CN115531240B - Cannabidiol emulsion and preparation method thereof - Google Patents
Cannabidiol emulsion and preparation method thereof Download PDFInfo
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- CN115531240B CN115531240B CN202211144804.XA CN202211144804A CN115531240B CN 115531240 B CN115531240 B CN 115531240B CN 202211144804 A CN202211144804 A CN 202211144804A CN 115531240 B CN115531240 B CN 115531240B
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- cannabidiol
- emulsion
- marine collagen
- emulsifier
- marine
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- QHMBSVQNZZTUGM-UHFFFAOYSA-N Trans-Cannabidiol Natural products OC1=CC(CCCCC)=CC(O)=C1C1C(C(C)=C)CCC(C)=C1 QHMBSVQNZZTUGM-UHFFFAOYSA-N 0.000 title claims abstract description 250
- QHMBSVQNZZTUGM-ZWKOTPCHSA-N cannabidiol Chemical compound OC1=CC(CCCCC)=CC(O)=C1[C@H]1[C@H](C(C)=C)CCC(C)=C1 QHMBSVQNZZTUGM-ZWKOTPCHSA-N 0.000 title claims abstract description 250
- 229950011318 cannabidiol Drugs 0.000 title claims abstract description 250
- ZTGXAWYVTLUPDT-UHFFFAOYSA-N cannabidiol Natural products OC1=CC(CCCCC)=CC(O)=C1C1C(C(C)=C)CC=C(C)C1 ZTGXAWYVTLUPDT-UHFFFAOYSA-N 0.000 title claims abstract description 250
- PCXRACLQFPRCBB-ZWKOTPCHSA-N dihydrocannabidiol Natural products OC1=CC(CCCCC)=CC(O)=C1[C@H]1[C@H](C(C)C)CCC(C)=C1 PCXRACLQFPRCBB-ZWKOTPCHSA-N 0.000 title claims abstract description 250
- 239000000839 emulsion Substances 0.000 title claims abstract description 178
- 238000002360 preparation method Methods 0.000 title abstract description 19
- 238000004945 emulsification Methods 0.000 title description 2
- 102000008186 Collagen Human genes 0.000 claims abstract description 83
- 108010035532 Collagen Proteins 0.000 claims abstract description 83
- 229920001436 collagen Polymers 0.000 claims abstract description 83
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 69
- 150000001875 compounds Chemical class 0.000 claims abstract description 45
- 239000002562 thickening agent Substances 0.000 claims abstract description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 150000001298 alcohols Chemical class 0.000 claims abstract description 4
- HIQIXEFWDLTDED-UHFFFAOYSA-N 4-hydroxy-1-piperidin-4-ylpyrrolidin-2-one Chemical compound O=C1CC(O)CN1C1CCNCC1 HIQIXEFWDLTDED-UHFFFAOYSA-N 0.000 claims description 36
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 31
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 31
- 229920000053 polysorbate 80 Polymers 0.000 claims description 31
- 238000003756 stirring Methods 0.000 claims description 28
- 239000000230 xanthan gum Substances 0.000 claims description 25
- 235000010493 xanthan gum Nutrition 0.000 claims description 25
- 229920001285 xanthan gum Polymers 0.000 claims description 25
- 229940082509 xanthan gum Drugs 0.000 claims description 25
- 239000004094 surface-active agent Substances 0.000 claims description 15
- 241000251468 Actinopterygii Species 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 12
- 241000949456 Zanthoxylum Species 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 229920000136 polysorbate Polymers 0.000 claims description 7
- 239000008601 oleoresin Substances 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000011835 investigation Methods 0.000 abstract description 9
- 239000000126 substance Substances 0.000 abstract description 7
- 238000001556 precipitation Methods 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 4
- 230000008859 change Effects 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 4
- 239000003814 drug Substances 0.000 abstract description 3
- 231100000344 non-irritating Toxicity 0.000 abstract description 2
- 239000003921 oil Substances 0.000 description 42
- 239000000243 solution Substances 0.000 description 39
- 239000012071 phase Substances 0.000 description 33
- 239000008346 aqueous phase Substances 0.000 description 15
- 230000000694 effects Effects 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 13
- 230000008719 thickening Effects 0.000 description 12
- 230000009286 beneficial effect Effects 0.000 description 9
- 239000007764 o/w emulsion Substances 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- 230000001133 acceleration Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000011347 resin Substances 0.000 description 6
- 229920005989 resin Polymers 0.000 description 6
- 230000007774 longterm Effects 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 4
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 239000000499 gel Substances 0.000 description 3
- SVTBMSDMJJWYQN-UHFFFAOYSA-N 2-methylpentane-2,4-diol Chemical compound CC(O)CC(C)(C)O SVTBMSDMJJWYQN-UHFFFAOYSA-N 0.000 description 2
- 102000012422 Collagen Type I Human genes 0.000 description 2
- 108010022452 Collagen Type I Proteins 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 239000004064 cosurfactant Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 230000007794 irritation Effects 0.000 description 2
- SZHOJFHSIKHZHA-UHFFFAOYSA-N tridecanoic acid Chemical compound CCCCCCCCCCCCC(O)=O SZHOJFHSIKHZHA-UHFFFAOYSA-N 0.000 description 2
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 235000008697 Cannabis sativa Nutrition 0.000 description 1
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 1
- 102000057297 Pepsin A Human genes 0.000 description 1
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- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000002921 anti-spasmodic effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000000949 anxiolytic effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
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- 239000001913 cellulose Substances 0.000 description 1
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- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000812 cholinergic antagonist Substances 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000010812 external standard method Methods 0.000 description 1
- HQVFCQRVQFYGRJ-UHFFFAOYSA-N formic acid;hydrate Chemical compound O.OC=O HQVFCQRVQFYGRJ-UHFFFAOYSA-N 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
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- 235000011852 gelatine desserts Nutrition 0.000 description 1
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229940051250 hexylene glycol Drugs 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000000338 in vitro Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- XUGNVMKQXJXZCD-UHFFFAOYSA-N isopropyl palmitate Chemical compound CCCCCCCCCCCCCCCC(=O)OC(C)C XUGNVMKQXJXZCD-UHFFFAOYSA-N 0.000 description 1
- 229940119170 jojoba wax Drugs 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 229910052760 oxygen Inorganic materials 0.000 description 1
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- 229940111202 pepsin Drugs 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
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- 238000000926 separation method Methods 0.000 description 1
- 208000017520 skin disease Diseases 0.000 description 1
- 239000000661 sodium alginate Substances 0.000 description 1
- 235000010413 sodium alginate Nutrition 0.000 description 1
- 229940005550 sodium alginate Drugs 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000013271 transdermal drug delivery Methods 0.000 description 1
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- A61K47/08—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing oxygen, e.g. ethers, acetals, ketones, quinones, aldehydes, peroxides
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Abstract
The invention provides cannabidiol emulsion and a preparation method thereof, belonging to the technical field of biological medicine. The cannabidiol emulsion comprises cannabidiol, an emulsifying agent, an oil phase, a marine collagen compound thickening agent and water. The cannabidiol emulsion has the advantages of no addition of alcohols, mild and non-irritating skin, good physical and chemical property stability, good content stability in stability investigation, no floating oil, no precipitation, no layering and no color change in stability investigation. The preparation method is simple and easy to operate, and is suitable for large-scale production.
Description
Technical Field
The invention belongs to the technical field of biological medicine, and in particular relates to cannabidiol emulsion and a preparation method thereof.
Background
Cannabidiol (CBD) is a non-psychoactive ingredient extracted from cannabis sativa leaves, is basically free from toxic and side effects, and has various pharmacological effects such as anti-inflammatory, antibacterial, antioxidant, antispasmodic and anxiolytic effects in vitro, and has attracted a great deal of attention in the field of medicine and pharmacology. Particularly, in recent years, the research shows that the CBD has good application prospect in the aspect of treating skin diseases and skin care. However, CBD is a fat-soluble compound, has problems of poor water solubility and transdermal absorbability, limited solubility in oils and fats, sensitivity to acids, alkalis and oxygen, poor thermal stability in solvents, low bioavailability and the like, and limits the application of CBD in various fields.
At present, in order to improve the solubility and transdermal absorption utilization rate of CBD, a main adopted method is to coat CBD by using gel or emulsion as a carrier, so that the CBD has the effects of slow release, permeation assistance, irritation reduction, stability improvement and the like. CBD gel is generally prepared by dissolving CBD in alcohol solution and then forming gel preparation with carbomer or hydroxy cellulose, and the transdermal drug delivery system can maintain blood concentration of CBD for a long time and controllably increase drug delivery, but alcohol has certain irritation to skin and is not suitable for long-term care and treatment of skin. The CBD emulsion is usually prepared by dissolving CBD in oil phase, mixing with surfactant (cosurfactant) and water at a certain ratio, and forming O/W emulsion under proper conditions to improve CBD dissolution and bioavailability. However, in the emulsion preparation disclosed in CN 110934757A, CN114306232A, CN114515250A, CN111135144A, CN 113730351a, etc., a lower alcohol (ethanol) or a polyhydric alcohol (propylene glycol, isopropanol, hexylene glycol, etc.) is mostly used as a cosurfactant, or heating is required in the emulsion preparation process, and a high-pressure homogenizer, an ultrasonic generator, a high-pressure micro-jet nano homogenizer, etc. special equipment is used, so that the emulsion containing cannabidiol can be obtained, but the operation is complex, the emulsion is not suitable for large-scale production, and the application limitation is very large.
Therefore, there is a need for cannabidiol emulsion that has good stability, is simple to operate, and does not contain alcohols.
Disclosure of Invention
Aiming at the problems that the addition of alcohol-containing substances in cannabidiol emulsion is complex in preparation method and unsuitable for large-scale production in the prior art, the invention provides cannabidiol emulsion containing marine collagen and a preparation method thereof. The marine collagen is collagen extracted from marine fish scales or fish skins, and is a waste material of marine fish byproducts and is developed and utilized in a high-value manner. The cannabidiol emulsion has the advantages of no addition of alcohols, mild and non-irritating skin, good physical and chemical property stability, good content stability in stability investigation, no floating oil, no precipitation, no layering and no color change in stability investigation. The preparation method is simple and easy to operate, and is suitable for large-scale production.
In order to solve the problems, the invention provides the following technical scheme.
In a first aspect, a cannabidiol emulsion is provided.
A cannabidiol emulsion comprising: cannabidiol, an emulsifying agent, an oil phase, a marine collagen compound thickening agent and water; the marine collagen compound thickener contains marine collagen and other thickeners.
In some embodiments, the cannabidiol emulsion comprises from 0.1wt% to 5.0wt% cannabidiol based on the total mass of the cannabidiol emulsion. In some embodiments, the cannabidiol emulsion comprises 0.1wt%, 0.5wt%, 1.0wt%, 1.5wt%, 2.0wt%, 2.5wt%, 3.0wt%, 3.5wt%, 4.0wt%, 4.5wt% or 5.0wt%, based on the total mass of the cannabidiol emulsion. In some embodiments, the cannabidiol emulsion comprises from 1.0wt% to 5.0wt% cannabidiol based on the total mass of the cannabidiol emulsion. In some embodiments, the cannabidiol emulsion comprises from 1.0wt% to 3.0wt% cannabidiol based on the total mass of the cannabidiol emulsion. In some embodiments, the cannabidiol emulsion comprises from 1.0wt% to 2.0wt% cannabidiol based on the total mass of the cannabidiol emulsion.
In some embodiments, the emulsifier is present in the cannabidiol emulsion in an amount of 0.1wt% to 10.0wt%, based on the total mass of the cannabidiol emulsion. In some embodiments, the amount of emulsifier in the cannabidiol emulsion is 1.0wt%, 2.0wt%, 3.0wt%, 4.0wt%, 5.0wt%, 6.0wt%, 7.0wt%, 8.0wt%, 9.0wt% or 10.0wt%, based on the total mass of the cannabidiol emulsion. In some embodiments, the emulsifier is present in the cannabidiol emulsion in an amount of 1.0wt% to 5.0wt%, based on the total mass of the cannabidiol emulsion. In some embodiments, the emulsifier is present in the cannabidiol emulsion in an amount of 1.0wt% to 4.0wt%, based on the total mass of the cannabidiol emulsion.
In some embodiments, the cannabidiol emulsion has an oil phase content of 1.0wt% to 40.0wt%, based on the total mass of the cannabidiol emulsion. In some embodiments, the oil phase is present in the cannabidiol emulsion in an amount of 1.0wt%, 5.0wt%, 10.0wt%, 15.0wt%, 20.0wt%, 25.0wt%, 30.0wt%, 35.0wt%, or 40.0wt% based on the total mass of the cannabidiol emulsion. In some embodiments, the cannabidiol emulsion has an oil phase content of 5.0wt% to 10.0wt%, based on the total mass of the cannabidiol emulsion.
In some embodiments, the total content of marine collagen built thickener in the cannabidiol emulsion is 0.1wt% to 10.0wt%, calculated on the total mass of the cannabidiol emulsion. In some embodiments, the total content of marine collagen built thickener in the cannabidiol emulsion is 0.5wt%, 1.0wt%, 2.0wt%, 3.0wt%, 4.0wt%, 5.0wt%, 6.0wt%, 7.0wt%, 8.0wt%, 9.0wt% or 10.0wt%, based on the total mass of the cannabidiol emulsion. In some embodiments, the total content of marine collagen built thickener in the cannabidiol emulsion is 0.5wt% to 5.0wt%, calculated on the total mass of the cannabidiol emulsion. In some embodiments, the total content of marine collagen built thickener in the cannabidiol emulsion is 0.5wt% to 2.0wt%, calculated on the total mass of the cannabidiol emulsion.
In some embodiments, the mass ratio of other thickening agents in the cannabidiol emulsion to the marine collagen is 1:1 to 5:1. in some embodiments, the mass ratio of other thickening agents to marine collagen in the cannabidiol emulsion is 1: 1. 2: 1. 3: 1. 4:1 or 5:1. in some embodiments, the mass ratio of other thickening agents in the cannabidiol emulsion to the marine collagen is 2:1 to 4:1.
in some embodiments, the cannabidiol emulsion has a water content of 35.0wt% to 98.7wt%, based on the total mass of the cannabidiol emulsion. In some embodiments, the cannabidiol emulsion has a water content of 35.0wt%, 40.0wt%, 45.0wt%, 50.0wt%, 55.0wt%, 60.0wt%, 65.0wt%, 70.0wt%, 75.0wt%, 80.0wt%, 85.0wt%, 90.0wt%, 95.0wt%, or 98.7wt%, based on the total mass of the cannabidiol emulsion.
In some embodiments, the total content of water and cannabidiol, emulsifier, oil phase, marine collagen built thickener in the cannabidiol emulsion is 100wt%.
In some embodiments, the oil phase comprises isopropyl myristate or zanthoxylum oleoresin.
In the cannabidiol emulsion provided by the invention, the cannabidiol emulsion does not contain alcohol substances.
In some embodiments, the additional thickener is xanthan gum.
In some embodiments, the marine collagen compound thickener is a mixture of xanthan gum and marine collagen.
In some embodiments, the marine collagen is collagen extracted from fish skin or scales of marine origin, having a purity of greater than or equal to 95%, and a molecular weight distribution of about 100KD to about 500KD, in some embodiments about 100KD to about 300KD, or about 150KD to about 250KD.
In some embodiments, the emulsifier has an HLB value of from 12 to 14.
In some embodiments, the emulsifier is a tween-based surfactant and span-based surfactant.
In some embodiments, the emulsifying agent is tween 80 and span 80.
In some embodiments, the mass ratio of tween-based surfactant to span-based surfactant is 2:1 to 10:1. in some embodiments, the mass ratio of tween-based surfactant to span-based surfactant is 2: 1. 3: 1. 4:1. 5:1. 6: 1. 7:1. 8: 1. 9:1 or 10:1. in some embodiments, the mass ratio of tween-based surfactant to span-based surfactant is from 2.6:1 to 9.7:1.
In some embodiments, a cannabidiol emulsion comprising: cannabidiol, an emulsifier, an oil phase, marine collagen, xanthan gum and water; the oil phase comprises isopropyl myristate or zanthoxylum oleoresin; the emulsifying agent is Tween 80 and span 80.
In some embodiments, a cannabidiol emulsion comprising: cannabidiol, an emulsifier, an oil phase, marine collagen, xanthan gum and water; calculated by the total mass of the cannabidiol emulsion, the content of cannabidiol in the cannabidiol emulsion is 0.1-5.0 wt%, the content of emulsifying agent in the cannabidiol emulsion is 0.1-10.0 wt%, the content of oil phase in the cannabidiol emulsion is 1.0-40.0 wt%, the total content of marine collagen and xanthan gum in the cannabidiol emulsion is 0.1-10.0 wt%, and the mass ratio of xanthan gum to marine collagen in the cannabidiol emulsion is 1:1 to 5:1, the total content of water, cannabidiol, an emulsifier, an oil phase, marine collagen and xanthan gum in the cannabidiol emulsion is 100wt%; the oil phase comprises isopropyl myristate or zanthoxylum oleoresin; the emulsifying agent is tween 80 and span 80; the mass ratio of the tween 80 to the span 80 is 2:1-10:1.
In some embodiments, a cannabidiol emulsion comprising: cannabidiol, an emulsifier, an oil phase, marine collagen, xanthan gum and water; calculated by the total mass of the cannabidiol emulsion, the content of cannabidiol in the cannabidiol emulsion is 1.0-2.0 wt%, the content of emulsifying agent in the cannabidiol emulsion is 1.0-4.0 wt%, the content of oil phase in the cannabidiol emulsion is 5.0-10.0 wt%, the total content of marine collagen and xanthan gum in the cannabidiol emulsion is 0.5-2.0 wt%, and the mass ratio of xanthan gum to marine collagen in the cannabidiol emulsion is 2:1 to 4:1, the total content of water, cannabidiol, an emulsifier, an oil phase, marine collagen and xanthan gum in the cannabidiol emulsion is 100wt%; the oil phase comprises isopropyl myristate or zanthoxylum oleoresin; the emulsifying agent is tween 80 and span 80; the mass ratio of the tween 80 to the span 80 is 2.6:1-9.7:1.
In a second aspect, there is provided a process for preparing the cannabidiol emulsion of the first aspect.
A method of preparing the cannabidiol emulsion of the first aspect, comprising the steps of:
(1) Dissolving cannabidiol in an oil phase to obtain a mixed solution 1;
(2) Mixing an emulsifier, a marine collagen compound thickener and water to obtain a mixed solution 2;
(3) Mixing the mixed solution 1 and the mixed solution 2, and stirring to obtain the cannabidiol emulsion.
In some embodiments, a method of preparing the cannabidiol emulsion of the first aspect comprises the steps of:
(1) Dissolving cannabidiol in an oil phase to obtain a mixed solution 1;
(2) Mixing an emulsifier, marine collagen and xanthan gum with water to obtain a mixed solution 2;
(3) Mixing the mixed solution 1 and the mixed solution 2, and stirring to obtain the cannabidiol emulsion.
In some embodiments, the stirring in step (3) is performed at a speed of 200rpm to 5000rpm for a period of 20min to 60min.
Advantageous effects
The embodiment provided by the invention has at least one of the following beneficial effects:
(1) According to the preparation method of the cannabidiol emulsion, alcohol substances are not needed, and marine collagen and xanthan gum are compounded to serve as a thickening agent, so that the effect of stabilizing the emulsion is achieved, and the cannabidiol emulsion is mild and does not irritate skin.
(2) The cannabidiol emulsion containing marine collagen prepared by the technical scheme of the invention has the advantages that the cannabidiol emulsion containing marine collagen is placed for 6 months under acceleration conditions (40+/-2 ℃ and 75%RH+/-5%) or is placed for 12 months under long-term conditions (25+/-2 ℃ and 60%RH+/-10%), and has no floating oil, no layering, no precipitation and no color change, and the stability is good.
(3) Compared with other types of thickeners and compared with single xanthan gum or marine collagen serving as a thickening component, the thickening component compounded by the xanthan gum and the marine collagen is more beneficial to avoiding the phenomena of oil slick, layering, precipitation and discoloration after the obtained cannabidiol emulsion is placed for 6 months or for 12 months under the acceleration condition (40 ℃ +/-2 ℃ and 75%RH+/-5%) or the long-term condition (25 ℃ +/-2 ℃ and 60%RH+/-10%), is more beneficial to avoiding the degradation of cannabidiol, and has unexpected technical effects.
(4) Compared with single xanthan gum or marine collagen serving as a thickening component, when the thickening component compounded by the xanthan gum and the marine collagen is adopted, the xanthan gum and the marine collagen have a synergistic effect, so that the physicochemical stability and the content stability of the obtained cannabidiol emulsion are greatly improved, and unexpected technical effects are achieved.
(5) Compared with other types of emulsifying agents and compared with the use of tween 80 or span 80 as the emulsifying agent alone, the compound emulsifying agent of tween 80 and span 80 is used as the emulsifying agent, the obtained cannabidiol emulsion is more beneficial to avoiding the phenomena of oil sliming, layering and precipitation after being placed for 6 months or for 12 months under the acceleration condition (40 ℃ +/-2 ℃ and 75%RH+/-5%) and the long-term condition (25 ℃ +/-2 ℃ and 60%RH+/-10%), and is more beneficial to avoiding the degradation of cannabidiol, and has unexpected technical effects.
(6) Compared with the method which adopts tween 80 or span 80 as an emulsifier and adopts a compound emulsifier of tween 80 and span 80 as an emulsifier, the tween 80 and span 80 have synergistic effect, so that the physicochemical stability and content stability of the obtained cannabidiol emulsion are greatly improved, and unexpected technical effects are achieved.
(7) Compared with other oil phases, the isopropyl myristate or the zanthoxylum oil resin is adopted as the oil phase, which is more favorable for the physical and chemical stability and content stability of the obtained cannabidiol emulsion, and has unexpected technical effects.
(8) The marine collagen with molecular weight distribution of 100 KD-500 KD is adopted, so that the stability of the obtained cannabidiol emulsion is improved, and the phenomenon of floating oil, layering and precipitation is avoided after the obtained cannabidiol emulsion is placed for 6 months under an acceleration condition (40 ℃ +/-2 ℃ and 75%RH+/-5%) or for 12 months under a long-term condition (25 ℃ +/-2 ℃ and 60%RH+/-10%).
Definition of terms
In the context of the present invention, all numbers disclosed herein are approximations, whether or not the word "about" or "about" is used. Based on the numbers disclosed, there is a possibility that the values of each number may differ by less than + -10% or a reasonable difference as recognized by those skilled in the art, such as + -1%, + -2%, + -3%, + -4%, or + -5%.
The term "marine collagen" is collagen extracted from marine source fish skin or collagen extracted from marine fish scales.
The terms "above," "below," "within," and the like are to be construed as including the present number, e.g., two or more means ≡two.
The term "and/or" is understood to mean any one of the selectable items or a combination of any two or more of the selectable items.
The term "wt%" means mass percent.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
Detailed Description
In order to better understand the technical solution of the present invention, some non-limiting examples are further disclosed below to further describe the present invention in detail.
The reagents used in the present invention are all commercially available or can be prepared by the methods described herein.
The marine collagen adopted in the following examples 1 to 3 and comparative examples 1 to 20 is collagen extracted from marine fish skin or fish scale, the purity is not less than 95%, and the molecular weight distribution is 100 KD-500 KD.
Marine collagen is commercially available or obtainable by the following preparation method: extracting fish scales or fish skins of marine fishes by using an acetic acid aqueous solution as an extracting agent by adopting a homogenizing technology, adding pepsin under a low-temperature condition (for example, 4 ℃), stirring for enzymolysis, purifying by a membrane separation technology, and freeze-drying to obtain type I collagen (namely marine collagen), wherein the three-helix structure of the type I collagen is complete, the purity is more than or equal to 95%, and the molecular weight distribution is 100 KD-300 KD or 100 KD-500 KD.
Example 1: preparation of cannabidiol emulsion containing marine collagen
(1) Dissolving cannabidiol in isopropyl myristate, wherein the cannabidiol accounts for 1.0wt% of the total weight of the cannabidiol emulsion, and the isopropyl myristate accounts for 5.0wt% of the total weight of the cannabidiol emulsion, so as to obtain an isopropyl myristate solution of the cannabidiol;
(2) Adding a compound emulsifier consisting of tween 80 and span 80 into water, wherein the mass ratio of the tween 80 to the span 80 is 2.6:1, the HLB value of the compound emulsifier is 12, the compound emulsifier accounts for 2.0wt% of the total weight of the cannabidiol emulsion, after being uniformly stirred, the compound thickener of marine collagen accounting for 1.0wt% of the total weight of the cannabidiol emulsion is added, wherein the compound thickener of marine collagen comprises the following components in percentage by mass: 1 and marine collagen (150 KD), and continuously stirring until the materials are uniformly mixed to obtain an aqueous phase solution;
(3) Slowly adding isopropyl myristate solution of cannabidiol into the aqueous phase solution at 500rpm, and stirring thoroughly for 30min to obtain white cannabidiol emulsion (oil-in-water emulsion).
Example 2: preparation of cannabidiol emulsion containing marine collagen
(1) Dissolving cannabidiol in isopropyl myristate, wherein the cannabidiol accounts for 2.0wt% of the total weight of the cannabidiol emulsion, and the isopropyl myristate accounts for 10.0wt% of the total weight of the cannabidiol emulsion, so as to obtain an isopropyl myristate solution of the cannabidiol;
(2) Adding a compound emulsifier consisting of tween 80 and span 80 into water, wherein the mass ratio of the tween 80 to the span 80 is 9.7:1, the HLB value of the compound emulsifier is 14, the compound emulsifier accounts for 4.0wt% of the total weight of the cannabidiol emulsion, after being uniformly stirred, the compound thickener of marine collagen accounting for 2.0wt% of the total weight of the cannabidiol emulsion is added, wherein the compound thickener of marine collagen comprises the following components in percentage by mass: 1 and marine collagen (250 KD), and continuously stirring until the materials are uniformly mixed to obtain an aqueous phase solution;
(3) Slowly adding isopropyl myristate solution of cannabidiol into the aqueous phase solution, stirring at 800rpm for 40min to obtain white cannabidiol emulsion (oil-in-water emulsion).
Example 3: preparation of cannabidiol emulsion containing marine collagen
(1) Dissolving cannabidiol in a zanthoxylum oil resin, wherein the cannabidiol accounts for 1.0 weight percent of the total weight of the cannabidiol emulsion, and the zanthoxylum oil resin accounts for 10.0 weight percent of the total weight of the cannabidiol emulsion, so as to obtain a cannabidiol zanthoxylum oil resin solution;
(2) Adding a compound emulsifier consisting of tween 80 and span 80 into water, wherein the mass ratio of the tween 80 to the span 80 is 2.6:1, the HLB value of the compound emulsifier is 12, the compound emulsifier accounts for 1.0 weight percent of the total weight of the cannabidiol emulsion, after being uniformly stirred, the compound thickener of marine collagen accounting for 0.5 weight percent of the total weight of the cannabidiol emulsion is added, wherein the compound thickener of marine collagen comprises the following components in percentage by mass: 1 and marine collagen, and continuously stirring until the materials are uniformly mixed to obtain an aqueous phase solution;
(3) Slowly adding the cannabidiol oil resin solution into the aqueous phase solution, stirring at 1000rpm for 30min to obtain white cannabidiol emulsion (oil-in-water emulsion).
Comparative example 1: preparation of cannabidiol emulsion
(1) Dissolving cannabidiol in isopropyl myristate, wherein the cannabidiol accounts for 1.0wt% of the total weight of the cannabidiol emulsion, and the isopropyl myristate accounts for 5.0wt% of the total weight of the cannabidiol emulsion, so as to obtain an isopropyl myristate solution of the cannabidiol;
(2) Adding a compound emulsifier consisting of tween 80 and span 80 into water, wherein the mass ratio of the tween 80 to the span 80 is 2.6:1, adding sodium alginate accounting for 2.0 weight percent of the total weight of the cannabidiol emulsion after uniformly stirring, and continuously stirring until uniformly mixing to obtain a water phase solution, wherein the HLB value of the compound emulsifier is 12, and the compound emulsifier accounts for 1.0 weight percent of the total weight of the cannabidiol emulsion;
(3) Slowly adding isopropyl myristate solution of cannabidiol into the aqueous phase solution at 500rpm, and stirring thoroughly for 30min to obtain white cannabidiol emulsion (oil-in-water emulsion).
Comparative example 2: preparation of cannabidiol emulsion
(1) Dissolving cannabidiol in isopropyl myristate, wherein the cannabidiol accounts for 1.0wt% of the total weight of the cannabidiol emulsion, and the isopropyl myristate accounts for 5.0wt% of the total weight of the cannabidiol emulsion, so as to obtain an isopropyl myristate solution of the cannabidiol;
(2) Adding a compound emulsifier consisting of tween 80 and span 80 into water, wherein the mass ratio of the tween 80 to the span 80 is 9.7:1, the HLB value of the compound emulsifier is 14, the compound emulsifier accounts for 2.0 weight percent of the total weight of the cannabidiol emulsion, after being uniformly stirred, gelatin accounting for 2.0 weight percent of the total weight of the cannabidiol emulsion is added, and the mixture is continuously stirred until the mixture is uniformly mixed, so as to obtain aqueous phase solution;
(3) Slowly adding isopropyl myristate solution of cannabidiol into the aqueous phase solution at 500rpm, and stirring thoroughly for 30min to obtain white cannabidiol emulsion (oil-in-water emulsion).
Comparative example 3: preparation of cannabidiol emulsion
(1) Dissolving cannabidiol in isopropyl myristate, wherein the cannabidiol accounts for 1.0wt% of the total weight of the cannabidiol emulsion, and the isopropyl myristate accounts for 5.0wt% of the total weight of the cannabidiol emulsion, so as to obtain an isopropyl myristate solution of the cannabidiol;
(2) Adding an emulsifier PEG40 hydrogenated castor oil into water, wherein the HLB value of the emulsifier is 14, the emulsifier accounts for 2.0wt% of the total weight of the cannabidiol emulsion, uniformly stirring, adding xanthan gum accounting for 2.0wt% of the total weight of the cannabidiol emulsion, and continuously stirring until uniformly mixing to obtain a water phase solution;
(3) Slowly adding isopropyl myristate solution of cannabidiol into the aqueous phase solution at 500rpm, and stirring thoroughly for 30min to obtain white cannabidiol emulsion (oil-in-water emulsion).
Comparative examples 4 to 11: investigation of thickening Components
(1) Dissolving cannabidiol in isopropyl myristate, wherein the cannabidiol accounts for 1.0wt% of the total weight of the cannabidiol emulsion, and the isopropyl myristate accounts for 5.0wt% of the total weight of the cannabidiol emulsion, so as to obtain an isopropyl myristate solution of the cannabidiol;
(2) Adding a compound emulsifier consisting of tween 80 and span 80 into water, wherein the mass ratio of the tween 80 to the span 80 is 2.6:1, adding a thickening component (thickener or compound thickener) accounting for 1.0 weight percent of the total weight of the cannabidiol emulsion after uniformly stirring, wherein the thickening component is shown in table 1, and continuously stirring until the mixture is uniformly mixed to obtain an aqueous phase solution;
(3) Slowly adding isopropyl myristate solution of cannabidiol into the aqueous phase solution at 500rpm, and stirring thoroughly for 30min to obtain white cannabidiol emulsion (oil-in-water emulsion).
Table 1: investigation of thickening Components
Comparative examples 12 to 16: examination of the emulsifiers
(1) Dissolving cannabidiol in isopropyl myristate, wherein the cannabidiol accounts for 1.0wt% of the total weight of the cannabidiol emulsion, and the isopropyl myristate accounts for 5.0wt% of the total weight of the cannabidiol emulsion, so as to obtain an isopropyl myristate solution of the cannabidiol;
(2) Adding the emulsifying agent shown in table 2 into water, wherein the emulsifying agent accounts for 2.0wt% of the total weight of the cannabidiol emulsion, uniformly stirring, and then adding the marine collagen compound thickening agent accounting for 1.0wt% of the total weight of the cannabidiol emulsion, wherein the marine collagen compound thickening agent comprises the following components in percentage by mass: 1 and marine collagen, and continuously stirring until the materials are uniformly mixed to obtain an aqueous phase solution;
(3) Slowly adding isopropyl myristate solution of cannabidiol into the aqueous phase solution at 500rpm, and stirring thoroughly for 30min to obtain white cannabidiol emulsion (oil-in-water emulsion).
Table 2: examination of the emulsifiers
Comparative examples 20 to 22: investigation of the oil phase
(1) Dissolving cannabidiol in an oil phase shown in table 3, wherein the cannabidiol accounts for 1.0wt% of the total weight of the cannabidiol emulsion, and the isopropyl myristate accounts for 5.0wt% of the total weight of the cannabidiol emulsion, so as to obtain an oil phase solution of the cannabidiol;
(2) Adding a compound emulsifier consisting of tween 80 and span 80 into water, wherein the mass ratio of the tween 80 to the span 80 is 2.6:1, the HLB value of the compound emulsifier is 12, the compound emulsifier accounts for 2.0wt% of the total weight of the cannabidiol emulsion, after being uniformly stirred, the compound thickener of marine collagen accounting for 1.0wt% of the total weight of the cannabidiol emulsion is added, wherein the compound thickener of marine collagen comprises the following components in percentage by mass: 1 and marine collagen, and continuously stirring until the materials are uniformly mixed to obtain an aqueous phase solution;
(3) Slowly adding cannabidiol oil phase solution into water phase solution, stirring at 500rpm for 30min to obtain white cannabidiol emulsion (oil-in-water emulsion).
Table 3: investigation of the oil phase
| Examples | Oil phase |
| Comparative example 19 | Isopropyl palmitate |
| Comparative example 20 | Tridecanoic acid triglyceride |
| Comparative example 21 | White oil |
| Comparative example 22 | Jojoba oil |
Example 4: stability investigation
1. The detection indexes are as follows: and (3) measuring the layering phenomenon and the CBD content of cannabidiol.
2. Experimental conditions: samples obtained in examples 1 to 3, comparative examples 1 to 7, and comparative examples 10 to 20 were placed under acceleration conditions (40 ℃.+ -. 2 ℃ C., 75% RH.+ -. 5%) for 6 months, respectively. The appearance of the samples and the cannabidiol content were examined at 0 days and 6 months, respectively. The results are shown in Table 4.
(1) Layering phenomenon: the centrifuge centrifuged the sample at 3000rpm for 15 minutes and observed for delamination.
(2) Cannabidiol content determination (high performance liquid chromatography): accurately preparing 0.15mg/mL cannabidiol methanol solution, and detecting by an external standard method. Chromatographic column: agilent TC-C18 column (250 mm. Times.4.6 mm,5 um); mobile phase: 0.1% formic acid water (a): gradient elution is carried out by 0.1 percent of acetonitrile (B) formate; the detection wavelength is 220nm, and the column temperature is 30 ℃; the flow rate is 1.2mL/min; the sample injection amount was 10. Mu.L.
Table 4: cannabidiol emulsion stability
Conclusion: from the results in Table 4, it can be seen that:
(1) Compared with other types of thickeners and compared with single xanthan gum or marine collagen serving as a thickening component, the thickening component compounded by the xanthan gum and the marine collagen is more beneficial to avoiding layering and color change phenomena after the obtained cannabidiol emulsion is placed for 6 months under an acceleration condition (40 ℃ +/-2 ℃ and 75%RH+/-5%), is more beneficial to avoiding degradation of cannabidiol, and has unexpected technical effects.
(2) Compared with single xanthan gum or marine collagen serving as a thickening component, when the thickening component compounded by the xanthan gum and the marine collagen is adopted, the xanthan gum and the marine collagen have a synergistic effect, so that the physicochemical stability and the content stability of the obtained cannabidiol emulsion are greatly improved, and unexpected technical effects are achieved.
(3) Compared with other types of emulsifying agents and compared with the method which singly uses tween 80 or span 80 as the emulsifying agent, the method which uses the compound emulsifying agent of tween 80 and span 80 as the emulsifying agent is more beneficial to avoiding oil slick and layering phenomena after the obtained cannabidiol emulsion is placed for 6 months under the acceleration condition (40 ℃ +/-2 ℃ and 75%RH+/-5%), is more beneficial to avoiding the degradation of cannabidiol, and has unexpected technical effects.
(4) Compared with the method which adopts tween 80 or span 80 as an emulsifier and adopts a compound emulsifier of tween 80 and span 80 as an emulsifier, the tween 80 and span 80 have synergistic effect, so that the physicochemical stability and content stability of the obtained cannabidiol emulsion are greatly improved, and unexpected technical effects are achieved.
(5) Compared with other oil phases, the isopropyl myristate or the zanthoxylum oil resin is adopted as the oil phase, which is more favorable for the physical and chemical stability and content stability of the obtained cannabidiol emulsion, and has unexpected technical effects.
While the methods of this invention have been described in terms of preferred embodiments, it will be apparent to those of skill in the art that variations and combinations of the methods and applications described herein can be made and applied within the spirit and scope of the invention. Those skilled in the art can, with the benefit of this disclosure, suitably modify the process parameters to achieve this. It is expressly noted that all such similar substitutions and modifications will be apparent to those skilled in the art, and are deemed to be included within the present invention.
Claims (12)
1. A cannabidiol emulsion comprising: cannabidiol, an emulsifying agent, an oil phase, a marine collagen compound thickening agent and water; the marine collagen compound thickener contains marine collagen and other thickeners; the emulsifier is a Tween surfactant and a span surfactant; the oil phase comprises isopropyl myristate or zanthoxylum oleoresin; calculated by the total mass of the cannabidiol emulsion, the cannabidiol content in the cannabidiol emulsion is 0.1-2.0 wt%, the emulsifier content in the cannabidiol emulsion is 1.0-1.0 wt.0 wt%, the oil phase content in the cannabidiol emulsion is 5.0-10.0 wt%, and the total content of the marine collagen compound thickener in the cannabidiol emulsion is 0.5-10.0 wt%; the mass ratio of other thickening agents in the cannabidiol emulsion to the marine collagen is 1: 1-5: 1, a step of; the other thickening agent is xanthan gum; the marine collagen is collagen extracted from marine fish skin or fish scales, and the molecular weight of the marine collagen is distributed in a range of 100 KD-500 KD; the emulsifying agent is tween 80 and span 80; the mass ratio of the Tween surfactant to the span surfactant is 2:1-10:1.
2. the cannabidiol emulsion of claim 1, wherein the cannabidiol emulsion comprises 1.0-wt-4.0 wt% of an emulsifier based on the total mass of the cannabidiol emulsion.
3. The cannabidiol emulsion of claim 1, wherein the total content of marine collagen built thickener in the cannabidiol emulsion is 0.5wt% to 5.0wt%, calculated as the total mass of the cannabidiol emulsion.
4. The cannabidiol emulsion of claim 1, wherein the total content of marine collagen built thickener in the cannabidiol emulsion is 0.5wt% to 2.0wt%, calculated as the total mass of the cannabidiol emulsion.
5. The cannabidiol emulsion of claim 1, wherein the mass ratio of other thickeners in the cannabidiol emulsion to the marine collagen is 2: 1-4: 1.
6. the cannabidiol emulsion of any one of claims 1-4, having a water content of 35.0wt% to 98.7wt%, based on the total mass of the cannabidiol emulsion.
7. The cannabidiol emulsion of any one of claims 1-4, wherein the total content of water and cannabidiol, emulsifier, oil phase, marine collagen compound thickener in the cannabidiol emulsion is 100wt%.
8. The cannabidiol emulsion of any one of claims 1-4, wherein the purity of the marine collagen is greater than or equal to 95%.
9. The cannabidiol emulsion of any one of claims 1-4, which is free of alcohols.
10. The cannabidiol emulsion of any one of claims 1-4, wherein the mass ratio of tween surfactant to span surfactant is 2.6:1-9.7:1.
11. A process for preparing the cannabidiol emulsion of any one of claims 1-10, comprising the steps of:
(1) Dissolving cannabidiol in an oil phase to obtain a mixed solution 1;
(2) Mixing an emulsifier, a marine collagen compound thickener and water to obtain a mixed solution 2;
(3) Mixing the mixed solution 1 and the mixed solution 2, and stirring to obtain the cannabidiol emulsion.
12. The method according to claim 11, wherein the stirring speed in the step (3) is 200 rpm-5000 rpm, and the stirring time is 20min-60min.
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