CN112842957A - Kyara perfume and preparation method thereof - Google Patents
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- CN112842957A CN112842957A CN202011564978.2A CN202011564978A CN112842957A CN 112842957 A CN112842957 A CN 112842957A CN 202011564978 A CN202011564978 A CN 202011564978A CN 112842957 A CN112842957 A CN 112842957A
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- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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- C11B9/00—Essential oils; Perfumes
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Abstract
The invention provides a Kyara perfume and a preparation method thereof, and the preparation method 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 according to a mass ratio of 2-3: 1: 50-80: 20-50: 0.5-1, stirring, standing, filtering, freezing and aging to obtain 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
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 contains other impurities besides the sesquiterpene compound and the 2- (2-phenethyl) chromone compound which are aroma components, and a method is urgently needed for improving the extraction of the aroma components and leading the agilawood volatile oil 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 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 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 (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 in a mass ratio of 2-3: 1: 50-80: 20-50: 0.5-1, stirring, standing, filtering, freezing and aging to obtain 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 percent.
Preferably, the aquilaria sinensis essential oil is volatile oil extracted from aquilaria sinensis produced by a new variety of planted aquilaria sinensis.
Preferably, 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 3-8 h.
Preferably, the supercritical extraction conditions are carbon dioxide as supercritical fluid, CO2The 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 powder is 60-80 mesh.
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 not only has elegant fragrance and rich variability, but also has the effects of central inhibitory sedation and hypnosis, the preparation method of Kyara is firstly carried out distillation extraction, the distilled Kyara powder is then subjected to supercritical extraction, cellulose in the Kyara is subjected to enzymolysis by cellulase in the preparation process, the gum in the Kyara is subjected to enzymolysis by pectinase, and the extraction components of aroma components of sesquiterpene compounds and 2- (2-phenylethyl) 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 pulverizer, pulverizing, and sieving with an 80-mesh sieve;
(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 (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: 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 ℃ and 30MPa for 30min to obtain linaloe oil A; extracting at 20 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: 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 to 100 ℃, distilling for 5 hours, and concentrating under reduced pressure to obtain a Kyara agilawood 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 lignum aquilariae resinatum, adding into a hopper of a grinder, grinding, 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, adding the mixture into the distillation extraction device, extracting by adopting a simultaneous distillation extraction method, heating to 90 ℃, distilling for 8 hours, and concentrating under reduced pressure to obtain a Kyara agilawood 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
The comparative example differs from example 2 in that in step (2), no cellulase or pectinase was added.
Comparative example 3
The difference between the comparative example and the example 3 is 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 differs 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 perfume prepared in the examples 1 to 4 with the eaglewood perfume prepared in the comparative examples 1 to 5, comparing 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 from the worst to the best, obtaining the average value of the points by 5 persons, and obtaining the evaluation result shown in the table 1:
the results show that the Kyara perfume prepared by the invention has the advantages of elegant perfume fragrance, and obvious effects of lasting fragrance, lasting fragrance and pleasure degree. In addition, the agalloch eaglewood perfume is not prepared according to the mass ratio of the agalloch eaglewood essential oil fraction 1, the agalloch eaglewood essential oil fraction 2, the dealdehydic ethanol, the deionized water and the essence in the comparative example 1, the cellulase and the pectinase are not added in the comparative example 2, the agalloch eaglewood perfume is not prepared according to the mass ratio of the invention in the comparative example 3, the supercritical extraction process parameters of the supercritical extraction are not adopted in the comparative example 4, the cellulase and the pectinase are not added in the comparative example 5 according to the mass ratio of the invention, the agalloch eaglewood perfume is not prepared according to the method in the.
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 Kyara perfume prepared in examples 1 to 4 and comparative examples 1 to 5 and the blank group were respectively put into bottles with spraying devices, and then the bottles were respectively sprayed into 10 thermostats containing mice, and the amount of the perfume was 5mg/Kg, 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
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 (10)
1. The preparation method of the Kyara perfume is characterized by comprising 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 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 (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 in a mass ratio of 2-3: 1: 50-80: 20-50: 0.5-1, stirring, standing, filtering, freezing and aging to obtain the Kyara perfume.
2. The aquilaria sinensis perfume of claim 1, wherein in the step (2), the aquilaria sinensis perfume comprises 80-120 parts by weight of aquilaria sinensis, 1 part by weight of cellulase and 1-2 parts by weight of pectinase.
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 3-8 h.
6. The method for preparing the aquilaria sinensis perfume of claim 1, wherein in the step (2), the aquilaria sinensis perfume is preparedThe supercritical extraction condition is that carbon dioxide is adopted as supercritical fluid, and CO is adopted2The 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 (1), the pulverizer is a universal pulverizer, and the pulverized product is sieved by a sieve of 60-80 meshes.
8. The method for preparing the machilus nandina perfume of claim 1, wherein in the step (2), the distilled extraction solvent is one or two of dichloromethane and diethyl ether.
9. The method for preparing the machi nanxiang perfume as claimed in 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 ℃.
10. A machi agilawood perfume characterized by being prepared by the method for preparing a machi agilawood perfume according to any one of claims 1 to 10.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116459192A (en) * | 2023-05-19 | 2023-07-21 | 广东兆禧健康产业投资有限公司 | Preparation method of aquilaria sinensis extract and toothpaste |
| CN116650387A (en) * | 2023-07-18 | 2023-08-29 | 广东兆禧健康产业投资有限公司 | Qilan agilawood shampoo for regulating micro-ecological balance of scalp and preparation method thereof |
| CN116763693A (en) * | 2023-06-12 | 2023-09-19 | 广东兆禧健康产业投资有限公司 | Perfume based on aquilaria sinensis extract and preparation method thereof |
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| CN116650387B (en) * | 2023-07-18 | 2024-01-23 | 广东兆禧健康产业投资有限公司 | Qilan agilawood shampoo for regulating micro-ecological balance of scalp and preparation method thereof |
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