NL2030871B1 - Method for extracting rose essential - Google Patents

Method for extracting rose essential Download PDF

Info

Publication number
NL2030871B1
NL2030871B1 NL2030871A NL2030871A NL2030871B1 NL 2030871 B1 NL2030871 B1 NL 2030871B1 NL 2030871 A NL2030871 A NL 2030871A NL 2030871 A NL2030871 A NL 2030871A NL 2030871 B1 NL2030871 B1 NL 2030871B1
Authority
NL
Netherlands
Prior art keywords
essential oil
rose essential
rose
water
carbon tetrachloride
Prior art date
Application number
NL2030871A
Other languages
Dutch (nl)
Inventor
Zhong Shuxian
Pan Xiaoou
Liu Weidong
Xu Yan
Chen Jianrong
Original Assignee
Univ Zhejiang Normal
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Univ Zhejiang Normal filed Critical Univ Zhejiang Normal
Priority to NL2030871A priority Critical patent/NL2030871B1/en
Application granted granted Critical
Publication of NL2030871B1 publication Critical patent/NL2030871B1/en

Links

Classifications

    • 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

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Fats And Perfumes (AREA)

Abstract

The present disclosure provides a method for extracting rose essential oil. The method comprises the following steps: (1) soaking fresh rose petals in water, and then pulping to obtain flower pulp; (2) pouring the flower pulp into water at 25—30°C, adding a compound enzyme for enzymolysis, then adding carbon tetrachloride, and standing for 2—3 h to obtain a rose essential oil crude extract; and (3) heating the rose essential oil crude extract in a water bath for reflux, then carrying out ice bath to 8—lO°C, separating out the carbon tetrachloride at the lower layer, and then heating and distilling in a closed water bath to obtain the rose essential oil. The method provided by the present disclosure has the advantages of simple eguipment, low loss, high oil yield of the rose essential oil and high extraction rate of top note in the rose essential oil.

Description

P1143/NLpd
METHOD FOR EXTRACTING ROSE ESSENTIAL
TECHNICAL FIELD
The present disclosure relates to a method for extracting fragrant oil, and particularly relates to a method for extracting rose essential oil.
BACKGROUND ART
Rose is one of the world-known flowers, known as “the queen of flowers”, and is respected as “the flower of goddess” in an- cient China. Rose belongs to rosaceae, is a kind of shrub with fallen leaves, has dense stems and sharp thorns, has beautiful color and fragrance, and is an economic flower integrating appre- ciation, eating and medicinal use. The rose essential oil ranks first in the fresh flower oil, it is elegant, soft, fine, and sweet like honey and has rose fragrance, and the fragrance is strong. The rose essential oil has the effects of inhibiting bac- teria, resisting oxidation, resisting sensitivity, preserving moisture, promoting cell regeneration, etc., has good effects on the respiratory system, the digestive system, the circulatory sys- tem and the reproductive system, and has the effects of suppress- ing, reducing pressure, promoting sleep, resisting conflict, re- lieving tension, resisting depression, etc. in the aspect of emo- tion. It has high price, its international market price is equal to that of gold, so there is a good reputation of “the queen of essential oil” and “liquid gold” for the rose essential oil. The rose essential oil is the most important and common precious flow- er fragrance raw material in spice blending, it is widely used in food, high-grade cosmetics and tobacco, and can also be used as a medicinal and food additive.
The natural rose essential oil is very complex in composi- tion, and comprises the main components of monoterpene compounds such as geraniol, B-citronellol and linalool, wherein rose oxide, sesquiterpene and sesquiterpene oxygen-containing compounds also account for a considerable proportion, the natural rose essential
0il also comprises other compounds such as heptaldehyde, ethanol and alkane series, and the content of the chemical components and the difference of the chemical components make subtle difference of the rose fragrance.
In general, geraniol, B-citronellol and nerol and esters thereof are basic components for forming the rose fragrance, and are main fragrance components of roses.
At present, the traditional extraction processes of the rose essential oil mainly comprise a steam distillation method and an organic solvent extraction method.
Most of manufacturers in China adopt the steam distillation method to extract the rose essential oil, and the method has the characteristics of simple equipment, low cost, con- venient operation, etc.; however, the operating temperature is close to 100°C, so the rose essential oil with low boiling point and water-soluble fragrant components such as 2-phenethyl alcohol, etc. are possibly lost or damaged, and the yield of the rose es- sential oil is low; and due to the adverse effect of high- temperature steam, the extracted rose essential oil has deep color and burnt smell.
The organic solvent extraction method can simul- taneously extract components with low boiling point and high boil- ing point so that the loss of fragrant oil components is reduced; the fragrance of the obtained rose essential oil is closer to that of natural rose, and the oil yield is higher than that of the steam distillation method, but the extraction time is long; and the first fragrance of the obtained essential oil is slightly in- sufficient, and solvent residue is easily produced.
In recent years, on the basis of the traditional extraction process, some new separation and purification technologies such as a supercriti- cal fluid extraction technology and a molecular distillation tech- nology are successfully applied to the extraction of the rose es- sential oil.
For example, CN 106281713 A discloses a method for extracting rose essential oil, which adopts supercritical carbon dioxide fluid for continuous circulating extraction, the extrac- tion pressure is up to 15-25 MPa, and the separation pressure is also up to 8-10 Mpa.
Therefore, the supercritical C02 extraction technology has high equipment operation pressure, and more im- portantly, the switching is frequent, design experience and an ef- fective design method are lacked, and sealing elements cannot be repeatedly used; and moreover, the design and production standards of the equipment are not available in China at present, and large- scale standardized production cannot be realized.
In China, roses have the unique styles of large flowers, thick petals, bright color and good fragrance, the development po- tential of the industry is huge, and the market prospect is wide.
However, at present, the rose essential oil produced in China is not good in quality and is difficult to be put together in the in- ternational market. Therefore, it is urgently needed to develop an extraction method which can increase the oil yield and improve the first fragrance of the rose essential oil.
SUMMARY
The purpose of the present disclosure is realized through the following technical solution: a method for extracting rose essen- tial oil comprises the following steps: (1) soaking fresh rose petals in water, and then pulping to obtain flower pulp; (2) pouring the flower pulp obtained in the step (1) into wa- ter at 25-30°C, adding a compound enzyme for enzymolysis to com- pletely volatilize the rose essential oil, then adding carbon tet- rachloride, and standing for 2-3 h to obtain a rose essential oil crude extract; and (3) heating the rose essential oil crude extract obtained in the step (2) in a water bath for reflux to completely dissolve the rose essential oil in an organic solvent, then carrying out ice bath to 8-10°C, separating out the carbon tetrachloride at the low- er layer, and then heating and distilling in a closed water bath to obtain the rose essential oil.
Further, in the step (1), the mass ratio of fresh rose petals to water (preferably purified water) is 1: (2.0-2.5), and the soaking time is 90-120 min.
Further, in the step (2), the mass ratio of the flower pulp to water at 25-30°C is 1: (4-5), the consumption of complex enzyme is 3x104 U/g-5.1x104 U/g, and the mass ratio of carbon tetrachlo- ride to the flower pulp is 1: (2-2.5).
Further, the complex enzyme is prepared from cellulase and pectinase according to the proportion of 1: 2.
Further, in the step (3), water bath heating is performed to reach 50-55°C for reflux, and closed water bath heating at 50-60°C is performed for distillation for 2.5-3 h.
In the present disclosure, under the effect of the complex enzyme, the rose essential oil is completely subjected to enzymol- ysis, then, through the combination of carbon tetrachloride ex- traction and water bath heating reflux, ingredients such as the rose essential oil, geraniol and citronellol are also effectively separated out, therefore, the yield of the rose essential oil is greatly improved; the fragrance is natural; the mouthfeel is good; the irritation is small; the quality of the rose essential oil is also obviously improved.
The present disclosure has the advantages that the equipment is simple, the loss is low, the oil yield of the rose essential oil is high, and the extraction rate of first fragrance in the rose essential oil is also high.
DETAILED DESCRIPTION OF THE EMBODIMENTS
Exemplary embodiments of the present disclosure will be de- scribed in more detail below with reference to the drawings. While exemplary embodiments of the present disclosure have been shown, it should be understood that the present disclosure may be embod- ied in various forms and should not be limited by the embodiments set forth herein. Rather, these embodiments are provided so that the present disclosure will be more thoroughly understood, and will fully convey the scope of the present disclosure to those skilled in the art.
Embodiment 1 (1) Fresh rose petals were soaked in purified water for 100 min and then were pulped to obtain flower pulp, wherein the mass ratio of the fresh rose petals to the purified water was 1: 2.2; (2) The flower pulp obtained in the step (1) was poured into water at 28°C, 1.2x104 U/g of cellulase and 2.4x104 U/g of pecti- nase were added for enzymolysis, then carbon tetrachloride was added, and the mixture was subjected to standing for 2.5 h to ob- tain a rose essential oil crude extract, wherein the mass ratio of the carbon tetrachloride to the flower pulp was 1: 2.1; and (3) The rose essential oil crude extract obtained in the step 5 (2) was heated in a water bath to 53°C for reflux, then ice bath was carried out until the temperature reached 9°%, the carbon tet- rachloride at the lower layer was separated out, and then heating and distilling were carried out in a closed water bath at 55°C for 2.8 h to obtain the rose essential oil, wherein the oil yield could be up to 0.8137%.
Embodiment 2 (1) Fresh rose petals were soaked in purified water for 110min and then were pulped to obtain flower pulp, wherein the mass ratio of the fresh rose petals to the purified water was 1: 2.3; (2) The flower pulp obtained in the step (1) was poured into water at 26°C, 1.5x104 U/g of cellulase and 3x104 U/g of pectinase were added for enzymolysis, then carbon tetrachloride was added, and the mixture was subjected to standing for 2.6 h to obtain a rose essential oil crude extract, wherein the mass ratio of the carbon tetrachloride to the flower pulp was 1: 2.2; and (3) The rose essential oil crude extract obtained in the step (2) was heated in a water bath to 52°C for reflux, then ice bath was carried out until the temperature reached 8.5°C, the carbon tetrachloride at the lower layer was separated out, and then heat- ing and distilling were carried out in a closed water bath at 56°C for 2.6 h to obtain the rose essential oil, wherein the oil yield could be up to 0.7842.
Embodiment 3 (1) Fresh rose petals were soaked in purified water for 90 min and then were pulped to obtain flower pulp, wherein the mass ratio of the fresh rose petals to the purified water was 1: 2.5; (2) The flower pulp obtained in the step (1) was poured into water at 30°C, 1x104 U/g of cellulase and 2x104 U/g of pectinase were added for enzymolysis, then carbon tetrachloride was added, and the mixture was subjected to standing for 2 h to obtain a rose essential oil crude extract, wherein the mass ratio of the carbon tetrachloride to the flower pulp was 1: 2; and (3) The rose essential oil crude extract obtained in the step (2) was heated in a water bath to 50°C for reflux, then ice bath was carried out until the temperature reached 10°C, the carbon tet- rachloride at the lower layer was separated out, and then heating and distilling were carried out in a closed water bath at 50°C for 3 h to obtain the rose essential oil, wherein the oil yield could be up to 0.8945%.
Embodiment 4 (1) Fresh rose petals were soaked in purified water for 120min and then were pulped to obtain flower pulp, wherein the mass ratio of the fresh rose petals to the purified water was 1: 2; (2) The flower pulp obtained in the step (1) was poured into water at 25°C, 1.7x104 U/g of cellulase and 3.4x104 U/g of pecti- nase were added for enzymolysis, then carbon tetrachloride was added, and the mixture was subjected to standing for 3 h to obtain a rose essential oil crude extract, wherein the mass ratio of the carbon tetrachloride to the flower pulp was 1: 25; and (3) The rose essential oil crude extract obtained in the step (2) was heated in a water bath to 55°C for reflux, then ice bath was carried out until the temperature reached 8°C, the carbon tet- rachloride at the lower layer was separated out, and then heating and distilling were carried out in a closed water bath at 60°C for 2.5 h to obtain the rose essential oil, wherein the oil yield could be up to 0.8561%.
A GC-MS (gas chromatography-mass spectrometer) was used for testing the content of effective components extracted by the Em- bodiment 1, and the result was shown in Table 1.
Test items 1509842:2003 First fragrance oil extraction en em
Citronellol 220 51.08
The above descriptions are only embodiments of the present disclosure, but the protection scope of the present disclosure is not limited thereto; any easily-thinkable modifications or substi- tutions made by those skilled in the art within the technical scope disclosed by the present disclosure shall be included in the protection scope of the present disclosure. Therefore, the protec- tion scope of the present disclosure shall follow the protection scope of the claims.

Claims (6)

CONCLUSIESCONCLUSIONS 1. Werkwijze voor het extraheren van essentiële rozenolie, omvat- tende de volgende stappen: (1) het in water laten weken van verse rozenblaadjes en het ver- volgens tot pulp verpulveren om bloempulp te verkrijgen; (2) het gieten van de in stap (1) verkregen bloempulp in water van 25 tot 30 °C, het toevoegen van een samengesteld enzym voor enzy- molyse, vervolgens het toevoegen van tetrachloorkoolstof en 2 tot 3 uur laten staan om een ruw extract van essentiële rozenolie te verkrijgen; en (3) het verhitten van het ruwe extract van essentiële rozenolie dat is verkregen in stap (2) in een waterbad voor reflux, vervol- gens uitvoeren van een ijsbad tot 8 tot 10 °C, het tetrachloor- koolstof scheiden in de onderste laag, en vervolgens het verwarmen en destilleren in een gesloten waterbad om de essentiële rozenolie te verkrijgen.A method for extracting rose essential oil, comprising the steps of: (1) soaking fresh rose petals in water and then pulping to obtain flower pulp; (2) pouring the flour pulp obtained in step (1) into water at 25 to 30 °C, adding a compound enzyme for enzyme molysis, then adding carbon tetrachloride and standing for 2 to 3 hours to obtain a crude extract of rose essential oil; and (3) heating the crude extract of rose essential oil obtained in step (2) in a water bath for reflux, then conducting an ice bath to 8 to 10°C, separating the carbon tetrachloride in the bottom layer , and then heating and distilling it in a closed water bath to obtain the rose essential oil. 2. Werkwijze voor het extraheren van essentiële rozenolie volgens conclusie 1, waarbij in stap {1) de massaverhouding van verse ro- zenblaadjes tot water 1: (2,0 tot 2,5) is en de inweektijd 90 tot 120 min is.The method of extracting rose essential oil according to claim 1, wherein in step {1), the mass ratio of fresh rose petals to water is 1: (2.0 to 2.5) and the soaking time is 90 to 120 minutes. 3. Werkwijze voor het extraheren van essentiële rozenolie volgens conclusie 2, waarbij het water gezuiverd water is.The method of extracting rose essential oil according to claim 2, wherein the water is purified water. 4. Werkwijze voor het extraheren van essentiële rozenolie volgens conclusie 1 of 2, waarbij in stap (2) de massaverhouding van de bloempulp tot water bij 25-30 °C 1: (4 tot 5) is, de toegevoegde hoeveelheid van het complexe enzym 3 x 104 U/g tot 5,1 x 104 U/g is, en de massaverhouding van tetrachloorkoolstof tot de bloempulp 1: (2 tot 2,5) is.The method of extracting rose essential oil according to claim 1 or 2, wherein in step (2), the mass ratio of the flower pulp to water at 25-30°C is 1: (4 to 5), the added amount of the complex enzyme is 3 x 10 4 U/g to 5.1 x 10 4 U/g, and the mass ratio of carbon tetrachloride to flour pulp is 1: (2 to 2.5). 5. Werkwijze voor het extraheren van essentiële rozenolie volgens conclusie 4, waarbij het complexe enzym wordt bereid uit cellulase en pectinase in de verhouding van 1: 2.The method of extracting rose essential oil according to claim 4, wherein the complex enzyme is prepared from cellulase and pectinase in the ratio of 1:2. 6. Werkwijze voor het extraheren van essentiële rozenolie volgens een van de conclusies 1, 2 of 4, waarbij in stap (3) waterbadver- warming wordt uitgevoerd om 50 tot 55 °C te bereiken voor reflux, en gesloten waterbadverwarming bij 50 tot 60 °C wordt uitgevoerd voor destillatie gedurende 2,5 tot 3 h.The method of extracting rose essential oil according to any one of claims 1, 2 or 4, wherein in step (3) water bath heating is performed to reach 50 to 55°C for reflux, and closed water bath heating at 50 to 60°C C is carried out for distillation for 2.5 to 3 hours.
NL2030871A 2022-02-09 2022-02-09 Method for extracting rose essential NL2030871B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
NL2030871A NL2030871B1 (en) 2022-02-09 2022-02-09 Method for extracting rose essential

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
NL2030871A NL2030871B1 (en) 2022-02-09 2022-02-09 Method for extracting rose essential

Publications (1)

Publication Number Publication Date
NL2030871B1 true NL2030871B1 (en) 2023-08-15

Family

ID=87654404

Family Applications (1)

Application Number Title Priority Date Filing Date
NL2030871A NL2030871B1 (en) 2022-02-09 2022-02-09 Method for extracting rose essential

Country Status (1)

Country Link
NL (1) NL2030871B1 (en)

Similar Documents

Publication Publication Date Title
US9200238B2 (en) Pomelo peel essential oil extraction method by peel icing and breaking
CN103614230B (en) Preparation method of garlic oil
CN102586018B (en) Method for extracting grape fragrance components from white grape pomace and application of method
CN106367208A (en) Separation and purification method of garlic essential oil
CN107446702A (en) A kind of extracting method of wormwood essential oil
CN106993789B (en) Method for extracting high-quality propolis by using subcritical multi-component mixed solvent
CN104026223B (en) A kind of edible blend oil and preparation method thereof
CN106617047B (en) Mulberry enzyme and production process thereof
CN107569433B (en) Tyrosinase inhibitor extracted from yellow wine lees and preparation method thereof
CN100345500C (en) Method for comprehensive utilization of fragrans by using special flavour improvement enzyme
CN110747234A (en) Preparation method of sophora flower extractum
CN1860947A (en) Supercritical carrot extractive juice, and its application in perfuming of cigarette
CN106539053A (en) A kind of preparation method of gold bergamot quintessence oil
CN109054992A (en) A method of extracting Seabuckthorm Seed Oil
NL2030871B1 (en) Method for extracting rose essential
CN106753774A (en) A kind of camellia oil preparation method
CN1748561A (en) Method for preparing meat smell flavours added with plant extract of twigs of chaste tree
CN110591823A (en) Extraction and separation method of gardenia volatile oil
KR20170056830A (en) Manufacturing method and cosmetic compositions using Dendropanax morbifera Lev extraction fluid
CN107400048A (en) A kind of technique that extraction irone is prepared in the new fresh quench from iris
CN105586153A (en) Truestar anisetree essential oil and preparation method thereof
CN108410582A (en) A kind of extracting method of Rosa Damascana
CN104905999A (en) Gardenia perfume and preparation method thereof
CN103571626A (en) Extracting technology of green Chinese prickly ash perfume oil
CN105176665A (en) Oil-tea-mixed nutrient solid oil capable of replenishing blood and beautifying face and preparation method of oil-tea-mixed nutrient solid oil