CN116473857A - Oil core coagulated bead, preparation method and cosmetics - Google Patents
Oil core coagulated bead, preparation method and cosmetics Download PDFInfo
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- CN116473857A CN116473857A CN202310352324.0A CN202310352324A CN116473857A CN 116473857 A CN116473857 A CN 116473857A CN 202310352324 A CN202310352324 A CN 202310352324A CN 116473857 A CN116473857 A CN 116473857A
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- Prior art keywords
- oil
- phase
- oil core
- gel bead
- acid
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- 239000011324 bead Substances 0.000 title claims abstract description 65
- 239000002537 cosmetic Substances 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 239000012071 phase Substances 0.000 claims abstract description 60
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 claims abstract description 47
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 claims abstract description 42
- GHVNFZFCNZKVNT-UHFFFAOYSA-N decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 claims abstract description 34
- PRAKJMSDJKAYCZ-UHFFFAOYSA-N squalane Chemical compound CC(C)CCCC(C)CCCC(C)CCCCC(C)CCCC(C)CCCC(C)C PRAKJMSDJKAYCZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000008385 outer phase Substances 0.000 claims abstract description 19
- HFVMEOPYDLEHBR-UHFFFAOYSA-N (2-fluorophenyl)-phenylmethanol Chemical compound C=1C=CC=C(F)C=1C(O)C1=CC=CC=C1 HFVMEOPYDLEHBR-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000005632 Capric acid (CAS 334-48-5) Substances 0.000 claims abstract description 17
- 239000005635 Caprylic acid (CAS 124-07-2) Substances 0.000 claims abstract description 17
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims abstract description 17
- JXTPJDDICSTXJX-UHFFFAOYSA-N n-Triacontane Natural products CCCCCCCCCCCCCCCCCCCCCCCCCCCCCC JXTPJDDICSTXJX-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229960002446 octanoic acid Drugs 0.000 claims abstract description 17
- 229940032094 squalane Drugs 0.000 claims abstract description 17
- 239000001384 succinic acid Substances 0.000 claims abstract description 17
- 239000013543 active substance Substances 0.000 claims abstract description 13
- ACTIUHUUMQJHFO-UHFFFAOYSA-N Coenzym Q10 Natural products COC1=C(OC)C(=O)C(CC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)C)=C(C)C1=O ACTIUHUUMQJHFO-UHFFFAOYSA-N 0.000 claims abstract description 11
- 235000017471 coenzyme Q10 Nutrition 0.000 claims abstract description 11
- GVJHHUAWPYXKBD-UHFFFAOYSA-N d-alpha-tocopherol Natural products OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000008384 inner phase Substances 0.000 claims abstract description 11
- NPCOQXAVBJJZBQ-UHFFFAOYSA-N reduced coenzyme Q9 Natural products COC1=C(O)C(C)=C(CC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)C)C(O)=C1OC NPCOQXAVBJJZBQ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229960001295 tocopherol Drugs 0.000 claims abstract description 11
- 229930003799 tocopherol Natural products 0.000 claims abstract description 11
- 235000010384 tocopherol Nutrition 0.000 claims abstract description 11
- 239000011732 tocopherol Substances 0.000 claims abstract description 11
- 229940035936 ubiquinone Drugs 0.000 claims abstract description 11
- GVJHHUAWPYXKBD-IEOSBIPESA-N α-tocopherol Chemical compound OC1=C(C)C(C)=C2O[C@@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-IEOSBIPESA-N 0.000 claims abstract description 11
- 150000002148 esters Chemical class 0.000 claims abstract description 10
- 235000010410 calcium alginate Nutrition 0.000 claims abstract description 8
- 239000000648 calcium alginate Substances 0.000 claims abstract description 8
- 229960002681 calcium alginate Drugs 0.000 claims abstract description 8
- OKHHGHGGPDJQHR-YMOPUZKJSA-L calcium;(2s,3s,4s,5s,6r)-6-[(2r,3s,4r,5s,6r)-2-carboxy-6-[(2r,3s,4r,5s,6r)-2-carboxylato-4,5,6-trihydroxyoxan-3-yl]oxy-4,5-dihydroxyoxan-3-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylate Chemical compound [Ca+2].O[C@@H]1[C@H](O)[C@H](O)O[C@@H](C([O-])=O)[C@H]1O[C@H]1[C@@H](O)[C@@H](O)[C@H](O[C@H]2[C@H]([C@@H](O)[C@H](O)[C@H](O2)C([O-])=O)O)[C@H](C(O)=O)O1 OKHHGHGGPDJQHR-YMOPUZKJSA-L 0.000 claims abstract description 8
- 125000001655 ubiquinone group Chemical group 0.000 claims abstract description 4
- 239000003921 oil Substances 0.000 claims description 86
- 235000019198 oils Nutrition 0.000 claims description 84
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 37
- 239000000499 gel Substances 0.000 claims description 28
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims description 26
- 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 claims description 18
- 235000010413 sodium alginate Nutrition 0.000 claims description 18
- 239000000661 sodium alginate Substances 0.000 claims description 18
- 229940005550 sodium alginate Drugs 0.000 claims description 18
- 239000002994 raw material Substances 0.000 claims description 17
- 229920001817 Agar Polymers 0.000 claims description 16
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims description 16
- 229920002148 Gellan gum Polymers 0.000 claims description 16
- 239000008272 agar Substances 0.000 claims description 16
- 235000010419 agar Nutrition 0.000 claims description 16
- 229910001424 calcium ion Inorganic materials 0.000 claims description 16
- 235000010492 gellan gum Nutrition 0.000 claims description 16
- 239000000216 gellan gum Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 235000011187 glycerol Nutrition 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 claims description 14
- QCDWFXQBSFUVSP-UHFFFAOYSA-N 2-phenoxyethanol Chemical compound OCCOC1=CC=CC=C1 QCDWFXQBSFUVSP-UHFFFAOYSA-N 0.000 claims description 13
- 229960005323 phenoxyethanol Drugs 0.000 claims description 13
- 235000010493 xanthan gum Nutrition 0.000 claims description 13
- 239000000230 xanthan gum Substances 0.000 claims description 13
- 229920001285 xanthan gum Polymers 0.000 claims description 13
- 229940082509 xanthan gum Drugs 0.000 claims description 13
- OBETXYAYXDNJHR-UHFFFAOYSA-N 2-Ethylhexanoic acid Chemical compound CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 claims description 8
- 239000003906 humectant Substances 0.000 claims description 8
- ACTIUHUUMQJHFO-UPTCCGCDSA-N coenzyme Q10 Chemical compound COC1=C(OC)C(=O)C(C\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CCC=C(C)C)=C(C)C1=O ACTIUHUUMQJHFO-UPTCCGCDSA-N 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 239000003755 preservative agent Substances 0.000 claims description 7
- 230000002335 preservative effect Effects 0.000 claims description 7
- FPIPGXGPPPQFEQ-OVSJKPMPSA-N all-trans-retinol Chemical compound OC\C=C(/C)\C=C\C=C(/C)\C=C\C1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-OVSJKPMPSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 239000012527 feed solution Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000002562 thickening agent Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 5
- 241000130781 Arnebia Species 0.000 claims description 4
- FPIPGXGPPPQFEQ-UHFFFAOYSA-N 13-cis retinol Natural products OCC=C(C)C=CC=C(C)C=CC1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-UHFFFAOYSA-N 0.000 claims description 3
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 claims description 3
- 239000004909 Moisturizer Substances 0.000 claims description 3
- 229940072056 alginate Drugs 0.000 claims description 3
- 235000010443 alginic acid Nutrition 0.000 claims description 3
- 229920000615 alginic acid Polymers 0.000 claims description 3
- 159000000007 calcium salts Chemical class 0.000 claims description 3
- 230000001333 moisturizer Effects 0.000 claims description 3
- 235000014593 oils and fats Nutrition 0.000 claims description 3
- 229920005862 polyol Polymers 0.000 claims description 3
- 150000003077 polyols Chemical class 0.000 claims description 3
- 229960003471 retinol Drugs 0.000 claims description 3
- 235000020944 retinol Nutrition 0.000 claims description 3
- 239000011607 retinol Substances 0.000 claims description 3
- 239000012266 salt solution Substances 0.000 claims description 3
- 235000015112 vegetable and seed oil Nutrition 0.000 claims description 3
- 239000008158 vegetable oil Substances 0.000 claims description 3
- 238000007667 floating Methods 0.000 abstract description 10
- 238000004062 sedimentation Methods 0.000 abstract description 8
- -1 ethyl caproic acid Chemical compound 0.000 abstract description 6
- 239000004519 grease Substances 0.000 abstract description 6
- FUZZWVXGSFPDMH-UHFFFAOYSA-N n-hexanoic acid Natural products CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 abstract description 6
- 238000009825 accumulation Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000002474 experimental method Methods 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 9
- 239000000686 essence Substances 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 8
- 239000000243 solution Substances 0.000 description 7
- SHZIWNPUGXLXDT-UHFFFAOYSA-N ethyl hexanoate Chemical compound CCCCCC(=O)OCC SHZIWNPUGXLXDT-UHFFFAOYSA-N 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 5
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 4
- 239000001110 calcium chloride Substances 0.000 description 4
- 229910001628 calcium chloride Inorganic materials 0.000 description 4
- MKJXYGKVIBWPFZ-UHFFFAOYSA-L calcium lactate Chemical compound [Ca+2].CC(O)C([O-])=O.CC(O)C([O-])=O MKJXYGKVIBWPFZ-UHFFFAOYSA-L 0.000 description 4
- 239000001527 calcium lactate Substances 0.000 description 4
- 229960002401 calcium lactate Drugs 0.000 description 4
- 235000011086 calcium lactate Nutrition 0.000 description 4
- 239000003094 microcapsule Substances 0.000 description 4
- 238000013112 stability test Methods 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000012295 chemical reaction liquid Substances 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000003925 fat Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 238000010438 heat treatment Methods 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
- 238000006864 oxidative decomposition reaction Methods 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 235000019871 vegetable fat Nutrition 0.000 description 2
- 239000007983 Tris buffer Substances 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 125000005456 glyceride group Chemical group 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 239000011325 microbead Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 238000000399 optical microscopy Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000011197 physicochemical method Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 210000002966 serum Anatomy 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920001059 synthetic polymer Polymers 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/37—Esters of carboxylic acids
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/11—Encapsulated compositions
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/56—Compounds, absorbed onto or entrapped into a solid carrier, e.g. encapsulated perfumes, inclusion compounds, sustained release forms
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The application relates to the field of cosmetics, and relates to an oil core gel bead, a preparation method and cosmetics. The present application provides an oil core gel bead comprising an outer phase and an inner phase; the outer phase comprises: calcium alginate; the internal phase comprises: grease and oil-soluble actives; the oil is caprylic acid/capric acid/succinic acid triglyceride, and squalane; the oil-soluble active substance is ubiquinone, tocopherol, radix Arnebiae extract; the internal phase comprises the following components in percentage by mass: 60-90% of caprylic acid/capric acid/succinic acid triglyceride, 5-30% of triglyceride (ethyl caproic acid) ester, 2.5-30% of squalane and the balance of oil-soluble active substances. According to the oil core gel bead, the caprylic acid/capric acid/succinic acid triglyceride is introduced into the inner phase, so that the oil core gel bead with excellent sedimentation and stable accumulation can be formed, and the problems of influence on subsequent experiments or production caused by floating and oil slick of the oil core coated gel bead are effectively solved.
Description
Technical Field
The application relates to the field of cosmetics, in particular to an oil core gel bead, a preparation method and cosmetics.
Background
The microcapsule/gel bead coating technology is a technology which uses natural or synthetic polymer materials to form one or more layers of semi-permeable or airtight outer phases, uses solid or liquid and the like as inner phases to coat, and relates to multidisciplinary and multi-field intersection. The technology is widely applied to various industries such as printing, medicines, foods and the like.
However, the technology has many problems of relatively complex production operation, limited available raw materials/systems, transportation crushing/deformation, skin feel requirement, cost control and the like, and is still immature in application in the cosmetic field and is not widely applied at present.
By utilizing the biphase wrapping technology, the effects of keeping fresh, slowly releasing the active substances and the like can be achieved while the visual sense pleasure is improved, so that the application of the technology in the cosmetic industry is promoted to have important significance.
The microcapsule/bead encapsulation technology can be broadly divided into chemical, physical and physicochemical methods according to the preparation route. The preparation methods commonly used in the cosmetic field are: dripping method, spraying method, stirring granulation method, etc. However, the oil core coagulated beads prepared by the prior preparation processes often have the problems of accumulation floating on the upper layer of the liquid surface, leakage of the oil core and the like.
Disclosure of Invention
The embodiment of the application aims at providing an oil core gel bead, a preparation method and cosmetics.
In a first aspect, the present application provides an oil core bead comprising an outer phase and an inner phase; the outer phase comprises: calcium alginate; the internal phase comprises: oils and fats, and oil-soluble actives; the oil is caprylic acid/capric acid/succinic acid triglyceride, and squalane; the oil-soluble active substance is ubiquinone, tocopherol, radix Arnebiae extract; the internal phase comprises, by mass, 60-90% of caprylic/capric/succinic triglyceride, 5-30% of triglyceride (ethyl caproic acid) ester, 2.5-30% of squalane, and the balance of oil-soluble active substances.
According to the oil core gel bead, the caprylic acid/capric acid/succinic acid triglyceride is introduced into the inner phase, so that the oil core gel bead with excellent sedimentation and stable accumulation can be formed, and the problems of influence on subsequent experiments or production caused by floating and oil slick of the oil core coated gel bead are effectively solved.
In other embodiments of the present application, the outer phase further comprises: water, humectant, preservative, thickener and solid agent;
optionally, the humectant comprises polyols.
In other embodiments of the present application, the moisturizer comprises: at least one of glycerol, dipropylene glycol, PEG/PPG-14/7 dimethyl ether;
the preservative comprises phenoxyethanol.
Optionally, the thickener and the solidifying agent comprise at least one of xanthan gum, gellan gum, agar.
In other embodiments of the present application, the raw materials of the external phase include, in mass percent: glycerin 1.0-10.0%, dipropylene glycol 1.0-10.0%, phenoxyethanol 0.1-1.0%, PEG/PPG-14/7 dimethyl ether 0.5-5.0%, xanthan gum 0-0.5%, gellan gum 0.1-1.0%, agar 0-1.0%, sodium alginate 0.4-0.8%, calcium ion 0.2-0.5%, and water in balance.
In other embodiments of the present application, the internal phase further comprises: grease and oil-soluble actives;
optionally, the oil is selected from caprylic acid/capric acid/succinic acid triglyceride, and squalane; the oil-soluble actives include: ubiquinone, tocopherol, arnebia root extract.
In other embodiments of the present application, the wall forming material of the outer phase comprises: sodium alginate and calcium ions; the mass ratio of the sodium alginate of the external phase to the calcium ions is (0.4-0.8): (0.2-0.5).
In other embodiments of the present application, the raw materials of the external phase include, in mass percent: glycerin 1.0-10.0%, dipropylene glycol 1.0-10.0%, phenoxyethanol 0.1-1.0%, PEG/PPG-14/7 dimethyl ether 0.5-5.0%, xanthan gum 0-0.5%, gellan gum 0.1-1.0%, agar 0-1.0%, sodium alginate 0.4-0.8%, calcium ion 0.2-0.5%, and water in balance.
In other embodiments of the present application, the internal phase comprises, in mass percent: 60-90% of caprylic acid/capric acid/succinic acid triglyceride, 5-30% of triglyceride (ethyl caproic acid) ester and 2.5-30% of squalane; the balance being oil-soluble active;
optionally, the internal phase comprises, in mass percent: 60-90% of caprylic acid/capric acid/succinic acid triglyceride, 5-30% of triglyceride (ethyl caproic acid) ester and 2.5-30% of squalane; the balance being oil-soluble active.
In other embodiments of the present application, the oil-soluble actives include: ubiquinone, tocopherol, or labile oil soluble actives; optionally, the labile oil-soluble active is selected from vegetable oils and fats that are susceptible to oxidative decomposition; alternatively, the labile oil-soluble active is selected from arnebia root extract, retinol and derivatives thereof.
In a second aspect, the present application provides a method of preparing an oil core coagulated bead comprising:
uniformly mixing caprylic acid/capric acid/succinic acid triglyceride, other grease and oil-soluble active substances to obtain an internal phase raw material liquid;
the inner phase feed solution and the outer phase feed solution comprising alginate are simultaneously drained into the calcium salt solution.
In a third aspect, the present application provides a cosmetic comprising the oil core globules provided in the first aspect above.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered limiting the scope, and that other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is an external view (side view) of the oil core beads prepared in example 3 at a first view angle;
fig. 2 is an external view (side view) of the first view angle of comparative example 1.
FIG. 3 is an external view (top view) of the oil core beads prepared in example 3 from a second perspective;
FIG. 4 is a microstructure of the oil core beads prepared in example 3.
Detailed Description
For the purposes of making the objects, technical solutions and advantages of the embodiments of the present application more clear, the technical solutions in the embodiments of the present application will be clearly and completely described below, and it is obvious that the described embodiments are some embodiments of the present application, but not all embodiments.
Thus, the following detailed description of the embodiments of the present application is not intended to limit the scope of the application, as claimed, but is merely representative of selected embodiments of the application. All other embodiments, which can be made by one of ordinary skill in the art based on the embodiments herein without making any inventive effort, are intended to be within the scope of the present application.
Because the density of grease is smaller than that of water, when the content of the wrapped oil core is higher, the inventor discovers that the problems of accumulation on the upper layer of the reaction liquid, leakage of the oil core and the like often occur in the preparation process of the oil-in-oil gel beads such as a dripping method, a spraying method and the like which are conventionally used by the existing calcium alginate and the like, and the subsequent dripping production flow is influenced.
Embodiments of the present application provide an oil core bead comprising an outer phase and an inner phase; the outer phase comprises: calcium alginate; the internal phase comprises: oils and fats, and oil-soluble actives; the oil is caprylic acid/capric acid/succinic acid triglyceride, triglyceride and tri (ethylhexanoic acid) ester; the oil-soluble active substance is ubiquinone, tocopherol, and radix Arnebiae extract; the internal phase comprises, by mass, 60-90% of caprylic/capric/succinic triglyceride, 5-30% of triglyceride (ethyl caproic acid) ester, 2.5-30% of squalane, and the balance of oil-soluble active substances.
According to the oil core gel bead, the caprylic acid/capric acid/succinic acid triglyceride is introduced into the internal phase (oil core/oil phase), and the caprylic acid/capric acid/succinic acid triglyceride is introduced into the internal phase, so that the oil core gel bead with excellent sedimentation and stable accumulation can be formed, and the problems of influence on subsequent experiments or production caused by floating of the oil core coated gel bead and floating oil are effectively solved.
Further, in other embodiments of the present application, the wall forming raw materials of the outer phase include: sodium alginate and calcium ions; sodium alginate and calcium ion (0.4-0.8): (0.2-0.5).
Further, in some embodiments of the present application, the above-mentioned external phase further includes: water, a humectant, a preservative, a thickener and a solid.
Further, in some embodiments of the present application, the humectant described above includes polyols.
Further, in some embodiments of the present application, the moisturizer described above includes: at least one of glycerol, dipropylene glycol, PEG/PPG-14/7 dimethyl ether.
The preservative comprises phenoxyethanol.
Illustratively, in some embodiments of the present application, the humectants described above are selected from glycerin and dipropylene glycol; or in some embodiments of the present application, the humectant described above is selected from glycerin, dipropylene glycol, and PEG/PPG-14/7 dimethyl ether.
Further, in some embodiments of the present application, the preservative is selected from phenoxyethanol.
Further, in some embodiments of the present application, the thickener and the solidifying agent are selected from at least one of xanthan gum, gellan gum, agar.
By controlling the mass ratio of sodium alginate and calcium ions within the above-described range, excellent formability of the oil core globules can be obtained.
Illustratively, the mass ratio of sodium alginate to calcium ions in the outer phase material is 0.4:0.2 to 0.5; or 0.5:0.2 to 0.5; or 0.6:0.2 to 0.5; or 0.7:0.2 to 0.5; or 0.8:0.2 to 0.5.
Further, in some embodiments of the present application, the raw materials of the external phase include, in mass percent: glycerin 1.0-10.0%, dipropylene glycol 1.0-10.0%, phenoxyethanol 0.1-1.0%, PEG/PPG-14/7 dimethyl ether 0.5-5.0%, xanthan gum 0-0.5%, gellan gum 0.1-1.0%, agar 0-1.0%, sodium alginate 0.4-0.8%, calcium ion 0.2-0.5%, and water in balance.
Further alternatively, in some embodiments of the present application, the raw materials of the external phase include, in mass percent: 2.0 to 8.0 percent of glycerin, 2.0 to 8.0 percent of dipropylene glycol, 0.2 to 0.9 percent of phenoxyethanol, 0.6 to 4.0 percent of PEG/PPG-14/7 dimethyl ether, 0.1 to 0.3 percent of xanthan gum, 0.2 to 0.9 percent of gellan gum, 0.1 to 0.9 percent of agar, 0.5 to 0.7 percent of sodium alginate, 0.3 to 0.4 percent of calcium ions and the balance of water.
Illustratively, in some embodiments of the present application, the raw materials of the external phase comprise, in mass percent:
glycerol 1.5%, 2.0%, 3%, 4%, 5%, 6%, 7%, 8% or 9%;
dipropylene glycol 1.5%, 2.0%, 3%, 4%, 5%, 6%, 7%, 8%, or 9%;
phenoxyethanol 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, or 0.8%;
PEG/PPG-14/7 dimethyl 1%, 2%, 3%, 4% or 4.5%;
xanthan gum 0.1%, 0.2%, 0.3% or 0.4%;
gellan gum 0.12%, 0.15%, 0.2%, 0.3%, 0.4%, 0.5%, or 0.8%;
agar 0.1%, 0.5%, 0.6%, 0.7%, 0.8% or 0.9%;
sodium alginate 0.5%, 0.6%, 0.7% or 0.8%;
0.2%, 0.3%, 0.4% or 0.5% of calcium ions.
In some embodiments of the present application, the internal phase comprises: grease and oil-soluble actives.
In some embodiments of the present application, the lipid is selected from caprylic/capric/succinic triglyceride, triglyceride tri (ethylhexanoate), squalane.
In some embodiments of the present application, the internal phase comprises, in mass percent: 60-90% of caprylic acid/capric acid/succinic acid triglyceride, 5-30% of triglyceride (ethyl caproic acid) ester and 2.5-30% of squalane; the balance being oil-soluble active.
Illustratively, in some embodiments of the present application, the internal phase comprises:
60%, 70%, 80%, 85% or 90% caprylic/capric/succinic triglyceride;
6%, 7%, 8%, 10%, 20% or 30% of tris (ethylhexanoate) glyceride;
3%, 7%, 8%, 10%, 20% or 30% squalane;
the balance being oil-soluble active.
Further, in some embodiments of the present application, the oil-soluble active includes: ubiquinone, tocopherol, or labile oil soluble actives; optionally, the labile oil-soluble active is selected from vegetable oils and fats that are susceptible to oxidative decomposition; alternatively, the labile oil-soluble active is selected from arnebia root extract, retinol and derivatives thereof.
In a second aspect, some embodiments of the present application provide a method for preparing an oil core gel bead, comprising:
uniformly mixing caprylic acid/capric acid/succinic acid triglyceride, other grease and oil-soluble active substances to obtain an internal phase raw material liquid;
the inner phase feed solution and the outer phase feed solution comprising alginate are simultaneously drained into the calcium salt solution.
Further, in some embodiments of the present application, 1000±200 μm oil core-coated beads excellent in sedimentation were prepared by a microfluidic technique molding and a dripping method using a calcium alginate system by adding the components caprylic/capric/succinic triglyceride.
Specifically, the method comprises the following steps:
(1) Configuring a first phase: according to the proportion of any of the previous embodiments, deionized water, glycerol, dipropylene glycol, xanthan gum, gellan gum, sodium alginate, phenoxyethanol, PEG/PPG-14/7 dimethyl ether and agar are mixed, then heated to above 90 ℃, kept for 20min, and homogenized at 8000rpm for 2min;
(2) Configuring a second phase: mixing caprylic/capric/succinic triglyceride, tri (ethylhexanoic acid) ester, squalane, ubiquinone, tocopherol, and radix Arnebiae extract according to the proportion of any embodiment, and stirring to uniformity;
(3) And (3) configuring a third phase: calcium chloride or calcium lactate was formulated as a 0.3% (w/w) soak.
(4) The first phase and the second phase are drained into a calcium chloride or calcium lactate solution of the third phase by means of pump force by adopting a T-shaped pipe, so that oil core-coated gel beads are formed.
In addition to the dropping method of the oil core coagulated beads, the other optional embodiments of the present application are also applicable to a preparation method of oil core microcapsules such as an O/W/O microcapsule extraction method in a stirring granulation method, and can increase the sedimentation rate, reduce the proportion of oil-containing coagulated beads at a water-oil intersection, and reduce the cleaning residue of an external medium oil phase.
In a third aspect, some embodiments of the present application provide a cosmetic comprising the oil core globules provided in any one of the preceding embodiments.
The features and capabilities of the present application are described in further detail below in connection with the examples:
the oil core coated gel beads of 1000+/-200 mu m are prepared by adopting a calcium alginate system and adopting a microfluidic technology mould shape and a dripping method.
(one) preparation of oil core gel beads
The oil core coagulated beads, the external phase raw materials include: deionized water, glycerol, butanediol, xanthan gum, gellan gum, sodium alginate, calcium ions, agar, PEG/PPG-14/7 dimethyl ether, and antiseptic. The internal phase raw materials comprise: caprylic/capric/succinic triglyceride, squalane, ubiquinone, tocopherol, and radix Arnebiae extract.
In each of the examples and comparative examples, the specific raw materials and contents of the oil core beads are shown in Table 1.
TABLE 1 raw material components and contents (w/w%) of examples and comparative examples
The preparation method comprises the following steps:
taking a microfluidic-model-based dripping method as an example, 1000+/-200 mu m oil core-coated gel beads are prepared in the example and the comparative example, and the method comprises the following steps:
(1) Configuring a first phase: mixing deionized water, glycerol, dipropylene glycol, xanthan gum, gellan gum, sodium alginate, phenoxyethanol, PEG/PPG-14/7 dimethyl ether and agar according to the proportion shown in Table 1, heating to above 90deg.C, maintaining the temperature for 20min, at 8000rpm, homogenizing for 2min;
(2) Configuring a second phase: mixing caprylic acid/capric acid/succinic acid triglyceride, triglyceride (ethyl caproate), squalane, ubiquinone, tocopherol, and radix Arnebiae extract according to the ratio of table 1, and stirring to uniformity;
(3) And (3) configuring a third phase: calcium chloride or calcium lactate was formulated as a 0.3% (w/w) soak.
(4) And (3) simultaneously draining the first phase prepared in the step (1) and the second phase prepared in the step (2) into the calcium chloride or calcium lactate solution of the third phase prepared in the step (3) by using a T-shaped pipe by means of pumping force to form oil core coated gel beads. The first phase and the third phase react to form an outer phase; the second phase is an internal phase, and is surrounded by an external phase.
(5) Filtering the oil core coagulated beads prepared in the step (4), and cleaning with deionized water.
(II) preparing essence matrix:
the composition and composition of the matrix are shown in Table 2.
TABLE 2 raw material composition of essence matrix and content (w/w%)
The specific preparation method of the essence matrix comprises the following steps:
heating the phase A to 85 ℃, preserving heat for 20min, and homogenizing at 7000rpm for 2min; stirring and cooling, and adding phase B into phase A; the temperature is reduced to below 40 ℃ and phase C is added; stirring uniformly and discharging.
And (III) preparing essence.
Soaking the oil core beads prepared in the first step and the comparative example in an external phase for more than 1 hour to fully react, filtering, cleaning by using deionized water, and adding the solution into the matrix prepared in the second step to prepare the oil-containing bead essence.
And (IV) testing the performance of the essence.
Experimental example 1 drip status, formability and stability test:
test sample: examples and comparative examples, and the essences thereof.
The testing method comprises the following steps:
1. drop state: visually observing sedimentation of oil core coagulated beads and oil floating condition thereof
2. Formability: visually observing whether the ball forming form of the oil core coagulated beads is complete
3. Stability test:
and (3) centrifuging, high-temperature, low-temperature and high-low-temperature alternation and normal-temperature treatment are carried out on each bead essence sample. The process parameters were as follows:
centrifugation (1500 rpm,10 min), high temperature (45 ℃,6 months), low temperature (-18 ℃,6 months), high-low temperature alternation (45 ℃ and-18 ℃ alternation, 6 months), normal temperature (25 ℃,6 months).
4. Skin feel evaluation: the oil core gel bead essence was applied to the arm and evaluated for residual feel and spreadability.
The results of each performance test are shown in Table 3.
TABLE 3 dripping State, formability and 6 month stability test results
As can be seen from table 3, all the examples of oil core beads added with 60-90% caprylic/capric/succinic triglyceride of the present application have excellent sedimentation properties, and do not generate the phenomena of floating of the beads and surface oil slivers, affecting the subsequent dripping. On the other hand, it was found from comparison of example 3 with comparative examples 1, 2 and 3 that the sedimentation properties of oil-containing globules were significantly affected when the content of other components in the first and third phases was kept constant while the amount of caprylic/capric/succinic triglyceride added in the second phase was decreased and the ratio of triglyceride to squalane was increased. From the above, it can be demonstrated that the oil core beads having 60 to 90% of caprylic/capric/succinic triglyceride added to the oil phase have excellent bulk stability.
Further, in comparative examples 1, 2 and 3, when the content of caprylic/capric/succinic triglyceride is less than 60%, the oil core coated beads floating on the surface of the soaking solution are stacked and collided, resulting in the influence of floating oil (refer to fig. 2); and when the oil slick is too much, the condensed beads which are dropped later cannot enter the soaking liquid for reaction due to the separation of the surface layer oil slick. In addition, as can be seen from Table 3, the lower the content of caprylic/capric/succinic triglyceride, the more pronounced the phenomenon of oil slick generation.
Further, as can be seen from table 3, examples 4, 5, 6 were inferior in skin feel. As is clear from Table 1, the higher the content of the solid agent such as gellan gum and agar, the higher the hardness of the resulting microbead, and the more serious the residual feeling. On the other hand, in examples 5 and 6, small bubbles appeared in the serum in the low-temperature and high-temperature alternating stability test. This phenomenon is considered to be a phenomenon in which bubbles are generated by low-temperature differentiated water when the added amount of gellan gum or agar is too high. Therefore, when there is a certain demand for skin feel and appearance, it is preferable that the gellan gum and agar content be less than 0.5%.
In summary, it is understood that example 3 is preferred in combination with the results of the centrifugal stability, the high-low temperature stability and the skin feel evaluation.
Experimental example 2
The appearance and microstructure of the oil core beads prepared in example 3 were examined. Wherein the microstructure of the oil core coagulated beads prepared in example 3 was observed by optical microscopy. The results are shown in figure 1, figure 3 and figure 4 of the specification.
FIG. 1 is an external view (side view) of the oil core beads prepared in example 3, which were settled and piled up at the bottom of a beaker, at a first view angle; fig. 2 is an external view (side view) of comparative example 1 at a first view angle, in which the oil core globules float above the reaction liquid and oil floating occurs on the surface layer of the liquid surface. Fig. 3 is an external view (top view) of the oil core beads prepared in example 3 from a second perspective. FIG. 4 is a microstructure of the oil core beads prepared in example 3.
As can be seen from fig. 1, fig. 3 and fig. 4, the inner phase of the oil core gel bead prepared in the embodiment of the application is an oil phase, the outer phase is a spherical calcium alginate capsule, and the oil core gel bead is coated with the oil core.
The foregoing description is only of the preferred embodiments of the present application and is not intended to limit the same, but rather, various modifications and variations may be made by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principles of the present application should be included in the protection scope of the present application.
Claims (10)
1. An oil core bead comprising an outer phase and an inner phase; the outer phase comprises: calcium alginate; the internal phase comprises: oils and fats, and oil-soluble actives; the oil is caprylic acid/capric acid/succinic acid triglyceride, triglyceride and tri (ethylhexanoic acid) ester; the oil-soluble active substance is ubiquinone, tocopherol, and radix Arnebiae extract; the internal phase component comprises, by mass, 60-90% of the caprylic/capric/succinic triglyceride, 5-30% of the tri (ethylhexanoic) ester, 2.5-30% of the squalane, and the balance of the oil-soluble active substance.
2. The oil core gel bead of claim 1, wherein,
the oil-soluble actives include: at least one of ubiquinone, tocopherol, or an unstable oil soluble active.
3. The oil core gel bead of claim 2, wherein,
the unstable oil-soluble active substance is vegetable oil which is easy to be oxidatively decomposed; optionally, the labile oil-soluble active is selected from arnebia root extract, retinol and derivatives thereof.
4. The oil core gel bead according to any one of claim 1 to 3,
the outer phase further comprises: water, humectant, preservative, thickener and solid agent;
optionally, the humectant comprises polyols.
5. The oil core gel bead of claim 4, wherein,
the moisturizer comprises: at least one of glycerol, dipropylene glycol, PEG/PPG-14/7 dimethyl ether;
the preservative comprises phenoxyethanol;
optionally, the thickener and the solidifying agent comprise at least one of xanthan gum, gellan gum and agar.
6. The oil core gel bead of claim 1, wherein,
1, the external phase wall forming raw material comprises: sodium alginate and calcium ions; the mass ratio of the sodium alginate of the external phase to the calcium ions is (0.4-0.8): (0.2-0.5).
7. The oil core gel bead of claim 6, wherein,
the external phase comprises the following raw materials in percentage by mass: glycerin 1.0-10.0%, dipropylene glycol 1.0-10.0%, phenoxyethanol 0.1-1.0%, PEG/PPG-14/7 dimethyl ether 0.5-5.0%, xanthan gum 0-0.5%, gellan gum 0.1-1.0%, agar 0-1.0%, sodium alginate 0.4-0.8%, calcium ion 0.2-0.5%, and water in balance.
8. The oil core gel bead of claim 6, wherein,
the external phase comprises the following raw materials in percentage by mass: glycerin 1.0-10.0%, dipropylene glycol 1.0-10.0%, phenoxyethanol 0.1-1.0%, PEG/PPG-14/7 dimethyl ether 0.5-5.0%, xanthan gum 0-0.5%, gellan gum 0.2-1.0%, agar 0-1.0%, sodium alginate 0.4-0.8%, calcium ion 0.2-0.5%, and water in balance.
9. A method of preparing an oil core gel bead according to any one of claims 1 to 8, comprising:
uniformly mixing the caprylic acid/capric acid/succinic acid triglyceride, the triglyceride (ethylhexanoic acid), the squalane and the oil-soluble active substance to obtain an internal phase feed liquid;
the inner phase feed solution and the outer phase feed solution comprising alginate are simultaneously drained into a calcium salt solution.
10. A cosmetic comprising the oil core gel bead of any one of claims 1 to 9.
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