CN105018235A - Method for rapid extracting of rose essential oil from fresh rose flower - Google Patents
Method for rapid extracting of rose essential oil from fresh rose flower Download PDFInfo
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- CN105018235A CN105018235A CN201510431512.8A CN201510431512A CN105018235A CN 105018235 A CN105018235 A CN 105018235A CN 201510431512 A CN201510431512 A CN 201510431512A CN 105018235 A CN105018235 A CN 105018235A
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Abstract
The present invention relates to a method for rapid extracting of rose essential oil from fresh rose flower. The method is as follows: rose petals and distilled water are simultaneously extracted and distilled, an extraction solvent is dichloromethane; after a certain time of distillation and extraction, a flask containing dichloromethane is taken down, added with anhydrous sodium sulfate for drying, then sealed overnight, and filtered, the filtrate is concentrated under a constant temperature water bath with Vigreux rectification column (Vigreux column); and an essential oil product is obtained by using nitrogen for purging to constant weight. Through combination of two steps comprising water vapor distillation and distillate solvent extraction into one step, the extraction efficiency is improved, and the use amount of the solvent is reduced. Meanwhile, volatile oil obtained by simultaneous distillation and extraction needs no complex pretreatment, GC-MS (gas chromatography - mass spectrometry) analysis can be directly performed, operational pollution is eliminated, extraction time is saved, the extracted product is strong in flavor, and mg / g level of volatile organic components can be concentrated for thousands of times from lipids or aqueous mediums.
Description
Technical field
The present invention relates to a kind of method extracting Flos Rosae Rugosae quintessence oil from fresh rose flower.
Background technology
Rose (Rosa rugosa Thunb.) is Rosaceae rose machaka, and various in style, fragrance is dense, is traditional famous flower of China.Rose is not only and views and admires the good plant material with soil conservation for people, and is the important source material of precious Chinese medicinal materials and perfume industry, foodstuffs industry.Flos Rosae Rugosae quintessence oil is the class volatile matter extracted from roseleaf, for the hat of ethereal oil of flower, there is the characteristics such as natural, nontoxic, graceful, soft, fragrance is pure, its value is several times of gold to tens times, have the laudatory title of " liquid golden ", be widely used in food, the cosmetics of super quality and tobacco, market demand is very huge.
Traditional extraction process mainly steam distillation and and the organic solvent extractionprocess of Flos Rosae Rugosae quintessence oil.Some new separation and purification technique such as molecular distillation technique and supercritical liquid extraction technique are then the extractions being just successfully applied to Flos Rosae Rugosae quintessence oil in recent years.In addition, in order to improve oil yield and the quality of Flos Rosae Rugosae quintessence oil further, multiple extraction method can be combined use.
With extraction by steam distillation Flos Rosae Rugosae quintessence oil, there is the advantages such as cost is low, equipment is simple, easy to operate, but because experimental temperature is close to 100 DEG C, thus lower boiling Flos Rosae Rugosae quintessence oil and water miscible fragrance ingredient likely incur loss as the stupid ethanol of 2-etc. or destroy, and cause the yield of rose oil and quality to decline.
Use organic solvent extraction Flos Rosae Rugosae quintessence oil, oil yield is higher than steam distillation, and can lower boiling and high boiling component be extracted simultaneously, thus can reduce the loss of perfume oil composition, and the fragrance of gained rose oil is closer to the fragrance of natural rose flower.But defect needs to consume a large amount of organic solvents, and have strict safety operation requirement, extraction time is longer, the head perfume (or spice) of gained essential oil shows slightly not enough, and easily produces dissolvent residual, has influence on the quality of essential oil thus limits its application.
Use supercritical CO
2extract Flos Rosae Rugosae quintessence oil and have that service temperature is low, selectivity good, percentage extraction is high, speed is fast, pollution-free, technique simple, can avoid the advantages such as oxidation, superior product quality, no solvent residue.There is due to Flos Rosae Rugosae quintessence oil the features such as molecular weight is lower, fat-soluble, lower boiling, be highly suitable in this way extracting Flos Rosae Rugosae quintessence oil from Rose.But extract in this way Flos Rosae Rugosae quintessence oil production cost high, there is no corresponding standard specifications to retrain, and the component of essential oil does not have the essential oil purity of extraction by steam distillation high.
At present, the many large-scale plants of extraction element of the relevant Flos Rosae Rugosae quintessence oil of report, are not suitable for applying at experiment condition both at home and abroad.And packaged unit extraction in laboratory conditions still adopts traditional steam distillation mostly.
Summary of the invention
The object of this invention is to provide a kind of method of rapid extraction Flos Rosae Rugosae quintessence oil from fresh rose flower, the present invention adopts SDE method to extract Flos Rosae Rugosae quintessence oil from fresh rose flower.
The method extracting Flos Rosae Rugosae quintessence oil from fresh rose flower provided by the present invention, comprises the steps:
(1) roseleaf and distilled water are put into flask, be linked into one end of SDE method; Design temperature heating is pressed with oil bath pan.
(2) flask of methylene dichloride is equipped with in the access of the distilling and extracting device the other end at the same time, heats with water bath with thermostatic control.
(3) after carrying out Simultaneous distillation-extraction certain hour, take off the flask that methylene dichloride is housed, add anhydrous sodium sulphate and carry out drying;
(4) then airtightly to spend the night, filter, concentrate with Vigreux rectifying column (Webster fractional column) under filtrate water bath with thermostatic control;
(5) again with nitrogen purging to constant weight, obtain essential oil product.
The Flos Rosae Rugosae quintessence oil obtained can be placed in after Brown Glass Brown glass bottles and jars only in refrigerator preservation.
In above-mentioned method, in step (1), the solid-liquid ratio of described roseleaf and distilled water is 1:3-6g/ml.Preferred 1:3 ~ 4, are preferably 1:4.Described oil bath temperature can be 115 ~ 130 DEG C, specifically can be 120 DEG C.
In above-mentioned method, in step (2), described methylene chloride volume can be 50 ~ 60ml, specifically can be 50ml; Described water bath with thermostatic control temperature should be 60 DEG C.
In above-mentioned method, in step (3), the described distillation extraction time can be 4 ~ 5h, specifically can be 4h.
In above-mentioned method, in step (4), described warm water bath temperature should be 60 DEG C; Described filtrate concentrates volume and can be 2-3ml, specifically can be 2ml.
The present invention take fresh rose flower as raw material, Simultaneous distillation is adopted to extract Flos Rosae Rugosae quintessence oil, compared with extracting with traditional wet distillation, what obtain due to Simultaneous distillation-extraction is volatile oil solution in organic solvent, volume is larger, convenient operation, avoid usual distillation method extract volatile oil time on wall adsorption losses and transfer trace volatile oil time operational difficulty; And solvent extraction two step of wet distillation and distillate unites two into one by this method, improves extraction efficiency, and decreases solvent load.And the volatile oil that Simultaneous distillation-extraction obtains does not need complicated pre-treatment, directly can carry out GC-MS (gas chromatography-mass spectrography) to analyze, eliminate operational pollution, save extraction time, the extract strong flavor obtained, can mg/g level volatile organic component from lipid or water quality medium concentrated thousands of times, be the effective ways of volatility in a kind of extracting and developing and enrichment sample, semi-volatility component.
Embodiment
Embodiment 1:
At distillation time 4h, under the condition that distillation temperature is 120 DEG C, Simultaneous distillation-extraction is carried out to roseleaf, according to mass volume ratio (w/v) that is colored and distillate, set solid-liquid ratio as 1:3,1:4,1:5,1:6 (g/ml) respectively, find that essential oil yield is respectively 5.00/10000ths, 5.96,3.89,2.21, when solid-liquid ratio is 1:4, the yield of Flos Rosae Rugosae quintessence oil is the highest, is 5.96/10000ths.
Embodiment 2:
Be under the condition of 1:4 at solid-liquid ratio, set distillation temperature as 115 DEG C, 120 DEG C, 125 DEG C, 130 DEG C respectively, Simultaneous distillation-extraction 4h, find that essential oil yield is respectively 5.56/10000ths, 6.66,6.66,6.71, namely when distillation temperature rises to 120 DEG C from 115 DEG C oil yield gather way very fast, after 120 DEG C, oil yield almost no longer increases, and distillation temperature 120 DEG C is little with the oil yield difference of 130 DEG C.
Embodiment 3:
Be 1:4 at solid-liquid ratio, under the condition that distillation temperature is 120 DEG C, set distillation time as 2h, 3h, 4h, 5h respectively, Simultaneous distillation-extraction is carried out to roseleaf, finds that essential oil yield is respectively 1.75/10000ths, 3.82,5.96,6.10, namely along with the prolongation of distillation time, Flos Rosae Rugosae quintessence oil oil yield significantly improves, after distillation time reaches 4 hours, essential oil yield increases slowly, and overall ascensional range presents first big after small trend.
Claims (8)
1. from fresh rose flower, extract a method for Flos Rosae Rugosae quintessence oil, it is characterized in that comprising the steps:
(1) roseleaf and distilled water are put into flask, be linked into one end of SDE method; Design temperature heating is pressed with oil bath pan;
(2) flask of methylene dichloride is equipped with in the access of the distilling and extracting device the other end at the same time, heats with water bath with thermostatic control;
(3) after carrying out Simultaneous distillation-extraction certain hour, take off the flask that methylene dichloride is housed, add anhydrous sodium sulphate and carry out drying;
(4) then airtightly to spend the night, filter, concentrate with Vigreux rectifying column under filtrate water bath with thermostatic control;
(5) again with nitrogen purging to constant weight, obtain essential oil product.
2. method according to claim 1, is characterized in that, in step (1), the solid-liquid ratio of roseleaf and distilled water is 1:3-6g/ml.
3. method according to claim 2, is characterized in that, the solid-liquid ratio of described roseleaf and distilled water is 1:4g/ml.
4. method according to claim 1, is characterized in that, in step (1), oil bath temperature can be 115 ~ 130 DEG C.
5. method according to claim 1, is characterized in that, in step (2), the volume of described methylene dichloride is 50 ~ 60ml; Described water bath with thermostatic control temperature is 60 DEG C.
6. method according to claim 5, is characterized in that, described methylene chloride volume is 50ml.
7. method according to claim 1, is characterized in that, in step (3), the described distillation extraction time is 4 ~ 5h.
8. method according to claim 1, is characterized in that, in step (4), described warm water bath temperature is 60 DEG C; It is 2-3ml that described filtrate is concentrated into volume.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106645478A (en) * | 2016-12-22 | 2017-05-10 | 淮阴师范学院 | Extracting and detecting method of volatile flavor components in rape seeds |
| CN107621513A (en) * | 2017-11-03 | 2018-01-23 | 厦门琥珀日化科技股份有限公司 | A kind of adulterated discrimination method of natural rose essential |
| CN107699347A (en) * | 2016-08-08 | 2018-02-16 | 庞锦霞 | A kind of method of Rosa Damascana extraction |
| CN108315098A (en) * | 2018-03-14 | 2018-07-24 | 海南大学 | A kind of Nymphaea caerulea method of extraction of essential oil and its application |
| CN111363626A (en) * | 2020-01-19 | 2020-07-03 | 宁波市妇女儿童医院 | Holographic rose essential oil and green preparation method thereof |
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| CN101851559A (en) * | 2010-06-11 | 2010-10-06 | 平阴县玫瑰研究所 | Method for extracting rose essential oil from rose dregs |
| CN102504952A (en) * | 2011-11-07 | 2012-06-20 | 云南烟草科学研究院 | Essential oil of Yunnan edible roses and application of essential oil to tobaccos |
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2015
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| CN101851559A (en) * | 2010-06-11 | 2010-10-06 | 平阴县玫瑰研究所 | Method for extracting rose essential oil from rose dregs |
| CN102504952A (en) * | 2011-11-07 | 2012-06-20 | 云南烟草科学研究院 | Essential oil of Yunnan edible roses and application of essential oil to tobaccos |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107699347A (en) * | 2016-08-08 | 2018-02-16 | 庞锦霞 | A kind of method of Rosa Damascana extraction |
| CN106645478A (en) * | 2016-12-22 | 2017-05-10 | 淮阴师范学院 | Extracting and detecting method of volatile flavor components in rape seeds |
| CN107621513A (en) * | 2017-11-03 | 2018-01-23 | 厦门琥珀日化科技股份有限公司 | A kind of adulterated discrimination method of natural rose essential |
| CN108315098A (en) * | 2018-03-14 | 2018-07-24 | 海南大学 | A kind of Nymphaea caerulea method of extraction of essential oil and its application |
| CN111363626A (en) * | 2020-01-19 | 2020-07-03 | 宁波市妇女儿童医院 | Holographic rose essential oil and green preparation method thereof |
| CN111363626B (en) * | 2020-01-19 | 2024-01-26 | 宁波市妇女儿童医院 | Holographic rose essential oil and green preparation method thereof |
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Application publication date: 20151104 |