CN117100663A - Preparation method of evodia rutaecarpa fruit extract, composition containing evodia rutaecarpa fruit extract and application of composition - Google Patents
Preparation method of evodia rutaecarpa fruit extract, composition containing evodia rutaecarpa fruit extract and application of composition Download PDFInfo
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- CN117100663A CN117100663A CN202311332741.5A CN202311332741A CN117100663A CN 117100663 A CN117100663 A CN 117100663A CN 202311332741 A CN202311332741 A CN 202311332741A CN 117100663 A CN117100663 A CN 117100663A
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- extract
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- evodia rutaecarpa
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- cosmetic
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- 241001078983 Tetradium ruticarpum Species 0.000 title claims abstract description 62
- 239000000203 mixture Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 235000013399 edible fruits Nutrition 0.000 title abstract description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 46
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229930013930 alkaloid Natural products 0.000 claims abstract description 17
- 150000003797 alkaloid derivatives Chemical class 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 8
- 238000002791 soaking Methods 0.000 claims abstract description 8
- YPFDHNVEDLHUCE-UHFFFAOYSA-N propane-1,3-diol Chemical compound OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000010298 pulverizing process Methods 0.000 claims abstract description 6
- 238000004821 distillation Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000001256 steam distillation Methods 0.000 claims abstract description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 4
- 239000002537 cosmetic Substances 0.000 claims description 33
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 claims description 20
- 239000002994 raw material Substances 0.000 claims description 16
- 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 description 11
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 claims description 10
- GOQYKNQRPGWPLP-UHFFFAOYSA-N n-heptadecyl alcohol Natural products CCCCCCCCCCCCCCCCCO GOQYKNQRPGWPLP-UHFFFAOYSA-N 0.000 claims description 10
- KBDSLGBFQAGHBE-MSGMIQHVSA-N limonin Chemical compound C=1([C@H]2[C@]3(C)CC[C@H]4[C@@]([C@@]53O[C@@H]5C(=O)O2)(C)C(=O)C[C@@H]2[C@]34COC(=O)C[C@@H]3OC2(C)C)C=COC=1 KBDSLGBFQAGHBE-MSGMIQHVSA-N 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000006210 lotion Substances 0.000 claims description 8
- 239000003755 preservative agent Substances 0.000 claims description 8
- 239000006071 cream Substances 0.000 claims description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 6
- 235000004347 Perilla Nutrition 0.000 claims description 6
- 229920002385 Sodium hyaluronate Polymers 0.000 claims description 6
- 229920002125 Sokalan® Polymers 0.000 claims description 6
- 229960001631 carbomer Drugs 0.000 claims description 6
- 230000002335 preservative effect Effects 0.000 claims description 6
- 229940010747 sodium hyaluronate Drugs 0.000 claims description 6
- YWIVKILSMZOHHF-QJZPQSOGSA-N sodium;(2s,3s,4s,5r,6r)-6-[(2s,3r,4r,5s,6r)-3-acetamido-2-[(2s,3s,4r,5r,6r)-6-[(2r,3r,4r,5s,6r)-3-acetamido-2,5-dihydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-2-carboxy-4,5-dihydroxyoxan-3-yl]oxy-5-hydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-3,4,5-trihydroxyoxane-2- Chemical compound [Na+].CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](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]3[C@@H]([C@@H](O)[C@H](O)[C@H](O3)C(O)=O)O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@@H](C(O)=O)O1 YWIVKILSMZOHHF-QJZPQSOGSA-N 0.000 claims description 6
- RFVNOJDQRGSOEL-UHFFFAOYSA-N 2-hydroxyethyl octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCCO RFVNOJDQRGSOEL-UHFFFAOYSA-N 0.000 claims description 5
- 235000021302 avocado oil Nutrition 0.000 claims description 5
- 239000008163 avocado oil Substances 0.000 claims description 5
- 235000019437 butane-1,3-diol Nutrition 0.000 claims description 5
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 5
- 239000000839 emulsion Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 229940078812 myristyl myristate Drugs 0.000 claims description 5
- JXTPJDDICSTXJX-UHFFFAOYSA-N n-Triacontane Natural products CCCCCCCCCCCCCCCCCCCCCCCCCCCCCC JXTPJDDICSTXJX-UHFFFAOYSA-N 0.000 claims description 5
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 claims description 5
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 5
- -1 polydimethylsiloxane Polymers 0.000 claims description 5
- 229940032094 squalane Drugs 0.000 claims description 5
- DZKXJUASMGQEMA-UHFFFAOYSA-N tetradecyl tetradecanoate Chemical compound CCCCCCCCCCCCCCOC(=O)CCCCCCCCCCCCC DZKXJUASMGQEMA-UHFFFAOYSA-N 0.000 claims description 5
- LADGBHLMCUINGV-UHFFFAOYSA-N tricaprin Chemical compound CCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCC)COC(=O)CCCCCCCCC LADGBHLMCUINGV-UHFFFAOYSA-N 0.000 claims description 5
- DNIAPMSPPWPWGF-VKHMYHEASA-N (+)-propylene glycol Chemical compound C[C@H](O)CO DNIAPMSPPWPWGF-VKHMYHEASA-N 0.000 claims description 4
- KIUKXJAPPMFGSW-DNGZLQJQSA-N (2S,3S,4S,5R,6R)-6-[(2S,3R,4R,5S,6R)-3-Acetamido-2-[(2S,3S,4R,5R,6R)-6-[(2R,3R,4R,5S,6R)-3-acetamido-2,5-dihydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-2-carboxy-4,5-dihydroxyoxan-3-yl]oxy-5-hydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylic acid Chemical compound CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](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]3[C@@H]([C@@H](O)[C@H](O)[C@H](O3)C(O)=O)O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@@H](C(O)=O)O1 KIUKXJAPPMFGSW-DNGZLQJQSA-N 0.000 claims description 4
- 229940035437 1,3-propanediol Drugs 0.000 claims description 4
- 244000308505 Filipendula ulmaria Species 0.000 claims description 4
- 235000016622 Filipendula ulmaria Nutrition 0.000 claims description 4
- 229920002674 hyaluronan Polymers 0.000 claims description 4
- 229960003160 hyaluronic acid Drugs 0.000 claims description 4
- 229920000166 polytrimethylene carbonate Polymers 0.000 claims description 4
- HDTRYLNUVZCQOY-UHFFFAOYSA-N α-D-glucopyranosyl-α-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OC1C(O)C(O)C(O)C(CO)O1 HDTRYLNUVZCQOY-UHFFFAOYSA-N 0.000 claims description 3
- BIVBRWYINDPWKA-VLQRKCJKSA-L Glycyrrhizinate dipotassium Chemical compound [K+].[K+].O([C@@H]1[C@@H](O)[C@H](O)[C@H](O[C@@H]1O[C@H]1CC[C@]2(C)[C@H]3C(=O)C=C4[C@@H]5C[C@](C)(CC[C@@]5(CC[C@@]4(C)[C@]3(C)CC[C@H]2C1(C)C)C)C(O)=O)C([O-])=O)[C@@H]1O[C@H](C([O-])=O)[C@@H](O)[C@H](O)[C@H]1O BIVBRWYINDPWKA-VLQRKCJKSA-L 0.000 claims description 3
- HDTRYLNUVZCQOY-WSWWMNSNSA-N Trehalose Natural products O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 HDTRYLNUVZCQOY-WSWWMNSNSA-N 0.000 claims description 3
- HDTRYLNUVZCQOY-LIZSDCNHSA-N alpha,alpha-trehalose Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 HDTRYLNUVZCQOY-LIZSDCNHSA-N 0.000 claims description 3
- 229940101029 dipotassium glycyrrhizinate Drugs 0.000 claims description 3
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 claims description 3
- 239000000686 essence Substances 0.000 claims description 2
- 239000000499 gel Substances 0.000 claims description 2
- 244000124853 Perilla frutescens Species 0.000 claims 1
- 238000000605 extraction Methods 0.000 abstract description 13
- 230000000694 effects Effects 0.000 abstract description 8
- 239000012535 impurity Substances 0.000 abstract description 3
- 231100000331 toxic Toxicity 0.000 abstract description 3
- 230000002588 toxic effect Effects 0.000 abstract description 3
- 230000009759 skin aging Effects 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 38
- 210000003491 skin Anatomy 0.000 description 30
- 230000000052 comparative effect Effects 0.000 description 11
- TXDUTHBFYKGSAH-SFHVURJKSA-N Evodiamine Chemical compound C1=CC=C2N(C)[C@@H]3C(NC=4C5=CC=CC=4)=C5CCN3C(=O)C2=C1 TXDUTHBFYKGSAH-SFHVURJKSA-N 0.000 description 8
- HMXRXBIGGYUEAX-SFHVURJKSA-N Evodiamine Natural products CN1[C@H]2N(CCc3[nH]c4ccccc4c23)C(=O)c5ccccc15 HMXRXBIGGYUEAX-SFHVURJKSA-N 0.000 description 8
- ACVGWSKVRYFWRP-UHFFFAOYSA-N Rutecarpine Chemical compound C1=CC=C2C(=O)N(CCC=3C4=CC=CC=C4NC=33)C3=NC2=C1 ACVGWSKVRYFWRP-UHFFFAOYSA-N 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 7
- 231100000430 skin reaction Toxicity 0.000 description 6
- 206010015150 Erythema Diseases 0.000 description 5
- 241000229722 Perilla <angiosperm> Species 0.000 description 5
- 231100000321 erythema Toxicity 0.000 description 5
- 239000004615 ingredient Substances 0.000 description 5
- 230000037394 skin elasticity Effects 0.000 description 5
- 239000000341 volatile oil Substances 0.000 description 5
- 206010030113 Oedema Diseases 0.000 description 4
- BCPAKGGXGLGKIO-UHFFFAOYSA-N Pseudorutaecarpin Natural products C1=CC=C2C(=O)N(CCC3=C4C5=CC=CC=C5N3)C4=NC2=C1 BCPAKGGXGLGKIO-UHFFFAOYSA-N 0.000 description 4
- 206010040914 Skin reaction Diseases 0.000 description 4
- 230000035483 skin reaction Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 230000032683 aging Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000011076 safety test Methods 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 2
- 241001093501 Rutaceae Species 0.000 description 2
- 239000002775 capsule Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 239000013558 reference substance Substances 0.000 description 2
- 230000037384 skin absorption Effects 0.000 description 2
- 231100000274 skin absorption Toxicity 0.000 description 2
- 210000000434 stratum corneum Anatomy 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- YYGNTYWPHWGJRM-UHFFFAOYSA-N (6E,10E,14E,18E)-2,6,10,15,19,23-hexamethyltetracosa-2,6,10,14,18,22-hexaene Chemical compound CC(C)=CCCC(C)=CCCC(C)=CCCC=C(C)CCC=C(C)CCC=C(C)C YYGNTYWPHWGJRM-UHFFFAOYSA-N 0.000 description 1
- 241000700198 Cavia Species 0.000 description 1
- VYZAHLCBVHPDDF-UHFFFAOYSA-N Dinitrochlorobenzene Chemical compound [O-][N+](=O)C1=CC=C(Cl)C([N+]([O-])=O)=C1 VYZAHLCBVHPDDF-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 206010051814 Eschar Diseases 0.000 description 1
- 241000628997 Flos Species 0.000 description 1
- 241001312741 Gekko swinhonis Species 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 206010067482 No adverse event Diseases 0.000 description 1
- 241000283973 Oryctolagus cuniculus Species 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- 206010040880 Skin irritation Diseases 0.000 description 1
- BHEOSNUKNHRBNM-UHFFFAOYSA-N Tetramethylsqualene Natural products CC(=C)C(C)CCC(=C)C(C)CCC(C)=CCCC=C(C)CCC(C)C(=C)CCC(C)C(C)=C BHEOSNUKNHRBNM-UHFFFAOYSA-N 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 231100000333 eschar Toxicity 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 230000004089 microcirculation Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000013642 negative control Substances 0.000 description 1
- 230000001575 pathological effect Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 230000001766 physiological effect Effects 0.000 description 1
- 239000013641 positive control Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 208000017520 skin disease Diseases 0.000 description 1
- 231100000475 skin irritation Toxicity 0.000 description 1
- 230000036556 skin irritation Effects 0.000 description 1
- 238000010181 skin prick test Methods 0.000 description 1
- 229940031439 squalene Drugs 0.000 description 1
- TUHBEKDERLKLEC-UHFFFAOYSA-N squalene Natural products CC(=CCCC(=CCCC(=CCCC=C(/C)CCC=C(/C)CC=C(C)C)C)C)C TUHBEKDERLKLEC-UHFFFAOYSA-N 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- SWGJCIMEBVHMTA-UHFFFAOYSA-K trisodium;6-oxido-4-sulfo-5-[(4-sulfonatonaphthalen-1-yl)diazenyl]naphthalene-2-sulfonate Chemical compound [Na+].[Na+].[Na+].C1=CC=C2C(N=NC3=C4C(=CC(=CC4=CC=C3O)S([O-])(=O)=O)S([O-])(=O)=O)=CC=C(S([O-])(=O)=O)C2=C1 SWGJCIMEBVHMTA-UHFFFAOYSA-K 0.000 description 1
- 230000024883 vasodilation Effects 0.000 description 1
- 238000003809 water extraction Methods 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
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
-
- 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
- A61Q19/08—Anti-ageing preparations
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0261—Solvent extraction of solids comprising vibrating mechanisms, e.g. mechanical, acoustical
- B01D11/0265—Applying ultrasound
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
-
- 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
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Chemical & Material Sciences (AREA)
- Acoustics & Sound (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Epidemiology (AREA)
- Biotechnology (AREA)
- Gerontology & Geriatric Medicine (AREA)
- Dermatology (AREA)
- Botany (AREA)
- Birds (AREA)
- Mechanical Engineering (AREA)
- Mycology (AREA)
- Microbiology (AREA)
- Cosmetics (AREA)
Abstract
The invention belongs to the technical field of extraction of evodia rutaecarpa, and discloses a preparation method of an evodia rutaecarpa extract, a composition containing the evodia rutaecarpa extract and application of the composition. The method comprises the following steps: pulverizing fructus evodiae fruit into powder, soaking in water, and extracting with steam distillation for 4 hr to obtain volatile extract and residue; soaking the residues in ethanol solution, carrying out ultrasonic treatment for 30-60 min at constant temperature, adding water into the ethanol solution, decompressing the ethanol solution at constant temperature until the residues are bubble, and continuously extracting the ethanol solution at the current pressure for 60min to obtain alkaloid extract solution; recovering ethanol from the alkaloid extract solution by rotary distillation to obtain alkaloid extract; dissolving and mixing the obtained alkaloid extract and volatile extract with 1, 3-propylene glycol to obtain fructus evodiae extract. The evodia rutaecarpa fruit extract not only has the effect of delaying skin aging, but also does not contain toxic impurities during extraction, and has stronger safety.
Description
Technical Field
The invention belongs to the technical field of extraction of evodia rutaecarpa, and particularly relates to a preparation method of an evodia rutaecarpa extract, a composition containing the evodia rutaecarpa extract and application of the composition.
Background
Evodiamine (Evodiamine) and rutaecarpine (Rutaecarpa) are mainly present in seeds or fruits of plants of Rutaceae (Rutaceae), such as fruits of Evodia Rutaecarpa, fruits of Gekko Swinhonis, fruits of Evodia Rutaecarpa, etc., and have high levels of Evodiamine and rutaecarpine. Pharmacological studies show that evodiamine and rutaecarpine have stronger physiological activity. Therefore, the evodiamine and the rutaecarpine are active ingredients with very high development value.
However, the application of the evodia rutaecarpa extract to cosmetics is rarely studied at present, and most of the evodia rutaecarpa extract is used as a medicament, so that the evodia rutaecarpa extract which can be directly applied to cosmetics is particularly important.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the primary aim of the invention is to provide a preparation method of an evodia rutaecarpa fruit extract, which can ensure that the extracted evodia rutaecarpa extract does not contain toxic impurities during extraction, and is safer and more convenient to apply.
The invention also aims to provide the evodia rutaecarpa extract prepared by the preparation method.
Still another object of the present invention is to provide the use of the aforementioned evodia rutaecarpa extract in cosmetics.
Still another object of the present invention is to provide a composition containing the aforementioned evodia rutaecarpa fruit extract.
It is a further object of the present invention to provide the use of the above composition in cosmetics.
The aim of the invention is achieved by the following technical scheme:
a preparation method of an evodia fruit extract comprises the following operation steps:
(1) Pulverizing fructus evodiae into powder, adding water with the mass of 13.5 times of that of the powder, soaking for 1h, and extracting for 4h by steam distillation to obtain volatile extract and residue;
(2) Soaking the residue obtained in the step (1) in ethanol solution, performing ultrasonic treatment at constant temperature for 30-60 min, adding water into the solution, decompressing the solution at constant temperature until bubbles emerge from the residue, and continuously extracting the solution at the current pressure for 60min to obtain alkaloid extract solution;
(3) Recovering ethanol from the alkaloid extract solution by rotary distillation to obtain alkaloid extract; dissolving and mixing the alkaloid extract and the volatile extract obtained in the step (1) with 1, 3-propanediol to obtain the evodia rutaecarpa extract.
The constant temperature in the step (2) refers to a temperature of 35 ℃.
The volume fraction of the ethanol solution in the step (2) is 60% -70%, and the feed liquid ratio of the residue to the ethanol solution is 1g:10mL. The ethanol solution is arranged in the mode of the volume fraction and the feed-liquid ratio, so that the extraction efficiency of the residues is higher.
And (3) the volume ratio of the added water to the ethanol solution in the step (2) is 2:1. The water is supplemented by the volume, so that the pressure is maintained to be reduced in the extraction process, and the extraction process is convenient to smoothly carry out.
An extract of fructus evodiae prepared by the above preparation method.
The evodia rutaecarpa extract can be applied to preparing cosmetics.
The composition containing the evodia rutaecarpa extract comprises the following components in parts by weight: 3-5 parts of evodia fruit extract and 1-2 parts of fructus forsythiae extract.
The weeping forsythiae capsule extract and the perilla leaf extract not only can further improve the anti-aging effect of the composition, but also can enhance the conditioning effect of the composition on skin and improve the application applicability of the composition.
The composition may further comprise 0.5 to 1 part by weight of perilla extract.
The use of the above composition for the preparation of a cosmetic product of the type comprising lotions, emulsions, essences, gels, creams and/or masks.
When the cosmetic is skin care lotion, the cosmetic is prepared from the following raw materials in percentage by weight: 2-4% of the composition, 6% of dipropylene glycol, 3% of trehalose, 1% of dipotassium glycyrrhizinate, 0.2% of preservative and the balance of deionized water;
when the cosmetic is an emulsion, the cosmetic is prepared from the following raw materials in percentage by weight: 4-6% of the composition, 2% of hydrolyzed sodium hyaluronate, 4% of 1, 3-butanediol, 0.32% of spiraea ulmaria, 3% of hyaluronic acid, 5% of carbomer, 2% of stearyl alcohol, 4% of avocado oil, 2% of polydimethylsiloxane, 2% of caprylic/capric triglyceride, 3% of myristyl myristate, 2% of squalane, 2% of PEG-8 stearate, 1.5% of stearyl alcohol, 0.3% of preservative and the balance of deionized water;
when the cosmetic is cream, the cosmetic is prepared from the following raw materials in percentage by weight: 4-8% of the composition, 2% of hydrolyzed sodium hyaluronate, 4% of 1, 3-butanediol, 0.32% of spiraea ulmaria, 3% of hyaluronic acid, 18-20% of carbomer, 2% of stearyl alcohol, 4% of avocado oil, 2% of polydimethylsiloxane, 2% of caprylic/capric triglyceride, 3% of myristyl myristate, 2% of squalane, 2% of PEG-8 stearate, 1.5% of stearyl alcohol, 0.5% of preservative and the balance of deionized water.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) According to the preparation method, the volatile oil component and the alkali component of the evodia rutaecarpa fruit are respectively extracted in a segmented extraction mode, so that the evodia rutaecarpa extract does not need to be additionally added with an absorption promoting agent when being applied to cosmetics, and meanwhile, the compatibility of the product is better, and the evodia rutaecarpa fruit extract can be enabled to exert the best effect of relieving aging.
(2) According to the preparation method, the volatile extract is obtained by adopting a steam distillation method, the residues are extracted by adopting an ultrasonic and decompression mode, the extraction rate is high, toxic impurities such as an organic extractant or a resolving agent and the like are prevented from being mixed in the evodia rutaecarpa extract, and therefore, the use safety of the evodia rutaecarpa extract extracted by the preparation method is higher.
(3) The evodia rutaecarpa extract applied to cosmetics prepared by the invention can induce vasodilation by regulating and controlling nitric oxide release, thereby improving blood microcirculation and further achieving the effect of delaying aging.
Detailed Description
The present invention will be described in further detail with reference to examples, but embodiments of the present invention are not limited thereto.
Example 1
The aim of the embodiment is to provide a preparation method of an evodia fruit extract, which comprises the following steps:
(1) Pulverizing fructus evodiae into powder, adding water with the mass of 13.5 times of that of the powder, soaking for 1h, and extracting for 4h by steam distillation to obtain volatile extract and residue;
(2) Soaking the residue obtained in the step (1) in 70% ethanol solution (the feed liquid ratio of the residue to the ethanol solution is 1g:10 mL), carrying out ultrasonic treatment at the constant temperature of 35 ℃ for 30-60 min, adding 35 ℃ of water into the solution, wherein the volume ratio of the added water to the ethanol solution is 2:1, decompressing the solution at the constant temperature of 35 ℃ until the residue is bubble-free, and continuously extracting the solution at the current pressure for 60min to obtain an alkaloid extract solution;
(3) Recovering ethanol from the alkaloid extract solution by rotary distillation to obtain alkaloid extract; it should be noted that before mixing, the ethanol content in the extract II can be detected to determine whether the extract meets the use standard, and the ethanol content can be further reduced by rotary distillation if the extract does not meet the use standard; dissolving and mixing the alkaloid extract and the volatile extract obtained in the step (1) with 1, 3-propanediol to obtain the evodia rutaecarpa extract.
Example 2
The aim of the embodiment is to provide a composition containing evodia rutaecarpa fruit extract, which comprises the following raw materials: 4g of evodia rutaecarpa fruit extract and 2g of fructus forsythiae extract.
Example 3
The aim of the embodiment is to provide a composition containing evodia rutaecarpa fruit extract, which comprises the following raw materials: 4g of evodia rutaecarpa fruit extract, 2g of fructus forsythiae extract and 1g of perilla extract.
Example 4
The aim of the embodiment is to provide a composition containing evodia rutaecarpa fruit extract, which comprises the following raw materials: 3g of evodia rutaecarpa fruit extract, 1g of weeping forsythiae capsule extract and 0.5g of perilla extract.
Example 5
The aim of the embodiment is to provide a composition containing evodia rutaecarpa fruit extract, which comprises the following raw materials: 5g of evodia rutaecarpa fruit extract, 2g of fructus forsythiae extract and 1g of perilla extract.
Example 6
The purpose of this example is to provide a skin care lotion, the specific ingredients are shown in table 1 below:
table 1 skin care moisture table containing compositions
| Composition of the components | Weight percent% |
| The above composition (prepared in example 3) | 2. 3 or 4 |
| Dipropylene glycol | 6 |
| Trehalose | 3 |
| Dipotassium glycyrrhizinate | 1 |
| Preservative agent | 0.2 |
| Deionized water | Allowance of |
Example 7
The purpose of this example is to provide an emulsion with the specific ingredients shown in table 2 below:
TABLE 2 emulsion ingredients Table of compositions
| Composition of the components | Weight percent% |
| The above composition (prepared in example 3) | 4. 5 or 6 |
| Hydrolysis of sodium hyaluronate | 2 |
| Sodium hyaluronate | 3 |
| 1, 3-butanediol | 4 |
| Flos ulmi pumilae | 0.32 |
| Carbomer (carbomer) | 5 |
| Stearyl alcohol | 2 |
| Avocado oil | 4 |
| Polydimethylsiloxane | 2 |
| Caprylic/capric triglyceride | 2 |
| Myristyl myristate | 3 |
| Squalane (Squalene) | 2 |
| PEG-8 stearate | 2 |
| Stearyl alcohol | 1.5 |
| Preservative agent | 0.3 |
| Deionized water | Allowance of |
Example 8
The purpose of this example is to provide a cream, the specific ingredients are shown in table 3 below:
TABLE 3 cream ingredients Table of compositions
Comparative example 1
The other steps were the same as in example 1 except that the volatile extract was not extracted in step (1), but the Evodia rutaecarpa fruit was directly powdered and then immersed in 70% ethanol solution by volume fraction to perform the operations of steps (2) and (3), and the obtained Evodia rutaecarpa fruit extract was used to prepare reference 1 with reference to example 6.
Comparative example 2
The Evodia rutaecarpa fruit extract was prepared by pulverizing Evodia rutaecarpa fruit, extracting with distilled water at a ratio of 1.5g/1mL to obtain Evodia rutaecarpa fruit extract, and preparing reference substance 2 with reference to example 6.
Comparative example 3
The evodia rutaecarpa extract extracted by the acid extraction method is specifically prepared by pulverizing evodia rutaecarpa, extracting the powder of evodia rutaecarpa with dilute hydrochloric acid at a ratio of 1.5g/1mL to obtain the evodia rutaecarpa extract, and preparing reference 3 by referring to example 6.
Effect example
1. Detection of evodia rutaecarpa fruit extract components
The Evodia rutaecarpa extract prepared in example 1 was sent for inspection, and the analysis results were shown in the following table:
TABLE 4 analysis results of the components
| Composition of the components | CAS# | EINECS# | Composition% |
| Evodia rutaecarpa fruit extract | 1174710-48-5 | - | 10.0-15.0 |
| 1, 3-propanediol | 504-63-2 | 207-997-3 | 85.0-90.0 |
Moreover, the sample to be examined is a yellow to reddish brown transparent liquid.
2. Safety test
Skin multiple irritation test: the healthy white rabbits without skin diseases can be female and male, the weight is 2.0-2.1 kg, and the shearing of the two sides of the spine is 3.0cm х 2.5.5 cm. The products prepared in example 2-example 8 and the controls 1-3 obtained in comparative examples 1-3 were directly applied to one side of the skin using 1.0g, respectively, and the other side was used as a control, once daily, continuously applied for 14d, and sheared as necessary. Skin reactions were recorded daily observations. And taking local skin after the test is finished for pathological histology.
Skin allergy test: three groups of tests were conducted on guinea pigs, namely a test substance group, a 2, 4-dinitrochlorobenzene positive control group and a negative control group, wherein samples used in the test substance group were the products prepared in examples 2 to 8 and the controls 1 to 3 in comparative examples 1 to 3. Local blocking coating (BT), after 2 weeks of induction, coating was continued for 6h, 24h and 48h after challenge contact, skin response was observed, and skin response scoring and sensitization intensity grading were performed.
The safety test results are specifically shown in the following table:
TABLE 5 safety test results
As can be seen from the above table, the extract of evodia rutaecarpa still contains a part of acid substances in the way of acid extraction, so that the extract has obvious stimulation to skin, and is not suitable for preparing cosmetics, so that in the subsequent human skin test, the reference substance 3 (namely the evodia rutaecarpa extract corresponding to comparative example 3) does not participate in the skin test.
3. Human skin test
The number of subjects was 41, 11 men and 30 women, the age distribution was 18 to 42 years, and the average age was 33.4 years. The results of the skin reaction were recorded in the classification standards of skin reaction in the "cosmetic safety evaluation procedure and method" GB7919-87 ", as shown in Table 6, using the product prepared in example 6 (the weight percentage of the composition in the raw material was 3%), the product prepared in example 7 (the weight percentage of the composition in the raw material was 5%), the product prepared in example 8 (the weight percentage of the composition in the raw material was 6%), the control 1 obtained in comparative example 1, and the control 2 obtained in comparative example 2, and the sample or the control was removed after 2 hours by the closed patch test method, and the skin reaction was observed in the patch tests for 0.5 hours, 24 hours, and 48 hours, respectively.
TABLE 6 human skin test results
Wherein, grade 0 indicates no erythema and no edema; grade 1 indicates barely visible erythema or edema; scale 2 indicates clear outline of visibly apparent erythema or skin doming; grade 3 represents moderate to severe erythema or edema bulge of about 1mm; scale 4 indicates a purple red erythema with eschar formation or edema bulge exceeding 1mm, a range extending.
Therefore, the evodia rutaecarpa extract, the composition and the cosmetics provided by the invention have no adverse reaction to the skin.
4. Skin absorbency test
The number of subjects was 41, 11 men and 30 women, the age distribution was 18 to 42 years, and the average age was 33.4 years. The following skin absorption test was conducted using the product prepared in example 6 (the weight percentage of the composition in the raw material was 3%), the product prepared in example 7 (the weight percentage of the composition in the raw material was 5%), the product prepared in example 8 (the weight percentage of the composition in the raw material was 6%), the control 1 obtained in comparative example 1, and the control 2 obtained in comparative example 2 as samples.
The test method comprises the following steps: the same position inside the same side arm of different subjects was divided into five test areas (the test area was not applied with any cosmetics within 1 month before the test), the diameter was 1cm, the cosmetics moistened with the sample were applied to the test area for 60s, and the unabsorbed cosmetics were removed after 60 s. The D-Squame disk (Cuderm, USA) was then attached to the test area and pressed for 30 seconds, removing the D-Squame disk. The absorption rate of the sample or control in the stratum corneum was measured by extracting the stratum corneum stuck on the D-square disc.
The absorption rate calculation mode is as follows: test evodiamine content (μg) 100%/evodiamine content in sample (μg)
The absorption results were as follows:
TABLE 7 skin absorption results
As is clear from the table above, the absorption rate of the skin care lotion prepared in example 6 is best because of the absence of volatile extract in the control 1, while the absorption effect of evodiamine in the skin care lotion prepared in example 6 is best, and the conventional water extraction method is adopted in the control 2, although the evodia rutaecarpa extract obtained by the method does not contain other substances having skin irritation effects, the volatile oil content in the volatile oil extract is low because the extraction efficiency is low, so that the absorption rate of the skin to the lotion is low, and the volatile oil, alkaloid extract and miscibility in the stepwise preparation of the evodia rutaecarpa provided by the invention have obvious advantages.
5. Examples 6 to 8 and Performance test on control
The number of subjects was 41, 11 men and 30 women, the age distribution was 18 to 42 years, and the average age was 33.4 years.
The same position on the inner side of the two arms of the subject is divided into 11 test areas (the test part is not coated with any cosmetics within 1 month before the test), and the test areas are respectively marked as a No. 1 test area, a No. 2 test area, a No. 3 test area, a No. 4 test area, a No. 5 test area, a No. 6 test area, a No. 7 test area, a No. 8 test area, a No. 9 test area, a No. 10 test area and a No. 11 test area, and the No. 1-11 test areas respectively correspond to products coated with the different compositions of the examples 6-8 in percentage by weight and the controls 1 and 2 corresponding to the comparative examples 1-2.
The smearing mode is as follows: the test is carried out by cleaning with clear water before each test for 30 days, and measuring after 20 min.
Skin moisture loss the skin moisture loss in the test area was measured using a VapoMeter moisture evaporation tester from Delfin, finland. The specific calculation mode is as follows: skin moisture loss rate= (skin moisture loss after use of sample-initial skin moisture loss)/initial skin moisture loss x 100%.
Skin elasticity change skin viscoelasticity of the test area was measured using a skin elasticity tester Cutometer MPA 580. The specific calculation mode is as follows: skin elasticity change rate = (skin viscoelasticity after use of the sample-initial skin viscoelasticity)/initial skin viscoelasticity x 100%.
The skin moisture loss and skin elasticity change after the use of the subjects were unified, and the results are shown in Table 8 below.
Table 8 cosmetic performance comparison
From the above table, it is apparent that the greater the content of the composition containing the evodia rutaecarpa extract in the above sample, the smaller the loss of skin moisture, and the better the skin elasticity, thereby demonstrating that the evodia rutaecarpa extract has a better effect of relieving aging. Moreover, compared with the control 1, the volatile extract has better penetration promoting effect, and simultaneously can lead the performance of the cosmetic to be better. As can be seen from comparison with control 2, when the Evodia rutaecarpa fruit extract contains a small amount of volatile oil, the effect of the extract for preparing cosmetics is poor due to the low extraction efficiency of other components.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (10)
1. A preparation method of an evodia fruit extract is characterized by comprising the following operation steps:
(1) Pulverizing fructus evodiae into powder, adding water with the mass of 13.5 times of that of the powder, soaking for 1h, and extracting for 4h by steam distillation to obtain volatile extract and residue;
(2) Soaking the residue obtained in the step (1) in ethanol solution, performing ultrasonic treatment at constant temperature for 30-60 min, adding water into the solution, decompressing the solution at constant temperature until bubbles emerge from the residue, and continuously extracting the solution at the current pressure for 60min to obtain alkaloid extract solution;
(3) Recovering ethanol from the alkaloid extract solution by rotary distillation to obtain alkaloid extract; dissolving and mixing the alkaloid extract and the volatile extract obtained in the step (1) with 1, 3-propanediol to obtain the evodia rutaecarpa extract.
2. The method for preparing the evodia fruit extract according to claim 1, which is characterized in that: the constant temperature in the step (2) refers to a temperature of 35 ℃.
3. The method for preparing the evodia fruit extract according to claim 1, which is characterized in that: the volume fraction of the ethanol solution in the step (2) is 60% -70%, and the feed liquid ratio of the residue to the ethanol solution is 1g:10mL.
4. The method for preparing the evodia fruit extract according to claim 1, which is characterized in that: and (3) the volume ratio of the added water to the ethanol solution in the step (2) is 2:1.
5. An extract of evodia rutaecarpa prepared by the preparation method of any one of claims 1 to 4.
6. The use of the evodia rutaecarpa extract according to claim 5 in the preparation of cosmetics.
7. A composition comprising the evodia fruit extract of claim 5, which is characterized in that: the composition comprises the following components in parts by weight: 3-5 parts of evodia fruit extract and 1-2 parts of fructus forsythiae extract.
8. The composition of claim 7, wherein: the composition also comprises 0.5 to 1 weight part of perilla extract.
9. Use of a composition according to claim 7 or 8 for the preparation of a cosmetic, characterized in that: the cosmetic types include lotions, creams, essences, gels, creams and/or masks.
10. The use according to claim 9, characterized in that: when the cosmetic is skin care lotion, the cosmetic is prepared from the following raw materials in percentage by weight: 2-4% of the composition, 6% of dipropylene glycol, 3% of trehalose, 1% of dipotassium glycyrrhizinate, 0.2% of preservative and the balance of deionized water;
when the cosmetic is an emulsion, the cosmetic is prepared from the following raw materials in percentage by weight: 4-6% of the composition, 2% of hydrolyzed sodium hyaluronate, 4% of 1, 3-butanediol, 0.32% of spiraea ulmaria, 3% of hyaluronic acid, 5% of carbomer, 2% of stearyl alcohol, 4% of avocado oil, 2% of polydimethylsiloxane, 2% of caprylic/capric triglyceride, 3% of myristyl myristate, 2% of squalane, 2% of PEG-8 stearate, 1.5% of stearyl alcohol, 0.3% of preservative and the balance of deionized water;
when the cosmetic is cream, the cosmetic is prepared from the following raw materials in percentage by weight: 4-8% of the composition, 2% of hydrolyzed sodium hyaluronate, 4% of 1, 3-butanediol, 0.32% of spiraea ulmaria, 3% of hyaluronic acid, 18-20% of carbomer, 2% of stearyl alcohol, 4% of avocado oil, 2% of polydimethylsiloxane, 2% of caprylic/capric triglyceride, 3% of myristyl myristate, 2% of squalane, 2% of PEG-8 stearate, 1.5% of stearyl alcohol, 0.5% of preservative and the balance of deionized water.
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