CN115531240A - Cannabidiol emulsion and preparation method thereof - Google Patents
Cannabidiol emulsion and preparation method thereof Download PDFInfo
- Publication number
- CN115531240A CN115531240A CN202211144804.XA CN202211144804A CN115531240A CN 115531240 A CN115531240 A CN 115531240A CN 202211144804 A CN202211144804 A CN 202211144804A CN 115531240 A CN115531240 A CN 115531240A
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- CN
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- Prior art keywords
- cannabidiol
- emulsion
- emulsifier
- marine collagen
- water
- Prior art date
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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 246
- 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 246
- 229950011318 cannabidiol Drugs 0.000 title claims abstract description 246
- 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 246
- 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 246
- 239000000839 emulsion Substances 0.000 title claims abstract description 176
- 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 73
- 108010035532 Collagen Proteins 0.000 claims abstract description 73
- 229920001436 collagen Polymers 0.000 claims abstract description 73
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 70
- 150000001875 compounds Chemical class 0.000 claims abstract description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000002562 thickening agent Substances 0.000 claims abstract description 38
- 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
- 241000251468 Actinopterygii Species 0.000 claims description 14
- 239000004094 surface-active agent Substances 0.000 claims description 13
- 239000011259 mixed solution Substances 0.000 claims description 12
- 241000949456 Zanthoxylum Species 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 229920000136 polysorbate Polymers 0.000 claims description 6
- 150000001298 alcohols Chemical class 0.000 claims description 4
- 238000009826 distribution Methods 0.000 claims description 4
- 239000008601 oleoresin Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 8
- 238000011835 investigation Methods 0.000 abstract description 8
- 238000001556 precipitation Methods 0.000 abstract description 6
- 238000002845 discoloration Methods 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 4
- 229940079593 drug Drugs 0.000 abstract description 2
- 239000003814 drug Substances 0.000 abstract description 2
- 231100000344 non-irritating Toxicity 0.000 abstract description 2
- 239000003921 oil Substances 0.000 description 43
- 239000012071 phase Substances 0.000 description 40
- 239000000243 solution Substances 0.000 description 40
- 230000000694 effects Effects 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 13
- 230000008719 thickening Effects 0.000 description 12
- 239000000203 mixture Substances 0.000 description 9
- 239000008346 aqueous phase Substances 0.000 description 8
- 230000002349 favourable effect Effects 0.000 description 8
- 239000007764 o/w emulsion Substances 0.000 description 7
- 239000011347 resin Substances 0.000 description 7
- 229920005989 resin Polymers 0.000 description 7
- 230000007774 longterm Effects 0.000 description 5
- 230000001133 acceleration Effects 0.000 description 4
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- 230000002195 synergetic effect Effects 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-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
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000032798 delamination Effects 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
- 238000004090 dissolution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007794 irritation Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000047 product Substances 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
- 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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- XBJFCYDKBDVADW-UHFFFAOYSA-N acetonitrile;formic acid Chemical compound CC#N.OC=O XBJFCYDKBDVADW-UHFFFAOYSA-N 0.000 description 1
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- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 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
- 239000002249 anxiolytic agent Substances 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
- 210000004369 blood Anatomy 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
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- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000812 cholinergic antagonist Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000011161 development 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
- 235000019322 gelatine Nutrition 0.000 description 1
- 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
- 239000004519 grease Substances 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
- 238000000265 homogenisation 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
- 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
- 240000004308 marijuana Species 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 229940111202 pepsin Drugs 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
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- 238000011160 research Methods 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
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000037317 transdermal delivery Effects 0.000 description 1
- LADGBHLMCUINGV-UHFFFAOYSA-N tricaprin Chemical compound CCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCC)COC(=O)CCCCCCCCC LADGBHLMCUINGV-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
The invention provides a cannabidiol emulsion and a preparation method thereof, belonging to the technical field of skin care products and biological medicines. The cannabidiol emulsion comprises cannabidiol, an emulsifier, an oil phase, a marine collagen compound thickener and water. The cannabidiol emulsion is free of alcohol substances, mild and non-irritating to skin, good in physical and chemical property stability, good in content stability in stability investigation, and free of floating oil, precipitation, layering and discoloration 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 skin care products and biological medicines, and particularly relates to cannabidiol emulsion and a preparation method thereof.
Technical Field
Cannabidiol (CBD) is a non-psychoactive ingredient extracted from cannabis leaves, has substantially no toxic or side effects, has various pharmacological effects such as in vitro anti-inflammatory, antibacterial, antioxidant, antispasmodic, anxiolytic, etc., and has attracted wide attention in the pharmaceutical and cosmetic fields. Especially, recent researches show that CBD has good application prospects in the aspects of treating skin diseases and caring skin. However, CBD is a fat-soluble compound, has the problems of poor water solubility and transdermal absorbability, limited solubility in grease, sensitivity to acid, alkali and oxygen, poor thermal stability in a solvent, 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, gel or emulsion is mainly used as a carrier to coat CBD, so that the CBD has the effects of slow release, penetration 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, etc., the gel transdermal delivery system can keep blood concentration of CBD for a long time and controllably increase drug delivery, but alcohol substances have certain irritation to skin and are not suitable for long-term care and treatment of skin. CBD emulsion is usually prepared by dissolving CBD in oil phase, mixing with surfactant (cosurfactant) and water at a certain ratio after complete dissolution, and forming O/W type emulsion under proper conditions to improve CBD dissolution and bioavailability. However, in the emulsion preparation disclosed in patents CN 110934757A, CN114306232A, CN114515250A, CN111135144A, CN 113730351A, etc., mostly lower alcohols (ethanol) or polyols (propylene glycol, isopropanol, hexylene glycol, etc.) are used as cosurfactants, or heating is needed in the emulsion preparation process, and special equipment such as a high-pressure homogenizer, an ultrasonic generator, a high-pressure micro-jet nano homogenizer, etc. is used, although the emulsion containing cannabidiol can be obtained, the operation is complex, and the emulsion is not suitable for large-scale production, and alcohols are not suitable for addition of skin care products, so that the emulsion has great application limitation.
Therefore, there is a need for cannabidiol emulsions that are stable, easy to handle, and free of alcohol.
Disclosure of Invention
The invention provides a cannabidiol emulsion containing marine collagen and a preparation method thereof, aiming at the problems that in the prior art, cannabidiol emulsion containing alcohol substances is added, the preparation method is complex, and large-scale production is not suitable. The marine collagen is extracted from marine fish scales or fish skins, and is a high-value development and utilization method for changing waste into valuable of marine fish byproducts. The cannabidiol emulsion is free of alcohol substances, mild and non-irritating to skin, good in physical and chemical property stability, good in content stability in stability investigation, and free of floating oil, precipitation, layering and discoloration in stability investigation. The preparation method is simple and easy to operate, and is suitable for large-scale production.
In order to solve the above problems, the present invention provides the following technical solutions.
In a first aspect, a cannabidiol emulsion is provided.
A cannabidiol emulsion, comprising: cannabidiol, an emulsifier, an oil phase, a marine collagen compound thickener and water; the marine collagen compound thickener contains marine collagen and other thickeners.
In some embodiments, the cannabidiol is present in the cannabidiol emulsion in an amount of 0.1wt% to 5.0wt% based on the total mass of the cannabidiol emulsion. In some embodiments, the cannabidiol is present in the cannabidiol emulsion in an amount of 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 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 cannabidiol is present in the cannabidiol emulsion in an amount of 1.0wt% to 3.0wt% based on the total mass of the cannabidiol emulsion. In some embodiments, the cannabidiol is present in the cannabidiol emulsion in an amount of 1.0wt% to 2.0wt% based on the total mass of the cannabidiol emulsion.
In some embodiments, the emulsifier is present in the cannabidiol emulsion in an amount of 0.1wt% to 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%, 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 comprises an oil phase in an amount of 1.0wt% to 40.0wt%, based on the total weight of the cannabidiol emulsion. In some embodiments, the cannabidiol emulsion comprises an oil phase 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 weight of the cannabidiol emulsion.
In some embodiments, the total content of marine collagen complex thickener in the cannabidiol emulsion is 0.1wt% to 10.0wt% based on the total mass of the cannabidiol emulsion. In some embodiments, the total content of marine collagen complex 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 complex thickener in the cannabidiol emulsion is 0.5wt% to 5.0wt% based on the total mass of the cannabidiol emulsion. In some embodiments, the total content of marine collagen complex thickener in the cannabidiol emulsion is 0.5wt% to 2.0wt% based on the total mass of the cannabidiol emulsion.
In some embodiments, the mass ratio of the other thickeners in the cannabidiol emulsion to the marine collagen is 1:1 to 5:1. in some embodiments, the mass ratio of the other thickeners 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 the other thickeners to the marine collagen in the cannabidiol emulsion is 2:1 to 4:1.
in some embodiments, the water content of the cannabidiol emulsion is 35.0wt% to 98.7wt% based on the total mass of the cannabidiol emulsion. In some embodiments, the amount of water in the cannabidiol emulsion is 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 cannabidiol emulsion has a total content of water, cannabidiol, emulsifier, oil phase, marine collagen built thickener of 100wt%.
In some embodiments, the oil phase comprises isopropyl myristate or zanthoxylum oleoresin.
In the cannabidiol emulsion provided by the invention, the cannabidiol emulsion is free of alcohols.
In some embodiments, the other thickener is xanthan gum.
In some embodiments, the marine collagen complex thickener is a mixture of xanthan gum and marine collagen.
In some embodiments, the marine collagen is collagen extracted from fish skin or fish scales of marine origin, has a purity of 95% or more, and has 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 12 to 14.
In some embodiments, the emulsifier is a tween surfactant and a span surfactant.
In some embodiments, the emulsifier is tween 80 and span 80.
In some embodiments, the weight ratio of tween surfactant to span surfactant is 2:1 to 10:1. in some embodiments, the weight ratio of tween surfactant to span 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 weight ratio of tween surfactant to span surfactant is 2.6.
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 oil resin; the emulsifier 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 0.1wt% -5.0wt%, the content of emulsifier in the cannabidiol emulsion is 0.1wt% -10.0wt%, the content of oil phase in the cannabidiol emulsion is 1.0wt% -40.0 wt%, the total content of marine collagen and xanthan gum in the cannabidiol emulsion is 0.1wt% -10.0wt%, 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 oil resin; the emulsifier is tween 80 and span 80; the mass ratio of the Tween 80 to the span 80 is (2).
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 1.0wt% -2.0wt%, the content of emulsifier in the cannabidiol emulsion is 1.0wt% -4.0wt%, the content of oil phase in the cannabidiol emulsion is 5.0wt% -10.0wt%, the total content of marine collagen and xanthan gum in the cannabidiol emulsion is 0.5wt% -2.0wt%, 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 oil resin; the emulsifier is Tween 80 and span 80; the mass ratio of the Tween 80 to the span 80 is 2.6.
In a second aspect, there is provided a method of making the cannabidiol emulsion of the first aspect.
A method of preparing a cannabidiol emulsion of the first aspect, comprising the steps of:
(1) Dissolving cannabidiol in the 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) And mixing the mixed solution 1 and the mixed solution 2, and stirring to obtain the cannabidiol emulsion.
In some embodiments, a method of making the cannabidiol emulsion of the first aspect, comprising the steps of:
(1) Dissolving cannabidiol in the oil phase to obtain a mixed solution 1;
(2) Mixing emulsifier, marine collagen and xanthan gum with water to obtain a mixed solution 2;
(3) And 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 20min to 60min.
Advantageous effects
One 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, the marine collagen and the xanthan gum are compounded to serve as the thickening agent, the effect of stabilizing the emulsion is achieved, and the cannabidiol emulsion is moisture-keeping and skin-care, is mild and does not irritate the skin.
(2) The cannabidiol emulsion containing marine collagen prepared by the technical scheme of the invention is free from floating oil, layering, precipitation and color change after being placed for 6 months under accelerated conditions (40 ℃ plus or minus 2 ℃ and 75% RH plus or minus 5%) or 12 months under long-term conditions (25 ℃ plus or minus 2 ℃ and 60% RH plus or minus 10%) and has good stability.
(3) Compared with other types of thickeners and single xanthan gum or marine collagen as the thickening component, the thickening component compounded by the xanthan gum and the marine collagen is more beneficial to avoiding phenomena of floating oil, layering, precipitation and discoloration after the cannabidiol emulsion is placed for 6 months under the acceleration condition (40 +/-2 ℃ and 75-RH +/-5%) or placed for 12 months under the long-term condition (25 +/-2 ℃ and 60 +/-10%) and is more beneficial to avoiding the degradation of the cannabidiol, and has unexpected technical effects.
(4) Compared with the single xanthan gum or marine collagen serving as the thickening component, when the thickening component compounded by the xanthan gum and the marine collagen is adopted, the xanthan gum and the marine collagen play a synergistic effect, the physical and chemical stability and the content stability of the obtained cannabidiol emulsion are greatly improved, and the unexpected technical effect is achieved.
(5) Compared with other types of emulsifiers and the emulsifier which is Tween 80 or span 80 alone, the compound emulsifier of Tween 80 and span 80 is used as the emulsifier, so that the phenomena of floating oil, layering and precipitation can be avoided after the cannabidiol emulsion is placed under the accelerated condition (40 +/-2 ℃ and 75% RH +/-5%) for 6 months or the long-term condition (25 +/-2 ℃ and 60% RH +/-10%) for 12 months, the degradation of the cannabidiol can be avoided, and the technical effect is unexpected.
(6) Compared with the method that the Tween 80 or the span 80 is used as the emulsifier alone, and the compounded emulsifier of the Tween 80 and the span 80 is used as the emulsifier, the Tween 80 and the span 80 have a synergistic effect, so that the physical and chemical stability and the content stability of the obtained cannabidiol emulsion are greatly improved, and an unexpected technical effect is achieved.
(7) Compared with other oil phases, the adoption of isopropyl myristate or zanthoxylum oleoresin as the oil phase is more favorable for the physicochemical stability and the content stability of the obtained cannabidiol emulsion, and has unexpected technical effects.
(8) The use of marine collagen with molecular weight distribution of 100 KD-500 KD is more favorable for improving the stability of the obtained cannabidiol emulsion, and more favorable for avoiding the phenomena of floating oil, delamination and precipitation after the obtained cannabidiol emulsion is placed for 6 months under accelerated conditions (40 ℃ plus or minus 2 ℃, 75 percent RH plus or minus 5%) or placed for 12 months under long-term conditions (25 ℃ plus or minus 2 ℃, 60 percent RH plus or minus 10%).
Definition of terms
In the context of the present invention, all numbers disclosed herein are approximate values, regardless of whether the word "about" or "approximately" is used. Based on the numbers disclosed, the numerical values of each number may vary by less than + -10% or reasonably as recognized by one of ordinary skill in the art, such as by + -1%, + -2%, + -3%, + -4%, or + -5%.
The term "marine collagen" is collagen extracted from the skin of a fish of marine origin or collagen extracted from the scales of marine fish.
The terms "above," "below," "within," and the like are to be understood to include the instant numbers, e.g., two or more means ≧ two.
The term "and/or" should be understood to mean any one of the options or a combination of any two or more of the options.
The term "wt%" means mass percent.
In the description of the specification, reference to the description of "one embodiment," "some embodiments," "an example," "a specific example," or "some examples" or the like 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 invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer 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, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, some non-limiting examples are further disclosed below to further explain the present invention in detail.
The reagents used in the present invention are either 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 more than or equal to 95 percent, and the molecular weight distribution is 100KD to 500KD.
Marine collagen is commercially available or can be obtained by the following preparation method: taking fish scales or fish skins of marine fishes as an extractant by using an acetic acid aqueous solution, extracting by adopting a homogenization technology, adding pepsin under a low temperature condition (such as 4 ℃), stirring for enzymolysis, purifying by a membrane separation technology, and freeze-drying to obtain the type I collagen (i.e. the marine collagen), wherein the obtained type I collagen has a complete triple helix structure, the purity is more than or equal to 95%, and the molecular weight is distributed between 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 cannabidiol is 1.0wt% of the total weight of cannabidiol emulsion, and isopropyl myristate is 5.0wt% of the total weight of cannabidiol emulsion, to obtain isopropyl myristate solution of 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, and after uniform stirring, the marine collagen compound thickener accounting for 1.0wt% of the total weight of the cannabidiol emulsion is added, wherein the marine collagen compound thickener comprises the following components in percentage by mass of 4:1 and marine collagen (150 KD), and continuously stirring until the components are uniformly mixed to obtain an aqueous phase solution;
(3) Slowly adding isopropyl myristate solution of cannabidiol into the water 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, the cannabidiol accounting for 2.0wt% of the total weight of the cannabidiol emulsion, and the isopropyl myristate accounting for 10.0wt% of the total weight of the cannabidiol emulsion, to obtain an isopropyl myristate solution of 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, and after the compound emulsifier is uniformly stirred, the marine collagen compound thickener accounting for 2.0wt% of the total weight of the cannabidiol emulsion is added, wherein the marine collagen compound thickener is prepared from the following raw materials in a mass ratio of 2:1 and marine collagen (250 KD), and continuously stirring until the components are uniformly mixed to obtain an aqueous phase solution;
(3) Slowly adding isopropyl myristate solution of cannabidiol into the water phase solution at 800rpm, and stirring for 40min to obtain white cannabidiol emulsion (oil-in-water emulsion).
Example 3: preparation of cannabidiol emulsion containing marine collagen
(1) Dissolving cannabidiol in zanthoxylum oil resin, the cannabidiol accounts for 1.0wt% of the total weight of the cannabidiol emulsion, and the zanthoxylum oil resin accounts for 10.0wt% of the total weight of the cannabidiol emulsion, so as to obtain a zanthoxylum oil resin 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 1.0wt% of the total weight of the cannabidiol emulsion, and after uniform stirring, the marine collagen compound thickener accounting for 0.5wt% of the total weight of the cannabidiol emulsion is added, wherein the marine collagen compound thickener comprises the following components in percentage by mass of 4:1, continuously stirring until the components are uniformly mixed to obtain an aqueous phase solution;
(3) Slowly adding fructus Zanthoxyli oleoresin solution of cannabidiol into the water phase solution, rotating at 1000rpm, and stirring thoroughly for 30min to obtain white cannabidiol emulsion (oil-in-water type emulsion).
Comparative example 1: cannabidiol emulsion preparation
(1) Dissolving cannabidiol in isopropyl myristate, wherein cannabidiol is 1.0wt% of the total weight of cannabidiol emulsion, and isopropyl myristate is 5.0wt% of the total weight of cannabidiol emulsion, to obtain isopropyl myristate solution of 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 1.0wt% of the total weight of the cannabidiol emulsion, after uniform stirring, sodium alginate accounting for 2.0wt% of the total weight of the cannabidiol emulsion is added, and the mixture is continuously stirred until uniform mixing is carried out, so as to obtain an aqueous phase solution;
(3) Slowly adding isopropyl myristate solution of cannabidiol into the water phase solution at 500rpm, and stirring thoroughly for 30min to obtain white cannabidiol emulsion (oil-in-water emulsion).
Comparative example 2: cannabidiol emulsion preparation
(1) Dissolving cannabidiol in isopropyl myristate, the cannabidiol accounting for 1.0wt% of the total weight of the cannabidiol emulsion, and the isopropyl myristate accounting for 5.0wt% of the total weight of the cannabidiol emulsion, to obtain an isopropyl myristate solution of 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 2.0wt% of the total weight of the cannabidiol emulsion, after uniform stirring, gelatin which accounts for 2.0wt% of the total weight of the cannabidiol emulsion is added, and the mixture is continuously stirred until uniform mixing is carried out, so as to obtain a water phase solution;
(3) Slowly adding isopropyl myristate solution of cannabidiol into the water phase solution at 500rpm, and stirring thoroughly for 30min to obtain white cannabidiol emulsion (oil-in-water emulsion).
Comparative example 3: cannabidiol emulsion preparation
(1) Dissolving cannabidiol in isopropyl myristate, wherein cannabidiol is 1.0wt% of the total weight of cannabidiol emulsion, and isopropyl myristate is 5.0wt% of the total weight of cannabidiol emulsion, to obtain isopropyl myristate solution of cannabidiol;
(2) Adding an emulsifier PEG40 hydrogenated castor oil into water, wherein the emulsifier has an HLB value of 14 and 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 the mixture is uniformly mixed to obtain an aqueous phase solution;
(3) Slowly adding isopropyl myristate solution of cannabidiol into the water 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, the cannabidiol accounting for 1.0wt% of the total weight of the cannabidiol emulsion, and the isopropyl myristate accounting for 5.0wt% of the total weight of the cannabidiol emulsion, to obtain an isopropyl myristate solution of 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, and after the mixture is uniformly stirred, a thickening component (a thickening agent or a compound thickening agent) accounting for 1.0wt% of the total weight of the cannabidiol emulsion is added, wherein the thickening component is shown in table 1, and the mixture is continuously stirred until the mixture is uniformly mixed, so that an aqueous phase solution is obtained;
(3) Slowly adding isopropyl myristate solution of cannabidiol into the water phase solution at 500rpm, and stirring thoroughly for 30min to obtain white cannabidiol emulsion (oil-in-water emulsion).
Table 1: component investigation of thickening Effect
Comparative examples 12 to 16: examination of emulsifiers
(1) Dissolving cannabidiol in isopropyl myristate, the cannabidiol accounting for 1.0wt% of the total weight of the cannabidiol emulsion, and the isopropyl myristate accounting for 5.0wt% of the total weight of the cannabidiol emulsion, to obtain an isopropyl myristate solution of cannabidiol;
(2) Adding an emulsifier shown in table 2 into water, wherein the emulsifier accounts for 2.0wt% of the total weight of the cannabidiol emulsion, uniformly stirring, and then adding a marine collagen compound thickener accounting for 1.0wt% of the total weight of the cannabidiol emulsion, wherein the marine collagen compound thickener comprises the following components in percentage by mass of 4:1, continuously stirring until the components are uniformly mixed to obtain an aqueous phase solution;
(3) Slowly adding isopropyl myristate solution of cannabidiol into the water phase solution at 500rpm, and stirring thoroughly for 30min to obtain white cannabidiol emulsion (oil-in-water emulsion).
Table 2: examination of emulsifiers
Comparative examples 20 to 22: investigation of oil phase
(1) Dissolving cannabidiol in an oil phase as shown in table 3, the cannabidiol comprising 1.0wt% of the total weight of the cannabidiol emulsion, and isopropyl myristate comprising 5.0wt% of the total weight of the cannabidiol emulsion, to obtain an oil phase solution of 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, and after uniform stirring, the marine collagen compound thickener accounting for 1.0wt% of the total weight of the cannabidiol emulsion is added, wherein the marine collagen compound thickener comprises the following components in percentage by mass of 4:1, continuously stirring until the components are uniformly mixed to obtain an aqueous phase solution;
(3) Slowly adding the oil phase solution of cannabidiol into the water phase solution, rotating at 500rpm, and stirring thoroughly for 30min to obtain white cannabidiol emulsion (oil-in-water type emulsion).
Table 3: investigation of oil phase
| Examples | Oil phase |
| Comparative example 19 | Palmitic acid isopropyl ester |
| Comparative example 20 | Capric acid triglyceride |
| Comparative example 21 | White oil |
| Comparative example 22 | Jojoba oil |
Example 4: stability survey
1. The detection indexes are as follows: delamination phenomenon and cannabidiol CBD content determination.
2. The experimental conditions are as follows: the 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 ℃, 75% RH. + -. 5%) for 6 months, respectively. The appearance and cannabidiol content of the samples were tested on day 0 and month 6 respectively. The results are shown in Table 4.
(1) Layering phenomenon: the sample was centrifuged at 3000rpm for 15 minutes by a centrifuge and observed for delamination.
(2) Cannabidiol content determination (high performance liquid chromatography): precisely preparing 0.15mg/mL cannabidiol methanol solution, and detecting by adopting an external standard method. A chromatographic column: a gilent TC-C18 column (250 mm. Times.4.6 mm,5 um); mobile phase: 0.1% formic acid water (a): gradient elution with 0.1% formic acid acetonitrile (B); the detection wavelength is 220nm, and the column temperature is 30 ℃; the flow rate is 1.2mL/min; the amount of the sample was 10. Mu.L.
Table 4: cannabidiol emulsion stability
And (4) conclusion: from the results of table 4, it can be seen that:
(1) Compared with other types of thickeners and the xanthan gum or marine collagen which is used as the thickening component alone, the thickening component compounded by the xanthan gum and the marine collagen is more favorable for avoiding the phenomena of layering and discoloration after the cannabidiol emulsion is placed under the acceleration condition (40 ℃ plus or minus 2 ℃, 75 percent RH plus or minus 5 percent) for 6 months, and is more favorable for avoiding the degradation of the cannabidiol, thereby having unexpected technical effects.
(2) Compared with the single xanthan gum or marine collagen serving as the thickening component, when the thickening component compounded by the xanthan gum and the marine collagen is adopted, the xanthan gum and the marine collagen play a synergistic effect, the physical and chemical stability and the content stability of the obtained cannabidiol emulsion are greatly improved, and the unexpected technical effect is achieved.
(3) Compared with other types of emulsifiers and the emulsifier which is the mixture of Tween 80 and span 80, the emulsifier which is the mixture of Tween 80 and span 80 is more favorable for avoiding the phenomena of floating oil and layering after the cannabidiol emulsion is placed for 6 months under the acceleration condition (40 ℃ plus or minus 2 ℃, 75 percent RH plus or minus 5 percent), and more favorable for avoiding the degradation of cannabidiol, and has unexpected technical effects.
(4) Compared with the method that the Tween 80 or the span 80 is singly adopted as the emulsifier, and the compound emulsifier of the Tween 80 and the span 80 is adopted as the emulsifier, the Tween 80 and the span 80 have the synergistic effect, the physical and chemical stability and the content stability of the obtained cannabidiol emulsion are greatly improved, and the unexpected technical effect is achieved.
(5) Compared with other oil phases, the adoption of isopropyl myristate or zanthoxylum oil resin as the oil phase is more favorable for the physicochemical stability and the content stability of the obtained cannabidiol emulsion, and has an unexpected technical effect.
While the methods of the present invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and modifications of the methods and applications described herein, as well as other suitable variations and combinations, may be made to implement and use the techniques of the present invention within the context, spirit and scope of the invention. Those skilled in the art can modify the process parameters appropriately to achieve the desired results with reference to the disclosure herein. It is specifically noted that all such substitutions and modifications will be apparent to those skilled in the art and are intended to be included within the present invention.
Claims (10)
1. A cannabidiol emulsion, comprising: cannabidiol, an emulsifier, an oil phase, a marine collagen compound thickener and water; the marine collagen compound thickener contains marine collagen and other thickeners.
2. A cannabidiol emulsion as claimed in claim 1, wherein the cannabidiol emulsion comprises cannabidiol in an amount of 0.1wt% to 5.0wt%, 1.0wt% to 5.0wt% or 1.0wt% to 2.0wt% based on the total weight of the cannabidiol emulsion.
3. A cannabidiol emulsion according to any of claims 1-2, wherein the emulsifier is present in the cannabidiol emulsion in an amount of 0.1wt% to 10.0wt%, 1.0wt% to 5.0wt% or 1.0wt% to 4.0wt% based on the total mass of the cannabidiol emulsion.
4. A cannabidiol emulsion as claimed in any of claims 1 to 3, wherein the content of the oil phase in the cannabidiol emulsion is from 1.0wt% to 40.0wt% or from 5.0wt% to 10.0wt% based on the total mass of the cannabidiol emulsion.
5. The cannabidiol emulsion of any one of claims 1-4, wherein the cannabidiol emulsion comprises a total content of marine collagen complex thickener of 0.1wt% to 10.0wt%, 0.5wt% to 5.0wt%, or 0.5wt% to 2.0wt%, based on the total weight of the cannabidiol emulsion; and/or
The mass ratio of other thickeners in the cannabidiol emulsion to the marine collagen is 1:1 to 5:1 or 2:1 to 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; or the total content of the water, the cannabidiol, the emulsifier, the oil phase and the marine collagen compound thickener in the cannabidiol emulsion is 100wt%.
7. The cannabidiol emulsion of any one of claims 1-6, wherein the oil phase comprises isopropyl myristate or zanthoxylum oleoresin; and/or
The other thickener is xanthan gum; and/or
The marine collagen is collagen extracted from marine fish skin or fish scales, the purity is more than or equal to 95 percent, and the molecular weight distribution is 100 KD-500 KD; and/or
The cannabidiol emulsion is free of alcohols.
8. Cannabidiol emulsion according to any of claims 1-7, wherein the emulsifier has an HLB value of 12-14; and/or
The emulsifier is Tween surfactant and span surfactant; and/or
The emulsifier is Tween 80 and span 80; and/or
The mass ratio of the Tween surfactants to the span surfactants is 2:1 to 10:1 or 2.6.
9. A method of making the cannabidiol emulsion of any one of claims 1-8, comprising the steps of:
(1) Dissolving cannabidiol in the 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) And mixing the mixed solution 1 and the mixed solution 2, and stirring to obtain the cannabidiol emulsion.
10. The method according to claim 9, wherein the stirring in step (3) is performed at a rotation speed of 200rpm to 5000rpm for 20min to 60min.
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