CN112852548B - Perfume making process - Google Patents
Perfume making process Download PDFInfo
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- CN112852548B CN112852548B CN202011610073.4A CN202011610073A CN112852548B CN 112852548 B CN112852548 B CN 112852548B CN 202011610073 A CN202011610073 A CN 202011610073A CN 112852548 B CN112852548 B CN 112852548B
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- rose
- essential oil
- extract
- perfume
- molecular distillation
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- 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
-
- 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
- A61K8/68—Sphingolipids, e.g. ceramides, cerebrosides, gangliosides
-
- 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
- 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
- A61Q13/00—Formulations or additives for perfume preparations
-
- 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
- A61K2800/59—Mixtures
- A61K2800/591—Mixtures of compounds not provided for by any of the codes A61K2800/592 - A61K2800/596
Abstract
The invention discloses a manufacturing process of perfume, which belongs to the technical field of perfume, and comprises a rose essential oil extraction method, wherein rose essential oil is obtained by a pretreatment procedure, a leaching procedure, a purification and separation procedure and a molecular distillation procedure, and rose and 28-epibrassinolide are crushed together in the pretreatment procedure to obtain rose powder; in the leaching process, the rose powder is circularly extracted for 2-6 times by adopting an extracting agent to obtain an extracting solution, wherein the extracting agent is petroleum ether or diethyl ether. The invention improves the yield of the rose essential oil, the yield of the rose essential oil is increased by 0.008 percent, and the yield is improved by 18.39 percent.
Description
Technical Field
The invention belongs to the technical field of perfumes, and particularly relates to a manufacturing process of perfumes.
Background
The method for extracting the rose essential oil from the fresh rose flowers by using the steam distillation method is a commonly adopted rose essential oil production technology at present, but the oil yield of the method is only three parts per million. The oil yield can reach ten parts per million according to the supercritical carbon dioxide extraction of the fresh rose flowers in the test, which indicates that the water vapor distillation does not extract all the rose oil in the fresh rose flowers, but a large amount of rose essential oil is still not extracted. Therefore, a method for improving the yield of rose essential oil is still of great significance.
The perfume is a liquid mixed with essential oil, alcohol and auxiliary materials, and is used for enabling different parts of a human body to have lasting and pleasant smell. The alcohol containing perfume volatilizes relatively quickly, resulting in a relatively short fragrance retention time.
Disclosure of Invention
The invention aims to provide a method for extracting rose essential oil with high rose essential oil yield.
The technical scheme adopted by the invention for achieving the purpose is as follows:
a method for extracting rose essential oil, comprising: the rose is subjected to pretreatment, leaching, purification and separation and molecular distillation to obtain rose essential oil, and the rose and 28-epibrassinolide are crushed together in the pretreatment to obtain rose powder. After the rose and the 28-epibrassinolide are crushed together, the yield of the rose essential oil is improved, the utilization efficiency of the rose is improved, and the extraction effect is improved in the extraction process.
Preferably, in the pretreatment process, the rose is cleaned, drained and mixed with the 28-surface high brassinolide, and crushed by a crusher to obtain the rose powder. And the drained roses after cleaning are used for removing insoluble impurities on the surfaces, so that interference is avoided.
Preferably, the 28-epibrassinolide is added in an amount of 3-10wt% of rose.
Preferably, in the leaching process, mixing flos Rosae Rugosae powder with extractant, stirring for 1 time every 10-30min, leaching at 20-40deg.C for 2-5 hr, and filtering to obtain filtrate; and (3) circulating the leaching step for 2-6 times, and mixing the filtrates to obtain the rose extract. The essential oil of the rose is extracted into the solvent by full contact of the extractant with the rose powder.
Preferably, the extractant is petroleum ether or diethyl ether.
Preferably, the extractant is added in an amount of 2-5 times the mass fraction of the rose powder.
Preferably, in the purification and separation process, the extract is filtered and then concentrated in vacuum to obtain rose extract, and the rose extract is dewaxed by ethanol and then de-ethanol to obtain rose oil. The rose extract contains a considerable amount of vegetable wax, pigment, etc., and is removed by dewaxing with ethanol.
More preferably, the addition amount of the absolute ethyl alcohol is 3-5 times of the mass fraction of the rose extract.
More preferably, in the purification and separation process, the rose extract is filtered and then subjected to vacuum concentration by a rotary evaporator to obtain rose extract, wherein the temperature is 40-60 ℃, the rotating speed of a rotary bottle is 20-60 r/min, and the vacuum degree is minus 0.09 to minus 0.10MPa; mixing flos Rosae Rugosae extract with absolute ethanol, standing for 2-6 hr, filtering, and dewaxing; repeating dewaxing step for 2-3 times, removing ethanol from the dewaxed solution in a rotary evaporator, and separating to obtain the rose essential oil.
Preferably, in the molecular distillation process, a molecular distillation instrument is used for distilling the rose extract to obtain the rose essential oil.
Preferably, in the molecular distillation step, the distillation temperature is 100 to 200 ℃.
Preferably, in the molecular distillation process, the molecular distillation speed is 120-250r/min.
Preferably, in the molecular distillation step, the molecular distillation dropping speed is 1-5mL/min.
The invention discloses application of 28-epibrassinolide in improving the extraction effect of rose essential oil.
The invention aims to provide a manufacturing process of perfume with high rose essential oil yield and good durability.
The technical scheme adopted by the invention for achieving the purpose is as follows:
a process for preparing perfume, comprising: mixing flos Rosae Rugosae essential oil, bergamot oil, bay leaf oil, sweet orange oil, moschus tincture, and ethanol to obtain flos Rosae Rugosae perfume.
Preferably, the addition amount of the rose essential oil is 3-6wt% of the alcohol.
Preferably, the oil of bergamot is added in an amount of 0.05-0.2wt% of the alcohol.
Preferably, the amount of geranium oil added is 0.1-0.4wt% of alcohol.
Preferably, the sweet orange oil is added in an amount of 0.1-0.4wt% of alcohol.
Preferably, the musk tincture is added in an amount of 1-3wt% of alcohol.
Preferably, functional additives such as gamma-oryzanol and linseed lignan can be added in the manufacturing process of the perfume. The gamma-oryzanol and the linseed lignan act together with the rose essential oil and other components in the perfume, so that the rapid escape of the rose essential oil is prevented, and the durability of the perfume is improved.
More preferably, the gamma oryzanol is added in an amount of 0.1 to 0.5wt% of alcohol.
More preferably, the amount of flaxseed lignans added is 0.2-0.8wt% of alcohol.
The invention adopts the 28-epibrassinolide and the rose to be crushed together in the pretreatment procedure of the rose and then extracts the essential oil of the rose, so the invention has the following beneficial effects: the yield of the rose essential oil is improved, the yield of the rose essential oil is increased by 0.008%, and the yield is improved by 18.39%. The invention further adds gamma-oryzanol and linseed lignan in the process of preparing perfume, thus improving the durability of the perfume. Therefore, the invention is a manufacturing process of the perfume with high rose essential oil yield and good durability.
Drawings
FIG. 1 is a graph of rose essential oil yield;
fig. 2 is a graph of the permanence of rose scent.
Detailed Description
The technical scheme of the invention is further described in detail below with reference to the specific embodiments and the attached drawings:
example 1:
a process for preparing perfume,
pretreatment procedure: cleaning and draining the rose, mixing the cleaned rose with 28-surface high brassinolide, and crushing the mixture by a crusher to obtain rose powder. The addition amount of 28-epibrassinolide is 4wt% of rose.
Leaching procedure: mixing flos Rosae Rugosae powder with extractant, stirring for 1 time every 20min, leaching at 25deg.C for 3 hr, and filtering to obtain filtrate; and (3) circulating the leaching step for 5 times, and mixing the filtrates to obtain the rose extract. The extractant is petroleum ether, and the addition of the extractant is 3 times of the mass fraction of the rose powder.
Purification and separation procedures: filtering the rose extract, and vacuum concentrating by a rotary evaporator to obtain rose extract, wherein the temperature is 50 ℃, the rotating speed of a rotary bottle is 50 revolutions per minute, and the vacuum degree is minus 0.09MPa; mixing the rose extract with absolute ethyl alcohol, standing for 3 hours, filtering and dewaxing; repeating dewaxing step for 2 times, removing ethanol from the dewaxed solution in a rotary evaporator, and separating to obtain the rose essential oil. The addition amount of the absolute ethyl alcohol is 3 times of the mass fraction of the rose extract.
Molecular distillation process: and distilling the rose extract by using a molecular distillation instrument to obtain the rose essential oil. The molecular distillation temperature is 160 ℃; the molecular distillation rotating speed is 200r/min; the molecular distillation dropping speed was 1.5mL/min.
And (3) perfume preparation: mixing flos Rosae Rugosae essential oil, bergamot oil, bay leaf oil, sweet orange oil, moschus tincture, and ethanol to obtain flos Rosae Rugosae perfume. The addition amount of the rose essential oil is 5wt% of the alcohol, the addition amount of the bergamot oil is 0.1wt% of the alcohol, the addition amount of the geranium oil is 0.2wt% of the alcohol, the addition amount of the sweet orange oil is 0.2wt% of the alcohol, and the addition amount of the musk tincture is 2wt% of the alcohol.
Example 2:
a process for preparing perfume,
pretreatment procedure: cleaning and draining the rose, mixing the cleaned rose with 28-surface high brassinolide, and crushing the mixture by a crusher to obtain rose powder. The addition amount of 28-epibrassinolide is 8wt% of rose.
Leaching procedure: mixing flos Rosae Rugosae powder with extractant, stirring for 1 time every 20min, leaching at 25deg.C for 3 hr, and filtering to obtain filtrate; and (3) circulating the leaching step for 5 times, and mixing the filtrates to obtain the rose extract. The extractant is petroleum ether, and the addition of the extractant is 3 times of the mass fraction of the rose powder.
Purification and separation procedures: filtering the rose extract, and vacuum concentrating by a rotary evaporator to obtain rose extract, wherein the temperature is 50 ℃, the rotating speed of a rotary bottle is 50 revolutions per minute, and the vacuum degree is minus 0.09MPa; mixing the rose extract with absolute ethyl alcohol, standing for 3 hours, filtering and dewaxing; repeating dewaxing step for 2 times, removing ethanol from the dewaxed solution in a rotary evaporator, and separating to obtain the rose essential oil. The addition amount of the absolute ethyl alcohol is 3 times of the mass fraction of the rose extract.
Molecular distillation process: and distilling the rose extract by using a molecular distillation instrument to obtain the rose essential oil. The molecular distillation temperature is 160 ℃; the molecular distillation rotating speed is 200r/min; the molecular distillation dropping speed was 1.5mL/min.
And (3) perfume preparation: mixing flos Rosae Rugosae essential oil, bergamot oil, bay leaf oil, sweet orange oil, moschus tincture, and ethanol to obtain flos Rosae Rugosae perfume. The addition amount of the rose essential oil is 5wt% of the alcohol, the addition amount of the bergamot oil is 0.1wt% of the alcohol, the addition amount of the geranium oil is 0.2wt% of the alcohol, the addition amount of the sweet orange oil is 0.2wt% of the alcohol, and the addition amount of the musk tincture is 2wt% of the alcohol.
Example 3:
a process for preparing perfume,
pretreatment procedure: cleaning and draining the rose, mixing the cleaned rose with 28-surface high brassinolide, and crushing the mixture by a crusher to obtain rose powder. The addition amount of 28-epibrassinolide is 8wt% of rose.
Leaching procedure: mixing flos Rosae Rugosae powder with extractant, stirring for 1 time every 20min, leaching at 25deg.C for 3 hr, and filtering to obtain filtrate; and (3) circulating the leaching step for 5 times, and mixing the filtrates to obtain the rose extract. The extractant is petroleum ether, and the addition of the extractant is 3 times of the mass fraction of the rose powder.
Purification and separation procedures: filtering the rose extract, and vacuum concentrating by a rotary evaporator to obtain rose extract, wherein the temperature is 50 ℃, the rotating speed of a rotary bottle is 50 revolutions per minute, and the vacuum degree is minus 0.09MPa; mixing the rose extract with absolute ethyl alcohol, standing for 3 hours, filtering and dewaxing; repeating dewaxing step for 2 times, removing ethanol from the dewaxed solution in a rotary evaporator, and separating to obtain the rose essential oil. The addition amount of the absolute ethyl alcohol is 3 times of the mass fraction of the rose extract.
Molecular distillation process: and distilling the rose extract by using a molecular distillation instrument to obtain the rose essential oil. The molecular distillation temperature is 160 ℃; the molecular distillation rotating speed is 200r/min; the molecular distillation dropping speed was 1.5mL/min.
And (3) perfume preparation: mixing flos Rosae Rugosae essential oil, bergamot oil, bay leaf oil, sweet orange oil, moschus tincture, alcohol and functional additive to obtain flos Rosae Rugosae perfume. The rose essential oil is added in an amount of 5wt% of alcohol, the bergamot oil is added in an amount of 0.1wt% of alcohol, the geranium oil is added in an amount of 0.2wt% of alcohol, the sweet orange oil is added in an amount of 0.2wt% of alcohol, the musk tincture is added in an amount of 2wt% of alcohol, the functional additive is gamma-oryzanol and linseed lignan, the gamma-oryzanol is added in an amount of 0.2wt% of alcohol, and the linseed lignan is added in an amount of 0.3wt% of alcohol.
Example 4:
a process for preparing perfume,
pretreatment procedure: cleaning and draining the rose, mixing the cleaned rose with 28-surface high brassinolide, and crushing the mixture by a crusher to obtain rose powder. The addition amount of 28-epibrassinolide is 8wt% of rose.
Leaching procedure: mixing flos Rosae Rugosae powder with extractant, stirring for 1 time every 20min, leaching at 25deg.C for 3 hr, and filtering to obtain filtrate; and (3) circulating the leaching step for 5 times, and mixing the filtrates to obtain the rose extract. The extractant is petroleum ether, and the addition of the extractant is 3 times of the mass fraction of the rose powder.
Purification and separation procedures: filtering the rose extract, and vacuum concentrating by a rotary evaporator to obtain rose extract, wherein the temperature is 50 ℃, the rotating speed of a rotary bottle is 50 revolutions per minute, and the vacuum degree is minus 0.09MPa; mixing the rose extract with absolute ethyl alcohol, standing for 3 hours, filtering and dewaxing; repeating dewaxing step for 2 times, removing ethanol from the dewaxed solution in a rotary evaporator, and separating to obtain the rose essential oil. The addition amount of the absolute ethyl alcohol is 3 times of the mass fraction of the rose extract.
Molecular distillation process: and distilling the rose extract by using a molecular distillation instrument to obtain the rose essential oil. The molecular distillation temperature is 160 ℃; the molecular distillation rotating speed is 200r/min; the molecular distillation dropping speed was 1.5mL/min.
And (3) perfume preparation: mixing flos Rosae Rugosae essential oil, bergamot oil, bay leaf oil, sweet orange oil, moschus tincture, alcohol and functional additive to obtain flos Rosae Rugosae perfume. The rose essential oil is added in an amount of 5wt% of alcohol, the bergamot oil is added in an amount of 0.1wt% of alcohol, the geranium oil is added in an amount of 0.2wt% of alcohol, the sweet orange oil is added in an amount of 0.2wt% of alcohol, the musk tincture is added in an amount of 2wt% of alcohol, the functional additive is gamma-oryzanol and linseed lignan, the gamma-oryzanol is added in an amount of 0.4wt% of alcohol, and the linseed lignan is added in an amount of 0.6wt% of alcohol.
Comparative example 1:
this comparative example differs from example 2 only in that 28-epibrassinolide was not added in the pretreatment step.
Comparative example 2:
this comparative example differs from example 4 only in that no linseed lignan was added in the perfume preparation.
Comparative example 3:
this comparative example differs from example 4 only in that no gamma oryzanol was added in the perfume preparation.
Test example 1:
1. rose essential oil yield test
The test samples are the rose essential oils obtained in each example and comparative example.
Rose essential oil yield = rose essential oil yield/rose mass x 100%
The results of the rose essential oil yield test are shown in fig. 1, wherein the rose essential oil yield in example 2 is the highest, the rose essential oil yield is 0.0515%, the rose essential oil yield in example 1 is 0.0486%, the rose essential oil yield in comparative example 1 is 0.0435%, and the addition of 28-epibrassinolide in the pretreatment process improves the rose essential oil yield compared with comparative example 1, the rose essential oil yield is increased by 0.008%, and the rose essential oil yield is improved by 18.39% compared with comparative example 1.
2. Perfume durability test
The test samples were rose perfume obtained in each example and comparative example.
The test samples were sprayed on the ears, and after 30min and 60min of exercise, and after 3 and 6h of daily activities, the fragrance concentration was measured with a fragrance detector.
The perfume durability test results are shown in fig. 2, and initially, the perfume concentrations of each example and the comparative example are about 200ppb, the perfume concentrations obtained in different examples and comparative examples are no longer consistent with the lapse of time, the durability is different, after 30 minutes of movement, examples 3-4 are good in perfume durability compared with example 2, which indicates that the use of gamma-oryzanol and linseed lignan together improves the perfume durability, and example 4 is good in perfume durability compared with comparative examples 2-3, which indicates that the effect of the use of gamma-oryzanol and linseed lignan together has an effect on perfume durability better than that of gamma-oryzanol or linseed lignan. The co-use of gamma-oryzanol and linseed lignan also proved to have a superior effect at 60min of exercise. After normal activity for 3 hours, examples 3-4 have better perfume durability than example 2, indicating that the co-use of gamma-oryzanol and linseed lignan improves perfume durability, and example 4 has better perfume durability than comparative examples 2-3, indicating that the co-use of gamma-oryzanol and linseed lignan has better effect on perfume durability than gamma-oryzanol or linseed lignan. After 6h of exercise, the co-use of gamma-oryzanol and linseed lignan also proved to have a superior effect.
The above embodiments are merely for illustrating the present invention and not for limiting the same, and various changes and modifications may be made by one of ordinary skill in the art without departing from the spirit and scope of the invention. Therefore, all equivalent technical solutions are also within the scope of the present invention, which is defined by the claims.
Claims (3)
1. A method for extracting rose essential oil, comprising: the method comprises the steps of performing pretreatment, leaching, purification and separation, and molecular distillation on roses to obtain rose essential oil, wherein the roses and 28-epibrassinolide are crushed together in the pretreatment to obtain rose powder;
the addition amount of the 28-epibrassinolide is 3-10wt% of rose;
in the leaching process, extracting agent is adopted to circularly extract the rose powder for 2-6 times to obtain extract, and the extracting agent is petroleum ether or diethyl ether; in the purification and separation process, filtering the extract, and concentrating in vacuum to obtain rose extract, dewaxing the rose extract by ethanol, and removing ethanol to obtain rose oil; in the molecular distillation process, the distillation temperature is 100-200 ℃; the addition of the extractant is 2-5 times of the mass fraction of the rose powder.
2. The method for extracting rose essential oil according to claim 1, which is characterized in that: in the molecular distillation process, the dropping speed of molecular distillation is 1-5mL/min.
Use of 28-apparent brassinolide in improving extraction effect of oleum Rosae Rugosae.
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| CN202011610073.4A CN112852548B (en) | 2020-12-29 | 2020-12-29 | Perfume making process |
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| CN202011610073.4A CN112852548B (en) | 2020-12-29 | 2020-12-29 | Perfume making process |
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| CN101851559B (en) * | 2010-06-11 | 2012-07-11 | 平阴县玫瑰研究所 | Method for extracting rose essential oil from rose dregs |
| CN102031199A (en) * | 2010-06-11 | 2011-04-27 | 平阴县玫瑰研究所 | Method for extracting rose essential oil from fresh rose flowers |
| CN105769622A (en) * | 2016-04-22 | 2016-07-20 | 广西壮族自治区林业科学研究院 | Essence oil for dry skin care and preparation method thereof |
| CN111226992A (en) * | 2020-04-14 | 2020-06-05 | 江西鑫邦科技有限责任公司 | Method for improving plant absorption and utilization rate by using composition containing brassinolide compound and plant essential oil |
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Effective date of registration: 20230810 Address after: No. 2 Qixi Road, Shiqian Village, Huadong Town, Huadu District, Guangzhou City, Guangdong Province, 510800 Patentee after: Guangzhou qixidi Biotechnology Co.,Ltd. Address before: 315000 No. 581, East Section of Huancheng North Road, Jiangbei District, Ningbo City, Zhejiang Province Patentee before: NINGBO JIANGBEI YIRENBAO TRADE CO.,LTD. |