile oil nanocomposite comprises the following steps: the thermal stability experiment was: weighing the clathrate and the mixture, standing at 40 deg.C, 60 deg.C and 80 deg.C for 12 days, sampling at 0, 4, 8 and 12 days, and measuring eudesmol content change.
8. The method for preparing the propolis volatile oil nanocomposite taking silk fibroin as a wall material as claimed in claim 5, wherein the propolis volatile oil nanocomposite comprises the following steps: the high humidity stability test was: weighing appropriate amount of clathrate and mixture, standing at room temperature for 12 days under relative humidity of 75% and 95%, respectively, sampling at 0, 4, 8, and 12 days, and determining eudesmol content change.
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| CN115337247A (en) * | 2022-07-21 | 2022-11-15 | 安徽中医药大学 | Propolis volatile oil coating and preparation method of toothpaste prepared from same |
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| JP5643912B1 (en) * | 2014-05-12 | 2014-12-17 | 株式会社えがお | Propolis extract and method for producing the same, capsule, and antioxidant |
| CN107041549A (en) * | 2017-04-14 | 2017-08-15 | 广西大学 | A kind of preparation method of garlic oil microscapsule powder |
| CN110859776A (en) * | 2019-11-29 | 2020-03-06 | 苏州丝美特生物技术有限公司 | Silk fibroin-based nanoemulsion and preparation method and application thereof |
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| JP5643912B1 (en) * | 2014-05-12 | 2014-12-17 | 株式会社えがお | Propolis extract and method for producing the same, capsule, and antioxidant |
| CN107041549A (en) * | 2017-04-14 | 2017-08-15 | 广西大学 | A kind of preparation method of garlic oil microscapsule powder |
| CN110859776A (en) * | 2019-11-29 | 2020-03-06 | 苏州丝美特生物技术有限公司 | Silk fibroin-based nanoemulsion and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115337247A (en) * | 2022-07-21 | 2022-11-15 | 安徽中医药大学 | Propolis volatile oil coating and preparation method of toothpaste prepared from same |
| CN115337247B (en) * | 2022-07-21 | 2023-12-22 | 安徽中医药大学 | Propolis volatile oil coating and preparation method of toothpaste prepared from propolis volatile oil coating |
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