CN106867676A - A kind of extracting method of navel orange pericarp essential oil - Google Patents
A kind of extracting method of navel orange pericarp essential oil Download PDFInfo
- Publication number
- CN106867676A CN106867676A CN201710268736.0A CN201710268736A CN106867676A CN 106867676 A CN106867676 A CN 106867676A CN 201710268736 A CN201710268736 A CN 201710268736A CN 106867676 A CN106867676 A CN 106867676A
- Authority
- CN
- China
- Prior art keywords
- navel orange
- essential oil
- orange pericarp
- pericarp essential
- extracting method
- Prior art date
- Legal status (The legal status 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 status listed.)
- Withdrawn
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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0211—Solvent extraction of solids in combination with an electric or magnetic field
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0261—Solvent extraction of solids comprising vibrating mechanisms, e.g. mechanical, acoustical
- B01D11/0265—Applying ultrasound
-
- 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
The invention discloses a kind of extracting method of navel orange pericarp essential oil, comprise the following steps：(1) preparation of rough navel orange pericarp essential oil：After navel orange pericarp is crushed, it is placed in the extraction kettle of microwave ultrasonic wave synergic solvent extraction instrument, microwave ultrasonic wave synergic solvent extraction is carried out after adding extractant, extract is filtered, rectifying filtrate, obtains rough navel orange pericarp essential oil.(2) the de- terpene treatment of rough navel orange pericarp essential oil：Rough navel orange pericarp essential oil obtained by step (1) is placed in the reactor of molecular distillation instrument, molecular distillation is carried out, collection evaporates excess, obtains navel orange pericarp essential oil.The extracting method of the navel orange pericarp essential oil have the advantages that quickly, efficiently, high income, essential oil content be high, steady quality.
Description
Technical field
The present invention relates to the extractive technique field of natural plant essential oils, more particularly to a kind of extraction side of navel orange pericarp essential oil
Method.
Background technology
Fu Chuan counties of city of south china navel orange abundance, its pericarp be eat, the Main By product in process.According to tune
Look into, comprehensive utilization of this area at present to tribute mandarin orange, navel orange pericarp is less, is dropped mostly as discarded object, not only wastes
Valuable resource, goes back severe contamination environment.Domestic and international numerous studies confirm tangerine oil have make human central nervous it is calm,
Mitigate the effect of irritability, also with eliminating the phlegm, cough-relieving, promote the effects such as enterogastric peristalsis, analgesia and antiphlogistic antibacterial, while essential oil pair
Beauty and health care also has obvious effect.World's annual production about 2.6 ten thousand t, the 986.95 dollars/t of price of tangerine oil, and China
Annual production relatively low only 5,000,000 t, 500 dollars/t of price.International market tangerine oil is in great demand, good market prospect.Cause
This, navel orange pericarp is turned waste into wealth, and is finished and deep development, is not only greatly improved the economic worth of navel orange pericarp,
Extend the Citrus Industry chain of China, can also promote the exploitation and development of tangerine oil essence and flavoring agent.
Navel orange pericarp essential oil be by monoterpene alkenes, sesquiterpene and higher alcohols, aldehydes, ketone, esters, phenols,
The oxygenatedchemicals of the compositions such as acids, wherein limonene are the main components of navel orange pericarp essential oil, and alcohols, aldehydes and esters etc.
Compounds content is the main source of navel orange pericarp essential oil fragrance less than 8%, but.Limonene is contributed not essential oil fragrance component
Greatly, its chemical property is active, oxidizable into limonene peroxide under air and illumination condition, and this type oxide is unstable
It is fixed, a series of impurity such as carvol, carveol can be converted further into, so as to influence the quality of essential oil and use.Therefore, by lemon
Lemon alkene is separated from essential oil, helps to slow down essential oil generation qualitative change, improves essential oil stability and aroma quality, extends essential oil
Storage time, navel orange pericarp essential oil is effectively utilized.
At present, the tangerine oil oxide concentration in China market is not high, and fragrance is thin, and in the market rarely have it is special
Navel orange pericarp essential oil.Therefore, a kind of high income, essential oil content navel orange pericarp extracting method high are developed extremely necessary.
The content of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art, there is provided a kind of quick, efficient, high income,
Essential oil content is high, steady quality navel orange pericarp extracting method.
In order to solve the above technical problems, the present invention uses following technical scheme：
A kind of extracting method of navel orange pericarp essential oil, comprises the following steps：
(1) preparation of rough navel orange pericarp essential oil：After navel orange pericarp is crushed, Combined microwave-ultrasound extraction instrument is placed in
Extraction kettle in, add extractant after carry out Combined microwave-ultrasound extraction, extract is filtered, rectifying filtrate obtains
To rough navel orange pericarp essential oil；
(2) the de- terpene treatment of rough navel orange pericarp essential oil：Rough navel orange pericarp essential oil obtained by step (1) is placed in molecule
In the reactor of distillation apparatus, molecular distillation is carried out, collection evaporates excess, obtains navel orange pericarp essential oil.
The extracting method of above-mentioned navel orange pericarp essential oil, it is preferred that in the step (1), the extractant includes third
Ketone, n-hexane, ether or ethanol, the navel orange pericarp are 1g: 3mL~5mL with the ratio of extractant.
The extracting method of above-mentioned navel orange pericarp essential oil, it is preferred that in the step (1), 50 DEG C~80 DEG C of extraction temperature,
Extraction time is 18min~30min, extracting pressure 1.0 × 106Pa~2.0 × 106Pa, microwave irradiation power 350W~600W,
Ultrasonic frequency is 30kHz~50kHz.
The extracting method of above-mentioned navel orange pericarp essential oil, it is preferred that in the step (2), the molecular distillation temperature is
40 DEG C~50 DEG C, distillation pressure is 150Pa~300Pa, and charging rate is 1.5mL/min~3mL/min, and rotating speed is 200r/min
~300r/min.
The extracting method of above-mentioned navel orange pericarp essential oil, it is preferred that before the step (1), also including by navel orange pericarp
Stored 1 day~2 days at being placed in -15 DEG C~-25 DEG C.
Compared with prior art, the advantage of the invention is that：
1st, the present invention carries out the extraction of rough essential oil using Combined microwave-ultrasound extraction method to navel orange pericarp, due to micro-
The broken wall effect and fuel factor of ripple and the cavitation of ultrasonic wave and mechanical oscillation effect, there are essential oil in can accelerating plant cell
The dissolution of composition is imitated, significantly shortens extraction time, improved extraction efficiency and extract quality, and be avoided that high temperature to extract component
Influence.And, the present invention meets the optimal Combined microwave-ultrasound extraction technological parameter of navel orange pericarp by design, makes navel orange
Derived essential oil in pericarp can preferably dissolution.
2nd, the present invention carries out terpene compound and terpenes in the rough essential oil of navel orange pericarp and aoxidizes with molecular distillation technique
Thing is efficiently separated, and compared with traditional separation method, vapo(u)rizing temperature is low, and heated time is short, therefore alcohols, aldehydes and esters
Deng having, the loss of aromatic compound is few, and gained essential oil product essential oil content is high, give off a strong fragrance, and period of storage is long.Further,
The present invention meets the optimal molecular distillation technological parameter of the rough essential oil of navel orange pericarp by design, in making the rough essential oil of navel orange pericarp
Terpene compound especially limonene is maximized and slipped out, it is main with alcohols, aldehydes and esters etc. in the essential oil product of gained
Have based on aromatic compound.
Specific embodiment
Below in conjunction with specific preferred embodiment, the invention will be further described, following examples set forth of the invention
Specific embodiments, so that the present invention is further illustrated, these embodiments are explanation and do not indicate that the present invention is all
Possibility, the present invention is not limited only to material in these embodiments, reaction condition or parameter.These are without departing from this
Invent the basic conception of description, thus these modifications or it is different should all in the range of present invention covering.
Embodiment 1：
A kind of extracting method of navel orange pericarp essential oil of the invention, comprises the following steps：
(1) preparation of rough navel orange pericarp essential oil：By the navel orange pericarp 200g of the preservation one day in -20 DEG C of freezer through height
After fast medicinal herb grinder is crushed, it is placed in the extraction kettle of Combined microwave-ultrasound extraction instrument, adds 600mL absolute ethyl alcohols, carries out
Combined microwave-ultrasound extraction, 50 DEG C of extraction temperature, extraction time 20min, extracting pressure 1.21 × 106Pa, microwave work(
Rate is 500W, and ultrasonic frequency is 40kHz.Extraction is filtered extract after finishing, and rectifying filtrate obtains rough navel orange really
Peel essential oil.
(2) the de- terpene treatment of rough navel orange pericarp essential oil：Rough navel orange pericarp essential oil 10g obtained by step (1) is placed in
In the reactor of molecular distillation instrument, molecular distillation is carried out, molecular distillation temperature is 45 DEG C, and distillation pressure is 200Pa, charging rate
It is 2.0mL/min, rotating speed is 200r/min.Thing as (R)-4-isopropenyl-1-methyl-1-cyclohexene is slipped out, collection evaporates excess, obtains navel orange pericarp essential oil.
Using the content of titration measuring limonene.Take after limonene extract solution 10mL is settled to 1000mL, take 10mL this
Dilution adds 15mL isopropanols and 25mL distilled water in 150mL cucurbits, connects distilling apparatus, heating distillation.With first
Base orange is indicator, is titrated with potassium bromate standard liquid (0.0248mol/L), and indicator color disappears and is terminal,
Parallel sampling is averaged in triplicate, is done blank by same steps and is tested.Navel orange pericarp is calculated according to following equation (1)
The content of limonene in essential oil：
In formula：
W --- the content of limonene, g/kg in navel orange pericarp essential oil；
The quality of m --- essential oil, g；
V1--- titration potassium bromate standard liquid titration volumes, mL；
V0--- titration blank potassium bromate standard liquid titration volumes, mL；
0.00085 --- 0.0248mol/L potassium bromate standard liquid 1mL are equivalent to 0.00085g limonenes.
Taking off terpene rate computing formula (2) is：
Through measuring and calculating, the de- terpene rate of the present embodiment is 93.21%.
In order to judge that molecular distillation slips out whether thing is limonene, to slip out thing carry out respectively index of refraction, specific rotatory power and
The measure of relative density, its result of the test is as shown in table 1：
The contrast of the index of refraction of table 1, specific rotatory power and relative density values
| Constant | The standard value of limonene | Separation product measured value |
| Index of refraction | 1.4743 | 1.4740 |
| +123.8° | +124.0° | |
| Relative density | 0.841 | 0.839 |
From the data in table 1, it can be seen that the index of refraction of gained separation product, specific rotatory power and relative density measured value and limonene mark
Quasi- value is coincide substantially, it can be determined that gained separation product is limonene.
Embodiment 2：
A kind of extracting method of navel orange pericarp essential oil of the invention, comprises the following steps：
(1) preparation of rough navel orange pericarp essential oil：By the navel orange pericarp 200g of the preservation two days in -20 DEG C of freezer through height
After fast medicinal herb grinder is crushed, it is placed in the extraction kettle of Combined microwave-ultrasound extraction instrument, adds 800mL n-hexanes, carries out micro-
Ripple-ultrasonic synergistic extraction, 60 DEG C of extraction temperature, extraction time 25min, extracting pressure 1.50 × 106Pa, microwave irradiation power
It is 450W, ultrasonic frequency is 45kHz.Extraction is filtered extract after finishing, and rectifying filtrate obtains rough navel orange pericarp
Essential oil.
(2) the de- terpene treatment of rough navel orange pericarp essential oil：Rough navel orange pericarp essential oil 10g obtained by step (1) is placed in
In the reactor of molecular distillation instrument, molecular distillation is carried out, molecular distillation temperature is 40 DEG C, and distillation pressure is 250Pa, charging rate
It is 1.5mL/min, rotating speed is 250r/min.Thing as (R)-4-isopropenyl-1-methyl-1-cyclohexene is slipped out, collection evaporates excess, obtains navel orange pericarp essential oil.
Through measuring and calculating, the de- terpene rate of the present embodiment is 92.73%.
The above is only the preferred embodiment of the present invention, and protection scope of the present invention is not limited merely to above-mentioned implementation
Example.All technical schemes belonged under thinking of the present invention belong to protection scope of the present invention.It is noted that for the art
Those of ordinary skill for, improvements and modifications under the premise without departing from the principles of the invention, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (5)
1. a kind of extracting method of navel orange pericarp essential oil, comprises the following steps：
(1) preparation of rough navel orange pericarp essential oil：After navel orange pericarp is crushed, the extraction of Combined microwave-ultrasound extraction instrument is placed in
Take in kettle, Combined microwave-ultrasound extraction is carried out after adding extractant, extract is filtered, rectifying filtrate, obtain thick
Navel orange pericarp essential oil processed；
(2) the de- terpene treatment of rough navel orange pericarp essential oil：Rough navel orange pericarp essential oil obtained by step (1) is placed in molecular distillation
In the reactor of instrument, molecular distillation is carried out, collection evaporates excess, obtains navel orange pericarp essential oil.
2. the extracting method of navel orange pericarp essential oil according to claim 1, it is characterised in that described in the step (1)
Extractant includes acetone, n-hexane, ether or ethanol, and the navel orange pericarp is 1g: 3mL~5mL with the ratio of extractant.
3. the extracting method of navel orange pericarp essential oil according to claim 2, it is characterised in that in the step (1), extraction
Temperature 50 C~80 DEG C, extraction time is 18min~30min, extracting pressure 1.0 × 106Pa~2.0 × 106Pa, microwave
Power 350W~600W, ultrasonic frequency is 30kHz~50kHz.
4. the extracting method of navel orange pericarp essential oil according to claim 1, it is characterised in that described in the step (2)
Molecular distillation temperature is 40 DEG C~50 DEG C, and distillation pressure is 150Pa~300Pa, and charging rate is 1.5mL/min~3mL/min,
Rotating speed is 200r/min~300r/min.
5. the extracting method of navel orange pericarp essential oil according to claim 1, it is characterised in that before the step (1), also
Stored 1 day~2 days at including navel orange pericarp is placed in into -15 DEG C~-25 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710268736.0A CN106867676A (en) | 2017-04-21 | 2017-04-21 | A kind of extracting method of navel orange pericarp essential oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710268736.0A CN106867676A (en) | 2017-04-21 | 2017-04-21 | A kind of extracting method of navel orange pericarp essential oil |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106867676A true CN106867676A (en) | 2017-06-20 |
Family
ID=59163811
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710268736.0A Withdrawn CN106867676A (en) | 2017-04-21 | 2017-04-21 | A kind of extracting method of navel orange pericarp essential oil |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106867676A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107446706A (en) * | 2017-09-25 | 2017-12-08 | 广西壮族自治区农业科学院农产品加工研究所 | A kind of extracting method of mango core essential oil and its application in banana fresh-keeping |
| CN107937127A (en) * | 2017-11-23 | 2018-04-20 | 湖北聚注通用技术研究有限公司 | A kind of extracting method of pillworm oil and its application |
| CN113101690A (en) * | 2021-04-14 | 2021-07-13 | 云南省粮油科学研究院（云南省粮油产品质量监督检验测试中心） | Extraction method and application of antioxidant in juglans sigillata peel |
| CN113528243A (en) * | 2020-04-14 | 2021-10-22 | 广东省禾基生物科技有限公司 | Extraction method and application of navel orange peel cell water and navel orange peel essential oil |
| CN115125063A (en) * | 2022-07-29 | 2022-09-30 | 重庆三峡学院 | Extraction process and application of orange essential oil |
| WO2023133727A1 (en) * | 2022-01-12 | 2023-07-20 | 广州工商学院 | Household water purification device based on orange peel |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102559386A (en) * | 2011-12-30 | 2012-07-11 | 浙江省农业科学院 | Method for refining and concentrating citrus essential oil |
| CN103897806A (en) * | 2014-04-03 | 2014-07-02 | 广东添乐化妆品有限公司 | Microwave assisted extraction method of lemon essential oil |
| CN106318644A (en) * | 2016-11-02 | 2017-01-11 | 赣南师范大学 | Preparation method of navel orange essential oil molecule distillation component |
-
2017
- 2017-04-21 CN CN201710268736.0A patent/CN106867676A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102559386A (en) * | 2011-12-30 | 2012-07-11 | 浙江省农业科学院 | Method for refining and concentrating citrus essential oil |
| CN103897806A (en) * | 2014-04-03 | 2014-07-02 | 广东添乐化妆品有限公司 | Microwave assisted extraction method of lemon essential oil |
| CN106318644A (en) * | 2016-11-02 | 2017-01-11 | 赣南师范大学 | Preparation method of navel orange essential oil molecule distillation component |
Non-Patent Citations (1)
| Title |
|---|
| 涂招秀 等: "响应面法优化椪柑果皮精油提取新技术工艺研究", 《江西化工》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107446706A (en) * | 2017-09-25 | 2017-12-08 | 广西壮族自治区农业科学院农产品加工研究所 | A kind of extracting method of mango core essential oil and its application in banana fresh-keeping |
| CN107937127A (en) * | 2017-11-23 | 2018-04-20 | 湖北聚注通用技术研究有限公司 | A kind of extracting method of pillworm oil and its application |
| CN113528243A (en) * | 2020-04-14 | 2021-10-22 | 广东省禾基生物科技有限公司 | Extraction method and application of navel orange peel cell water and navel orange peel essential oil |
| CN113101690A (en) * | 2021-04-14 | 2021-07-13 | 云南省粮油科学研究院（云南省粮油产品质量监督检验测试中心） | Extraction method and application of antioxidant in juglans sigillata peel |
| WO2023133727A1 (en) * | 2022-01-12 | 2023-07-20 | 广州工商学院 | Household water purification device based on orange peel |
| CN115125063A (en) * | 2022-07-29 | 2022-09-30 | 重庆三峡学院 | Extraction process and application of orange essential oil |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106867676A (en) | A kind of extracting method of navel orange pericarp essential oil | |
| CN106978257A (en) | The extracting method of navel orange pericarp essential oil | |
| CN103045371B (en) | A kind of preparation method of purify from the wild Du Xiang in Daxing'an Mountainrange essential oil and ursolic acid | |
| CN102504957A (en) | Method for preparing essential oils | |
| CN103923749A (en) | Method for extracting Chinese eaglewood essential oil | |
| CN107051342A (en) | A kind of preparation method of navel orange pericarp essential oil microcapsules | |
| CN103708992B (en) | A kind of level chromatography method extracts the method for squalene in plant oil deodorizing distillate | |
| CN109609276A (en) | A kind of extracting method of oil camphor tree leaf essential oil | |
| CN112457918A (en) | Preparation method and application of citrus essential oil series products | |
| CN105886116A (en) | Method for subcritical fluid extraction of wolfberry seed oil | |
| CN102321503B (en) | Preparation method of fructus momordicae condensate and application thereof | |
| CN101953510B (en) | Method for extracting antioxidant from smashed tobacco powder | |
| Peng et al. | Separation of essential oil from fresh leaves of Phellodendron amurense rupr. By solvent-free microwave-assisted distillation with the addition of lithium salts | |
| CN105461001A (en) | Method and apparatus for treating coal gasification wastewater containing high concentration phenols, and use of extractant | |
| CN104178347B (en) | Azeotropic distillation preparation is without the method for terpene peppermint oil dementholized | |
| CN106316816A (en) | Method for preparing natural citral | |
| CN114931234B (en) | Tobacco source aroma substance, extraction method thereof and cigarette | |
| CN114716317B (en) | Method for separating ethyl acetate from aqueous solution by using eucalyptol | |
| CN101525559A (en) | Method for extracting spice oleoresin from spice | |
| CN103627525A (en) | Method for preparing tobacco essential oil by reduced pressure distillation | |
| CN109852477A (en) | A kind of preparation method of cinnamon essential oil | |
| CN109180618A (en) | A kind of decoloration process of andrographolide | |
| CN104892378B (en) | A kind of preparation method of fenchone | |
| CN106433988A (en) | Extraction method of cinnamon spices | |
| CN109320526B (en) | Method for separating 1, 8-cineole from eucalyptus globulus leaf oil |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20170620 |
|
| WW01 | Invention patent application withdrawn after publication |