CN112842957B - Kyara perfume and preparation method thereof - Google Patents

Kyara perfume and preparation method thereof Download PDF

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CN112842957B
CN112842957B CN202011564978.2A CN202011564978A CN112842957B CN 112842957 B CN112842957 B CN 112842957B CN 202011564978 A CN202011564978 A CN 202011564978A CN 112842957 B CN112842957 B CN 112842957B
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kyara
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oil
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aquilaria sinensis
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谌子旸
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HAINAN LIYAOTANG BIOTECHNOLOGY DEVELOPMENT CO LTD
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    • 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
    • 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
    • A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P25/00—Drugs for disorders of the nervous system
    • A61P25/20—Hypnotics; Sedatives
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q13/00—Formulations or additives for perfume preparations
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00—Essential oils; Perfumes
    • C11B9/02—Recovery or refining of essential oils from raw materials
    • C11B9/025—Recovery by solvent extraction
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00—Essential oils; Perfumes
    • C11B9/02—Recovery or refining of essential oils from raw materials
    • C11B9/027—Recovery of volatiles by distillation or stripping
    • 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
    • A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/91—Injection
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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Abstract

The invention provides a Kyara perfume and a preparation method thereof, and the perfume comprises the following steps: (1) Adding QINANGXIANGJIAO produced by radix aucklandiae into the hopper of a pulverizer, pulverizing, and sieving with a mesh sieve; (2) Mixing lignum Aquilariae Resinatum powder with cellulase and pectinase, and extracting by simultaneous distillation and extraction to obtain QINAOZHI oil fraction 1; (3) Performing supercritical extraction on the distilled QINAOJIAOXIANG powder, respectively preparing QINAOJIAOXIANG oil A and QINAOJIAOXIANG oil B under different conditions, and mixing the QINAOJIAOXIANG oil A and the QINAOJIAOXIANG oil B according to a mass ratio of 1:5, mixing to obtain a Kyara essential oil fraction 2; (4) Mixing fraction 1, fraction 2, dealdehydized ethanol, deionized water and essence in a mass ratio of 2-3: 1: 50-80: 20 to 50:0.5 to 1, stirring, standing, filtering, freezing and aging to prepare the Kyara perfume. The Kyara perfume prepared by the invention not only has elegant fragrance and rich variability, but also has the effects of central inhibitory sedation and hypnosis.

Description

Kyara perfume and preparation method thereof
Technical Field
The invention relates to the field of agilawood perfume, and in particular relates to a Kyara perfume and a preparation method thereof.
Background
Aquilaria is a resin-bearing wood of Aquilaria (Aquilaria) plants of the family Thymelaeaceae. The Kyara is the top and most precious variety of the aquilaria sinensis, also called Kyara, galnan, etc., the English is called Kanankoh, kyara, chi-Nan, qi-Nan, etc., because the Kyara has rich grease content compared with other aquilaria sinensis, and because the Kyara contains sesquiterpene compounds, the Kyara has the effects of tranquilizing and hypnotizing and invigorating stomach, the price is the most expensive in the market, and the national plant of the Kyara source of the aquilaria sinensis is aquilaria sinensis of Thymelaeaceae.
At present, the new species of aquilaria sinensis, including the name of thermal department No. 2 and others, can be injured to quickly produce agilawood, and after 1-3 years of agilawood formation, the produced agilawood has the quality of aquilaria sinensis, is rich in grease, has the chemical components consistent with that of aquilaria sinensis, has a shorter planting period than that of common aquilaria sinensis, has very high market acceptance and wide planting area, is collectively called as a variety of aquilaria sinensis, and is often called as aquilaria sinensis. The Kyara volatile oil produced by the new species of aquilaria sinensis can be used for preparing perfume and is an important raw material of perfume, which is a new resource and is abundant. However, the existing Kyara contain other impurities besides sesquiterpene compounds and 2- (2-phenethyl) chromone compounds which are aroma components, so that a method is urgently needed for improving the extraction of the aroma components and leading the volatile oil of the Kyara to be more widely applied.
Disclosure of Invention
In view of the above, the invention provides a Kyara perfume and a preparation method thereof, which solve the technical problems.
The technical scheme of the invention is realized as follows:
a preparation method of a Kyara agilawood perfume comprises the following steps:
(1) Crushing and sieving: adding QINANGXIANGJIAO produced by radix aucklandiae into the hopper of a pulverizer, pulverizing, and sieving with a mesh sieve;
(2) And (3) distillation: mixing the crushed and sieved agilawood powder in the step (1), cellulase and pectinase, adding the mixture into a distillation extraction device, extracting by adopting a simultaneous distillation extraction method, and concentrating under reduced pressure to obtain a Kyara agilawood essential oil fraction 1;
(3) And (3) extraction: performing supercritical extraction on the distilled Kyara powder in the step (2), and extracting for 10-60min at the temperature of 30-60 ℃ and under the pressure of 20-35MPa to prepare the linaloe oil A; extracting at 10-25 deg.C and 10-15MPa for 10-20min to obtain linaloe oil B; mixing linaloe oil A and linaloe oil B according to a mass ratio of 1:5, mixing to obtain a Kyara essential oil fraction 2;
(4) Mixing: and (3) mixing the fraction 1 of the aquilaria sinensis essential oil obtained in the step (2) and the step (3), the fraction 2 of the aquilaria sinensis essential oil, dealdehydized ethanol, deionized water and essence according to a mass ratio of 2-3: 1: 50-80: 20 to 50:0.5 to 1, stirring, standing, filtering, freezing and aging to prepare the Kyara perfume.
Preferably, the Chinese eaglewood vinegar beverage comprises, by weight, 80-120 parts of machilus nanensis, 1 part of cellulase and 1-2 parts of pectinase.
Preferably, the volume concentration of the dealdehydized ethanol is 90%.
Preferably, the Kyara essential oil is volatile oil extracted from Kyara which is produced from a new planted aquilaria sinensis new variety.
Preferably, in the step (2), the simultaneous distillation extraction method is to extract the machilus thunbergii powder by a simultaneous distillation extraction device, the heating temperature is 90-100 ℃, and the distillation time is 3-8h.
Preferably, the supercritical extraction conditions are carbon dioxide as supercritical fluid, CO 2 The flow rate is 12-20X 10-5kg/s, and ethanol is used as entrainer for extraction and separation.
Preferably, the pulverizer is a universal pulverizer, and the pulverized and sieved 60-80-mesh sieve.
Preferably, the distillation extraction solvent is one or two of dichloromethane and diethyl ether.
Preferably, the stirring time is 30-60min, the freezing time is 20-30min, and the freezing temperature is 0-5 ℃.
Preferably, the machilus nanensis agilawood perfume is prepared by a preparation method of the machilus nanensis agilawood perfume.
Compared with the prior art, the invention has the beneficial effects that:
the prepared Kyara perfume has elegant fragrance, is rich in changes, and also has the effects of central inhibitory sedation and hypnosis, distillation extraction is firstly carried out on the preparation method of the Kyara, then supercritical extraction is carried out on the distilled Kyara powder, cellulose in the Kyara is enzymolyzed by cellulase in the preparation process, gum in the Kyara is enzymolyzed by pectinase, and the extraction components of aroma components of sesquiterpene compounds and 2- (2-phenethyl) chromone compounds in the Kyara are improved.
Detailed Description
In order to better understand the technical content of the invention, specific examples are provided below to further illustrate the invention.
The experimental methods used in the examples of the present invention are all conventional methods unless otherwise specified.
The materials, reagents and the like used in the examples of the present invention can be obtained commercially without specific description.
Example 1
The Kyara perfume comprises the following steps:
(1) Adding 80 parts by weight of Kyara into a hopper of a grinder, grinding and sieving by a sieve of 80 meshes;
(2) Mixing the crushed and sieved agilawood powder in the step (1), 1 part by weight of cellulase and 1 part by weight of pectinase, adding the mixture into a distillation extraction device, extracting by adopting a simultaneous distillation extraction method, heating to 90 ℃, distilling for 5 hours, and concentrating under reduced pressure to obtain a Kyara essential oil fraction 1;
(3) Performing supercritical extraction on the distilled QINANGXIANG powder in the step (2), and extracting at 30 deg.C and 20MPa for 20min to obtain linaloe oil A; extracting at 15 deg.C under 10MPa for 15min to obtain linaloe oil B; mixing linaloe oil A and linaloe oil B according to a mass ratio of 1:5, mixing to obtain a Kyara essential oil fraction 2;
(4) And (4) mixing the fraction 1 of the aquilaria sinensis essential oil obtained in the step (2) and the step (3), the fraction 2 of the aquilaria sinensis essential oil, dealdehyded ethanol, deionized water and essence according to a mass ratio of 2:1:50:20:0.5, stirring, standing, filtering, freezing and aging to obtain the Kyara perfume.
Example 2
The Kyara perfume comprises the following steps:
(1) Adding 90 parts by weight of Kyara lignum aquilariae into a hopper of a pulverizer, pulverizing, and sieving with a 80-mesh sieve;
(2) Mixing the crushed and sieved agilawood powder in the step (1), 1 part by weight of cellulase and 2 parts by weight of pectinase, adding the mixture into a distillation extraction device, extracting by adopting a simultaneous distillation extraction method, heating to 90 ℃, distilling for 6 hours, and concentrating under reduced pressure to obtain a Kyara essential oil fraction 1;
(3) Performing supercritical extraction on the distilled QINANGXIANG powder in the step (2), and extracting at 50 deg.C and 30MPa for 30min to obtain linaloe oil A; extracting at 20 deg.C under 15MPa for 20min to obtain linaloe oil B; mixing linaloe oil A and linaloe oil B according to a mass ratio of 1:5, mixing to obtain a Kyara essential oil fraction 2;
(4) And (3) mixing the fraction 1 of the aquilaria sinensis essential oil obtained in the step (2) and the step (3), the fraction 2 of the aquilaria sinensis essential oil, dealdehydized ethanol, deionized water and essence according to a mass ratio of 2:1:70:30:0.5, stirring, standing, filtering, freezing and aging to obtain the Kyara perfume.
Example 3
The Kyara perfume comprises the following steps:
(1) 100 parts by weight of Kyara are taken and added into a hopper of a grinder, and the mixture is ground and sieved by a sieve of 80 meshes;
(2) Mixing the crushed and sieved agilawood powder in the step (1), 1 part by weight of cellulase and 2 parts by weight of pectinase, adding the mixture into a distillation extraction device, adding the mixture into the distillation extraction device, extracting by adopting a simultaneous distillation extraction method, heating at 100 ℃, distilling for 5 hours, and concentrating under reduced pressure to obtain a Machilus thunbergii essential oil fraction 1;
(3) Performing supercritical extraction on the distilled QINANGXIANG powder in the step (2), and extracting at 60 deg.C and 35MPa for 60min to obtain linaloe oil A; extracting at 25 deg.C and 15MPa for 10-20min to obtain linaloe oil B; mixing linaloe oil A and linaloe oil B according to a mass ratio of 1:5, mixing to obtain a Kyara essential oil fraction 2;
(5) And (3) mixing the fraction 1 of the aquilaria sinensis essential oil obtained in the step (2) and the step (3), the fraction 2 of the aquilaria sinensis essential oil, dealdehydized ethanol, deionized water and essence according to a mass ratio of 3:1:80:50:1, stirring, standing, filtering, freezing and aging to prepare the Kyara perfume.
Example 4
The Kyara perfume comprises the following steps:
(1) Taking 120 parts by weight of Kyara and adding into a hopper of a grinder, grinding and sieving by a sieve of 80 meshes;
(2) Mixing the crushed and sieved agilawood powder in the step (1), 1 part by weight of cellulase and 2 parts by weight of pectinase, adding the mixture into a distillation extraction device, adding the mixture into the distillation extraction device, extracting by adopting a simultaneous distillation extraction method, heating the mixture at 90 ℃, distilling the mixture for 8 hours, and concentrating the mixture under reduced pressure to obtain a chia aquilaria essential oil fraction 1;
(3) Performing supercritical extraction on the distilled QINANGXIANG powder in the step (2), and extracting at 60 deg.C and 30MPa for 50min to obtain linaloe oil A; extracting at 25 deg.C and 15MPa for 20min to obtain linaloe oil B; mixing linaloe oil A and linaloe oil B according to a mass ratio of 1:5, mixing to obtain a Kyara essential oil fraction 2;
(4) And (3) mixing the fraction 1 of the aquilaria sinensis essential oil obtained in the step (2) and the step (3), the fraction 2 of the aquilaria sinensis essential oil, dealdehydized ethanol, deionized water and essence according to a mass ratio of 2:1:50:30:1, stirring, standing, filtering, freezing and aging to prepare the Kyara perfume.
Comparative example 1
The difference between the comparative example and the example 2 is that in the step (4), the agilawood essential oil fraction 1, the agilawood essential oil fraction 2, the dealdehydized ethanol, the deionized water and the essence are mixed according to the mass ratio of 5:3:120:80:2 mixing to obtain the final product.
Comparative example 2
This comparative example is different from example 2 in that cellulase and pectinase were not added in step (2).
Comparative example 3
The comparative example is different from example 3 in that, in the step (3), the mass ratio of the linaloe oil A to the linaloe oil B is 1:10, and mixing.
Comparative example 4
The difference between the comparative example and the example 3 is that in the step (3), the distilled Kyara powder is subjected to supercritical extraction, and is extracted for 50min at 80 ℃ and 50MPa to prepare the linaloe oil A; extracting at 50 deg.C and 30MPa for 30min to obtain linaloe oil B; mixing linaloe oil A and linaloe oil B according to a mass ratio of 1:5 mixing to obtain QINAOJIAOXIANG oil fraction 2.
Comparative example 5
This comparative example is different from example 4 in that 5 parts by weight of cellulase and 8 parts by weight of pectinase were added in step (3).
Test example 1
Comparing the eaglewood perfumes prepared in the examples 1 to 4 with the eaglewood perfumes prepared in the comparative examples 1 to 5, the fragrance note (1 to 5 points), the fragrance lasting property (1 to 5 points) and the pleasure degree (1 to 5 points) of 1 to 5 points are divided into the worst to the best, the average value is obtained by the smoking of 5 persons in a small group, and the evaluation result is shown in the table 1:
Figure BDA0002860363270000051
Figure BDA0002860363270000061
the results show that the Kyara perfume prepared by the invention has the advantages of elegant perfume fragrance, lasting fragrance and obvious joyful effect. In addition, comparative example 1 does not prepare the aquilaria sinensis perfume according to the mass ratio of the aquilaria sinensis essential oil fraction 1, the aquilaria sinensis essential oil fraction 2, the dealdehydized ethanol, the deionized water and the essence of the invention, comparative example 2 does not add cellulase and pectinase, comparative example 3 does not prepare the aquilaria sinensis perfume according to the mass ratio of the invention, comparative example 4 does not add the supercritical extraction process parameters according to the supercritical extraction process of the invention, comparative example 5 does not add the cellulase and the pectinase according to the mass ratio of the invention, and the ratio of 1-5 does not prepare the aquilaria sinensis perfume according to the method of the invention, so that the fragrance note, fragrance persistence and pleasure degree effect of people are obviously reduced.
Test example 2
The test of the mouse center-calming inhibitory sedative and hypnotic effects comprises the following specific test processes:
taking 100 Kunming mice with the weight of 18-22 g/mouse without limitation; mice were randomly grouped into 10 groups of 10 mice each. The agalloch eaglewood perfume prepared in examples 1 to 4 and comparative examples 1 to 5 and a blank group were respectively filled in bottles with a spraying device, and then respectively sprayed into 10 thermostats filled with mice, and the amount of the perfume was 5mg/Kg of agalloch eaglewood, and the blank group was brand perfume purchased from the market. The number of mice falling asleep within 30min was observed. The results are shown in table 2:
TABLE 2 test results of the effect of QINANGXIANG perfume on mouse central inhibitory sedation and hypnosis
Figure BDA0002860363270000062
Figure BDA0002860363270000071
The above results show that the linaloe perfume prepared by the method has obvious central inhibitory sedative and hypnotic effects, and in addition, the linaloe perfume prepared by the method of the invention has sedative and hypnotic effects in comparative examples 1-5, but the effect is relatively poor.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (8)

1. The preparation method of the Kyara perfume is characterized by comprising the following steps:
(1) Crushing and sieving: adding QINANGXIANGJI produced by radix Inulae into hopper of universal pulverizer, pulverizing, and sieving with 60-80 mesh sieve;
(2) And (3) distillation: mixing the crushed and sieved agilawood powder in the step (1), cellulase and pectinase, adding the mixture into a distillation extraction device, extracting by adopting a simultaneous distillation extraction method, and concentrating under reduced pressure to obtain a Kyara agilawood essential oil fraction 1; the distillation extraction solvent is one or a combination of two of dichloromethane and diethyl ether;
(3) And (3) extraction: performing supercritical extraction on the distilled QINANGXIANG powder in the step (2), and extracting for 10-60min at 30-60 ℃ and 20-35MPa to obtain linaloe oil A; extracting at 10-25 deg.C and 10-15MPa for 10-20min to obtain linaloe oil B; mixing linaloe oil A and linaloe oil B according to a mass ratio of 1:5, mixing to obtain a Kyara essential oil fraction 2;
(4) Mixing: and (4) mixing the fraction 1 of the aquilaria sinensis essential oil obtained in the step (2) and the step (3), the fraction 2 of the aquilaria sinensis essential oil, dealdehyded ethanol, deionized water and essence according to a mass ratio of 2-3: 1: 50-80: 20 to 50:0.5 to 1, stirring, standing, filtering, freezing and aging to prepare the Kyara perfume.
2. The preparation method of the Kyara perfume according to claim 1, wherein in the step (2), 80-120 parts of Kyara, 1 part of cellulase and 1-2 parts of pectinase are calculated according to parts by weight.
3. The method for preparing the aquilaria sinensis perfume of claim 1, wherein in the step (4), the dealdehydized ethanol is 90% by volume.
4. The method for preparing aquilaria sinensis perfume according to claim 1, wherein the aquilaria sinensis essential oil is volatile oil extracted from aquilaria sinensis produced from a new species of planted aquilaria sinensis.
5. The preparation method of the aquilaria sinensis perfume of claim 1, wherein in the step (2), the simultaneous distillation extraction method is that the aquilaria sinensis powder is extracted by a simultaneous distillation extraction device, the heating temperature is 90-100 ℃, and the distillation time is 3-8h.
6. The preparation method of the Kyara perfume according to claim 1, wherein in the step (3), the supercritical extraction conditions are that carbon dioxide is used as a supercritical fluid, and CO is used as a supercritical fluid 2 The flow rate is 12-20X 10-5kg/s, and ethanol is used as entrainer for extraction and separation.
7. The preparation method of the aquilaria sinensis perfume of claim 1, wherein in the step (4), the stirring time is 30-60min, the freezing time is 20-30min, and the freezing temperature is 0-5 ℃.
8. The Kyara perfume is characterized by being prepared by the preparation method of the Kyara perfume of any one of claims 1 to 7.
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