CN108410582A - A kind of extracting method of Rosa Damascana - Google Patents
A kind of extracting method of Rosa Damascana Download PDFInfo
- Publication number
- CN108410582A CN108410582A CN201810354439.2A CN201810354439A CN108410582A CN 108410582 A CN108410582 A CN 108410582A CN 201810354439 A CN201810354439 A CN 201810354439A CN 108410582 A CN108410582 A CN 108410582A
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- CN
- China
- Prior art keywords
- rosa damascana
- water
- extracting method
- flower
- slurry
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Classifications
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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
-
- 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
Abstract
A kind of extracting method of Rosa Damascana, includes the following steps：(1) fresh rose flower valve is impregnated in water, is then beaten to obtain and spends slurry；(2) flower slurry is poured into 25~30 DEG C of water, complex enzyme zymohydrolysis is added, carbon tetrachloride is then added, stood 2~3h, obtain Rosa Damascana crude extract；(3) Rosa Damascana crude extract heating water bath is flowed back, then ice bath comes out the carbon tetrachloride liquid separation of lower layer to 8~10 DEG C, then in closed water bath heating distillation to get Rosa Damascana.The advantage of the invention is that equipment is simple, loss is small, and Rosa Damascana oil yield is high, and head perfume (or spice) recovery rate is also high in Rosa Damascana.
Description
Technical field
The present invention relates to a kind of extracting methods of aromatic oil, and in particular to a kind of extracting method of Rosa Damascana.
Background technology
Rose is one of world's famous flower, is referred to as " queen of flower ", and China is " flower of goddess " by honor in ancient times.Rose category
The rose family, is a kind of fallen leaves bush, the dense sharp thorn of stem, and color perfume (or spice) has both, and is a kind of to integrate ornamental, edible, medicinal
Economic flowers.Rosa Damascana is the hat of fresh flower oil, if having graceful, soft, fine and smooth, fragrant and sweet sweet, the fragrant Rose Essentielle to overflow,
Fragrance is dense, and with antibacterial, anti-oxidant, antiallergic sense, moisturizing, promotion cytothesis and other effects, to respiratory system, Digestive
There is preferable effect in terms of system, the circulatory system and reproductive system, there is suppression, decompression, sleeping, anti-impact in terms of mood
The effects that prominent, keeping tensions down and antidepression, it is expensive, and international market valence is of equal value with gold, is known as " essential oil queen ", " liquid
The good reputation of body gold " is most important, most common rare fragrance of a flower raw material in fragrance blending, is widely used in food, top grade
In cosmetics and tobacco, medicinal and food additives are can be used as.
Natural rose essential composition is sufficiently complex, and main component is monoterpenes compound, such as geraniol, β-citronellol, virtue
Camphor tree alcohol etc., rose oxide, sesquiterpene, sequiterpene oxygenatedchemicals also account for significant proportion, and other compounds have enanthaldehyde, ethyl alcohol, alkane
Hydrocarbon system row etc., and these chemical composition contents number and chemical composition on difference, cause the delicate of these rose fragrance
Difference.Generally speaking, geraniol, β-citronellol and nerol are to constitute the basis of Rose Essentielle with their esters, are
The main aroma ingredient of rose.Currently, the traditional extraction technique of Rosa Damascana mainly has steam distillation and organic solvent extraction
It follows the example of.Most domestic manufacturer is to use extraction by steam distillation Rosa Damascana, the method simple, cost with equipment
The features such as low, easy to operate, but since operation temperature is close to 100 DEG C, lead to low-boiling Rosa Damascana and water-soluble virtue
Fragrant ingredient such as 2 phenylethyl alcohol etc. is possible to incur loss or be destroyed, and causes Rosa Damascana yield relatively low, and due to high-temperature steam
Ill-effect, the Rosa Damascana color and luster extracted is deep, and with being charred taste.Organic solvent extractionprocess can simultaneously by low boiling point and
High boiling component extracts, and reduces the loss of fragrant oil component, what the fragrance of gained Rosa Damascana was spent closer to natural rose
Fragrance, and oil yield is higher than steam distillation, but extraction time is long, and the head perfume (or spice) of gained essential oil shows slightly insufficient, and is easy production
Raw dissolvent residual.In recent years, on the basis of traditional extraction technique, some new separation and purification technique such as supercritical fluid extract
Technology and molecular distillation technique is taken to be successfully applied to the extraction of Rosa Damascana.Such as 106281713 A of CN disclose a kind of rose
The extracting method of rare essential oil carries out continuous cycling extraction using supercritical carbon dioxide fluid, and extraction pressure is up to 15-25MPa,
Separating pressure is also reached for 8-10MPa.As it can be seen that supercritical CO2Abstraction technique equipment operation pressure is high, and more importantly opens
Close frequent, lack design experiences and effective design method, sealing element can not Reusability, and the country there is no this kind to set at present
Standby design, production standard, can not large-scale standardized production.
China rose, which has, spends that big, valve is thick, color is gorgeous, taste phase individual style, and the potentiality to be exploited of industry is huge, market prospects
It is wide, but at present, the Rosa Damascana of China's production is poor quality, it is difficult to spell to obtain one seat in the international market.
Therefore, oil yield can be improved and improve the extracting method of the head perfume of Rosa Damascana by being badly in need of exploration one kind.
Invention content
The purpose of the present invention is what is be achieved through the following technical solutions, a kind of extracting method of Rosa Damascana, including it is following
Step：
(1) fresh rose flower valve is impregnated in water, is then beaten to obtain and spends slurry；
(2) flower slurry obtained by step (1) is poured into 25~30 DEG C of water, complex enzyme zymohydrolysis is added, Rosa Damascana is made all to wave
It issues, carbon tetrachloride is then added, stand 2~3h, obtain Rosa Damascana crude extract；
(3) Rosa Damascana crude extract heating water bath obtained by step (2) is flowed back, so that Rosa Damascana is all dissolved in organic molten
In agent, then ice bath comes out the carbon tetrachloride liquid separation of lower layer to 8~10 DEG C, then in closed water bath heating distillation to get rose
Rare essential oil.
Further, in step (1), the mass ratio of the fresh rose flower valve and water (preferably purified water) is 1:2.0~2.5,
The soaking time is 90~120min.
Further, in step (2), the mass ratio of the flower slurry and 25~30 DEG C of water is 1：4~5, the compound enzyme dosage
It is 3 × 104U/g~5.1 × 104The mass ratio of U/g, the carbon tetrachloride and flower slurry is 1：2~2.5.
Further, the complex enzyme by cellulase and pectase enzyme according to 1:2 match.
Further, in step (3), heating water bath to 50~55 DEG C of reflux, closed 50~60 DEG C of heating water baths distillation 2.5~
3h。
The present invention is by under compound enzyme effect, Rosa Damascana all being digested, then passes through carbon tetrachloride extraction knot
Heshui bath is heated to reflux, and the ingredients such as Rosa Damascana and geraniol, citronellol is also effectively precipitated, Rosa Damascana yield obtains
It is greatly improved, and fragrance, naturally, in good taste, irritation is small, also significantly increases the quality of Rosa Damascana.
The advantage of the invention is that equipment is simple, loss is small, and Rosa Damascana oil yield is high, and head perfume (or spice) carries in Rosa Damascana
Take rate also high.
Specific implementation mode
Below with reference to the illustrative embodiments that the disclosure is more fully described.Although showing the exemplary of the disclosure
Embodiment, it being understood, however, that may be realized in various forms the disclosure without should be limited by embodiments set forth herein
System.It is to be able to be best understood from the disclosure on the contrary, providing these embodiments, and can be complete by the scope of the present disclosure
Whole is communicated to those skilled in the art.
Embodiment 1
(1) fresh rose flower valve is immersed in 100min in purified water, the mass ratio of fresh rose flower valve and purified water is 1:
2.2, it is then beaten to obtain and spends slurry；
(2) flower slurry obtained by step (1) is poured into 28 DEG C of water, is added 1.2 × 104U/g cellulases and 2.4 × 104U/g
Pectinase enzymatic hydrolysis, is then added carbon tetrachloride, and the carbon tetrachloride is 1 with the mass ratio that flower is starched：2.1,2.5h is stood, rose is obtained
Rare essential oil crude extract；
(3) the Rosa Damascana crude extract heating water bath obtained by step (2) is flowed back to 53 DEG C, then ice bath is to 9 DEG C, will under
The carbon tetrachloride liquid separation of layer comes out, and then distills 2.8h in closed 55 DEG C of heating water baths to get Rosa Damascana, oil yield is reachable
0.8137%.
Embodiment 2
(1) fresh rose flower valve is immersed in 110min in purified water, the mass ratio of fresh rose flower valve and purified water is 1:
2.3, it is then beaten to obtain and spends slurry；
(2) flower slurry obtained by step (1) is poured into 26 DEG C of water, is added 1.5 × 104U/g cellulases and 3 × 104U/g fruits
Glue enzyme digests, and carbon tetrachloride is then added, and the carbon tetrachloride is 1 with the mass ratio that flower is starched：2.2,2.6h is stood, rose is obtained
Essential oil crude extract；
(3) by the Rosa Damascana crude extract heating water bath obtained by step (2) to 52 DEG C of reflux, then ice bath, will to 8.5 DEG C
The carbon tetrachloride liquid separation of lower layer comes out, and then distills 2.6h in closed 56 DEG C of heating water baths to get Rosa Damascana, oil yield is reachable
0.7842%.
Embodiment 3
(1) fresh rose flower valve is immersed in 90min in purified water, the mass ratio of fresh rose flower valve and purified water is 1:2.5
Then it is beaten to obtain and spends slurry；
(2) flower slurry obtained by step (1) is poured into 30 DEG C of water, is added 1 × 104U/g cellulases and 2 × 104U/g pectin
Enzyme digests, and carbon tetrachloride is then added, and the carbon tetrachloride is 1 with the mass ratio that flower is starched：2,2h is stood, it is thick to obtain Rosa Damascana
Extract；
(3) by the Rosa Damascana crude extract heating water bath obtained by step (2) to 50 DEG C of reflux, then ice bath, will to 10 DEG C
The carbon tetrachloride liquid separation of lower layer comes out, and then distills 3h in closed 50 DEG C of heating water baths to get Rosa Damascana, oil yield is reachable
0.8945%.
Embodiment 3
(1) fresh rose flower valve is immersed in 120min in purified water, the mass ratio of fresh rose flower valve and purified water is 1:2,
Then it is beaten to obtain and spends slurry；
(2) flower slurry obtained by step (1) is poured into 25 DEG C of water, is added 1.7 × 104U/g cellulases and 3.4 × 104U/g
Pectinase enzymatic hydrolysis, is then added carbon tetrachloride, and the carbon tetrachloride is 1 with the mass ratio that flower is starched：2.5,3h is stood, rose is obtained
Essential oil crude extract；
(3) the Rosa Damascana crude extract heating water bath obtained by step (2) is flowed back to 55 DEG C, then ice bath is to 8 DEG C, will under
The carbon tetrachloride liquid separation of layer comes out, and then distills 2.5h in closed 60 DEG C of heating water baths to get Rosa Damascana, oil yield is reachable
0.8561%.
The active constituent content extracted using GC-MS gas chromatograph-mass spectrometers testing example 1 is shown in Table 1.
| Detection project | ISO9842：2003 | Head sesame oil recovery rate % |
| Citronellol | ≥20 | 51.08 |
| Geraniol | ≥15.0 | 30.71 |
| Nerol | ≥5.0 | 27.85 |
| Beta-phenyl ethyl alcohol | ≤3.5 | 0.62 |
| Heptadecane | ≤2.5 | 0.33 |
| Nonadecane | ≤15.0 | 1.97 |
| Heneicosane | ≤5.5 | 0.14 |
| Ethyl alcohol | ≤2.0 | 0.00 |
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, the change or replacement that can be readily occurred in,
It should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of the claim
Subject to enclosing.
Claims (6)
1. a kind of extracting method of Rosa Damascana, which is characterized in that include the following steps：
(1) fresh rose flower valve is impregnated in water, is then beaten to obtain and spends slurry；
(2) flower slurry obtained by step (1) is poured into 25~30 DEG C of water, complex enzyme zymohydrolysis is added, carbon tetrachloride is then added, stood
2~3h obtains Rosa Damascana crude extract；
(3) Rosa Damascana crude extract heating water bath obtained by step (2) is flowed back, then ice bath is to 8~10 DEG C, by the tetrachloro of lower layer
Change carbon liquid separation to come out, then in closed water bath heating distillation to get Rosa Damascana.
2. the extracting method of Rosa Damascana according to claim 1, which is characterized in that in step (1), the fresh rose flower
The mass ratio of valve and water is 1:2.0~2.5, the soaking time is 90~120min.
3. the extracting method of Rosa Damascana according to claim 2, which is characterized in that the water is purified water.
4. the extracting method of Rosa Damascana according to claim 1 or 2, which is characterized in that in step (2), the flower slurry
Mass ratio with 25~30 DEG C of water is 1：4~5, the compound enzyme dosage is 3 × 104U/g~5.1 × 104U/g, four chlorination
The mass ratio of carbon and flower slurry is 1：2~2.5.
5. the extracting method of Rosa Damascana according to claim 4, which is characterized in that the complex enzyme by cellulase and
Pectase enzyme is according to 1:2 match.
6. the extracting method of the Rosa Damascana according to one of claim 1,2 or 4, which is characterized in that in step (3), water
Bath is heated to 50~55 DEG C of reflux, and closed 50~60 DEG C of heating water baths distill 2.5~3h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810354439.2A CN108410582A (en) | 2018-04-19 | 2018-04-19 | A kind of extracting method of Rosa Damascana |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810354439.2A CN108410582A (en) | 2018-04-19 | 2018-04-19 | A kind of extracting method of Rosa Damascana |
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| Publication Number | Publication Date |
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| CN108410582A true CN108410582A (en) | 2018-08-17 |
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| CN201810354439.2A Pending CN108410582A (en) | 2018-04-19 | 2018-04-19 | A kind of extracting method of Rosa Damascana |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111671137A (en) * | 2020-05-14 | 2020-09-18 | 湖北中烟工业有限责任公司 | Rose extract spice, preparation method and cigarette not burning by heating |
| CN113930290A (en) * | 2021-11-29 | 2022-01-14 | 山东省食品发酵工业研究设计院 | High-quality rose essential oil efficient extraction method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102776072A (en) * | 2012-07-09 | 2012-11-14 | 广州市澳键丰泽生物科技有限公司 | Method for preparing rose essential oil |
| CN106367208A (en) * | 2016-11-25 | 2017-02-01 | 徐州黎明食品有限公司 | Separation and purification method of garlic essential oil |
| CN107557163A (en) * | 2017-10-10 | 2018-01-09 | 广东长利香精香料有限公司 | Lemongrass Rosa Damascana and preparation method thereof |
-
2018
- 2018-04-19 CN CN201810354439.2A patent/CN108410582A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102776072A (en) * | 2012-07-09 | 2012-11-14 | 广州市澳键丰泽生物科技有限公司 | Method for preparing rose essential oil |
| CN106367208A (en) * | 2016-11-25 | 2017-02-01 | 徐州黎明食品有限公司 | Separation and purification method of garlic essential oil |
| CN107557163A (en) * | 2017-10-10 | 2018-01-09 | 广东长利香精香料有限公司 | Lemongrass Rosa Damascana and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111671137A (en) * | 2020-05-14 | 2020-09-18 | 湖北中烟工业有限责任公司 | Rose extract spice, preparation method and cigarette not burning by heating |
| CN113930290A (en) * | 2021-11-29 | 2022-01-14 | 山东省食品发酵工业研究设计院 | High-quality rose essential oil efficient extraction method |
| CN113930290B (en) * | 2021-11-29 | 2024-04-16 | 山东省食品发酵工业研究设计院 | Efficient extraction method of high-quality rose essential oil |
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Application publication date: 20180817 |
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