CN105779131A - Method for extracting essential oil from citrus peels - Google Patents
Method for extracting essential oil from citrus peels Download PDFInfo
- Publication number
- CN105779131A CN105779131A CN201610295597.6A CN201610295597A CN105779131A CN 105779131 A CN105779131 A CN 105779131A CN 201610295597 A CN201610295597 A CN 201610295597A CN 105779131 A CN105779131 A CN 105779131A
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- Prior art keywords
- peel
- citrus
- quintessence oil
- solution
- crude product
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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
-
- 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
- C11B9/022—Refining
-
- 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
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- 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)
- Preparation Of Fruits And Vegetables (AREA)
- Cosmetics (AREA)
Abstract
The invention discloses a method for extracting essential oil from citrus peels. The method comprises the following steps of 1, collecting peels of fresh and non-decaying citrus fruits, and crushing by a crusher; 2, putting the crushed peels into a round-bottom flask, adding distilled water according to the material and liquid ratio of 1:(5-15), and forming a solution; 3, adding a salting-out agent into the solution, until the solution concentration is 1 to 5%; 4, performing microwave treatment for 30 to 90s; 5, heating to 100 to 120 DEG C, distilling for 30 to 150min, condensing and refluxing, and collecting a crude product; 6, freezing the crude product at the temperature of -40 to -15 DEG C, and removing iced water, so as to obtain the essential oil. The method has the advantages that the extraction rate is 1.38 to 1.77%; the method is simple, the requirement of field equipment is low, the operation is simple and convenient, the cycle is short, an extracting matter with toxic and side effects is not used, the extraction rate is high, and the purity is high.
Description
Technical field
The present invention relates to essential oil preparing technical field, be specifically related to the extracting method of a kind of citrus peel quintessence oil.
Background technology
Citrus is a genus of rutaceae, including Citrus chachiensis Hort., Fructus Citri tangerinae, Fructus Citri grandis, orange etc. 20 several kinds, and its fruit rinds has oil vacuole, generally contains volatile oil, is referred to as citrus.Citrus is mainly distributed on the region on the south north latitude 35-degree in the world.It is cultivated throughout five continents, and in the majority with Brazil, the U.S., China, Japan, Spain, Italy, Morocco, Mexico, Israel, South Africa, Algeria, Egypt, Greece, Turkey, Argentina, India, the cultivated area of Australia and yield.Research shows, major part citrus peel quintessence oil has antibacterial, antioxidation and the biologic activity such as walks quickly and keeps away, can be as the additive of food, medicine, health product and cosmetics.Along with expanding economy and growth in the living standard, people are increasingly stronger to the consciousness such as life and health and environmental conservation, therefore also get more and more the demand of natural antioxidant, repellant, antibacterial and various additive.Citrus class fruit is essentially all edible fruit, and peel quintessence oil is natural, safety is high for it, is with a wide range of applications.
Produce upper wide variety of method of extraction of essential oil at present mainly to have: steam distillation, milling process, solvent extraction three kinds: steam distillation is that the principle utilizing water vapour to take away volatile oil is to prepare essential oil.The essential oil so obtained is also referred to as " deep fat ".The operation of this method is the simplest, and cost is relatively low, is the most frequently used extracting process, is homogeneously added into the solid NaCl of 3% on broken Pericarpium Citri tangerinae, can improve oil yield about 20%.This method has the drawback that the composition of gained quintessence oil probably due to heat and some change.Milling process is to squeeze peel of Citrus reticulata Blanco with crunch so that it is oil cell ruptures, and causes oil content to flow out, and then separates oily.Use this method obtain peel of Citrus reticulata Blanco oil yield about 0.3%, pressed oil fragrance is close to orange fruital, and color is light yellow.The quintessence oil oil of this method gained is good, but it has the drawback that the extraction to tangerine essential oil is not thorough, and yield is relatively low.Solvent extraction method is to utilize lower boiling organic solvent such as hexane, ether, petroleum ether and ethanol etc. to soak peel of Citrus reticulata Blanco thus essential oil is put forward.This method it is critical only that selected solvent must have preferable selectivity and relatively low viscosity to effective ingredient, preferably selects performance to make effective ingredient have relatively large dissolubility, relatively low viscosity can be allowed to bigger diffusion velocity.The method is simple to operate, but gained quintessence oil often exists organic solvent residual, and yield is relatively low.Above-mentioned method is respectively arranged with quality, and some organic solvents of using a large amount of toxic side effects, the extraction effect that has are poor, and the extraction ratio of above-mentioned three kinds of methods is all between 0.2～0.5%, and extraction ratio is relatively low.Accordingly, it would be desirable to develop a kind of combined extraction method, solve drawbacks described above.
Summary of the invention
The invention is intended to provide the extracting method of a kind of citrus peel quintessence oil, to solve the problem that prior art uses the solvent extraction of toxic side effect, extraction effect is poor, extraction ratio is relatively low.
The extracting method of a kind of citrus peel quintessence oil in this programme, comprises the steps:
Step one, collect fresh, without the fruit rind of citrus rotted, pulverizer is pulverized；
Step 2, will pulverize after peel be placed in round-bottomed flask, by solid-liquid ratio 1:5～15 add distilled water, formed solution；
Step 3, add salting-out agents in the solution, be 1～5% to solution concentration；
Step 4, microwave treatment 30～90s；
Step 5, it is heated to 100～120 DEG C, distills 30～150min, condensing reflux, collect crude product；
Step 6, crude product is placed on freezing processing at-40 DEG C～-15 DEG C, removes the water frozen, obtain quintessence oil.
The operation principle of the present invention and beneficial effect: the peel of the present invention is pulverized by pulverizer, peel granule diminishes, and its specific surface area is significantly greatly increased so that it is contacts more fully with extracting solution, effectively facilitates the release of quintessence oil；Microwave treatment can make pericarp membrane fully burst so that quintessence oil release more fully.Salting-out agents are not participate in complex reaction, soluble and nontoxic inorganic salts, including sodium salt, potassium salt, magnesium salt, calcium salt, ammonium salt, iron salt and aluminium salt etc., on the one hand the dissolubility of quintessence oil is reduced further by salting out, on the other hand the boiling point of solution is properly increased, this can promote that quintessence oil is distilled off, improving overall extraction ratio, the extraction ratio of the present invention is 1.38～1.77%, much larger than the extraction ratio of traditional handicraft (traditional rate of mentioning is 0.2～0.5%).This method uses freezing to remove the water in crude product, it is to avoid uses poisonous and hazardous organic solvent to extract, makes extracted quintessence oil safer, green, and Simplified flowsheet simultaneously reduces cost.The present invention has the extraction of substance that method is simple, place equipment requirements is low, easy and simple to handle, the cycle is short, do not use band toxic and side effects, has the advantage that extraction ratio is high, purity is high.
Further, when described step one processes, when the Rhizoma Euonymus layer thickness of peel is more than 0.5mm, first remove Rhizoma Euonymus layer.Because quintessence oil typically concentrates existence and coloured exodermis, Rhizoma Euonymus layer does not contains quintessence oil, first removes the treating capacity that can reduce entirety, reduces cost.
Preferably, the salting-out agents in described step 3 are NaCl, CaCl2, one in KCl.These three salting-out agents are for other salting-out agents, notable to the raising effect of extraction of essential oil rate.
Detailed description of the invention
Below by detailed description of the invention, the present invention is further detailed explanation:
Embodiment 1:
The extracting method of a kind of citrus peel quintessence oil, comprises the following steps
Step one, collect fresh, without the peel 30g of citrus fruits rotted, if the Rhizoma Euonymus layer thickness of peel is more than 0.5mm, after first removing Rhizoma Euonymus layer, re-use pulverizer and peel pulverized；
Step 2, will pulverize after peel be placed in round-bottomed flask, by solid-liquid ratio (w/V) 1:7 add distilled water, formed solution；
Step 3, backward round-bottomed flask in add NaCl be 1% to solution concentration；
Step 4, by solution microwave treatment 60s after step 3 processes；
Step 5, it is heated to 100 DEG C, distills 120min, condensing reflux, collect crude product；
Step 6, crude product is placed on-40 DEG C of freezing processing, removes the water frozen further, obtain quintessence oil.Under this operation, extraction of essential oil rate can reach 1.65 ± 0.12%.
Embodiment 2:
The extracting method of a kind of citrus peel quintessence oil, comprises the following steps:
Step one, collect fresh, without the peel 40g of citrus fruits rotted, if the Rhizoma Euonymus layer thickness of peel is more than 0.5mm, after first removing Rhizoma Euonymus layer, re-use pulverizer and peel pulverized；
Step 2, will pulverize after peel be placed in round-bottomed flask, by solid-liquid ratio (w/V) 1:10 add distilled water, formed solution；
Step 3, backward round-bottomed flask in add CaCl2It is 1% to solution concentration；
Step 4, by solution microwave treatment 30s after step 3 processes；
Step 5, it is heated to 110 DEG C, distills 120min, condensing reflux, collect crude product；
Step 6, crude product is placed on-20 DEG C of freezing processing, removes the water frozen further, obtain quintessence oil.Under this operation, extraction of essential oil rate reaches 1.54 ± 0.08%.
Embodiment 3:
The extracting method of a kind of citrus peel quintessence oil, comprises the following steps:
Step one, collect fresh, without the peel 50g of citrus fruits rotted, if the Rhizoma Euonymus layer thickness of peel is more than 0.5mm, after first removing Rhizoma Euonymus layer, re-use pulverizer and peel pulverized；
Step 2, will pulverize after peel be placed in round-bottomed flask, by solid-liquid ratio (w/V) 1:15 add distilled water, formed solution；
Step 3, backward round-bottomed flask in add KCl be 3% to solution concentration；
Step 4, by solution microwave treatment 90s after step 3 processes；
Step 5, it is heated to 120 DEG C, distills 90min, condensing reflux, collect crude product；
Step 6, crude product is placed on-15 DEG C of freezing processing, removes the water frozen further, obtain quintessence oil.Under this operation, extraction of essential oil rate reaches 1.49 ± 0.11%.
Embodiment 4:
The extracting method of a kind of citrus peel quintessence oil, comprises the following steps:
Step one, collect fresh, without the peel 30g of citrus fruits rotted, if the Rhizoma Euonymus layer thickness of peel is more than 0.5mm, after first removing Rhizoma Euonymus layer, re-use pulverizer and peel pulverized；
Step 2, will pulverize after peel be placed in round-bottomed flask, by solid-liquid ratio (w/V) 1:10 add distilled water, formed solution；
Step 3, backward round-bottomed flask in add NaCl be 1% to solution concentration；
Step 4, by solution microwave treatment 30s after step 3 processes；
Step 5, it is heated to 100 DEG C, distills 150min, condensing reflux, collect crude product；
Step 6, crude product is placed on-20 DEG C of freezing processing, removes the water frozen further, obtain quintessence oil.Under this operation, extraction of essential oil rate reaches 1.57 ± 0.06%.
The foregoing is only the preferred embodiments of the present invention, it is not limited to the present invention, although the present invention being described in detail with reference to previous embodiment, for a person skilled in the art, technical scheme described in foregoing embodiments still can be modified by it, or wherein portion of techniques feature is carried out equivalent.All within the spirit and principles in the present invention, any modification, equivalent substitution and improvement etc. done, should be included within the scope of the present invention.
Claims (3)
1. the extracting method of a citrus peel quintessence oil, it is characterised in that comprise the steps:
Step one, collect fresh, without the peel of citrus fruits rotted, pulverizer is pulverized；
Step 2, will pulverize after peel be placed in round-bottomed flask, by solid-liquid ratio 1:5～15 add distilled water, formed solution；
Step 3, add salting-out agents in the solution, be 1 ~ 5% to solution concentration；
Step 4, microwave treatment 30～90s；
Step 5, it is heated to 100～120 DEG C, distills 30～150min, condensing reflux, collect crude product；
Step 6, crude product is placed on freezing processing at-40 DEG C～-15 DEG C, removes the water frozen, obtain quintessence oil.
The extracting method of citrus peel quintessence oil the most according to claim 1, it is characterised in that: when described step one processes, when the Rhizoma Euonymus layer thickness of peel is more than 0.5mm, first remove Rhizoma Euonymus layer.
The extracting method of citrus peel quintessence oil the most according to claim 1, it is characterised in that: the salting-out agents in described step 3 are NaCl, CaCl2, one in KCl.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610295597.6A CN105779131A (en) | 2016-05-06 | 2016-05-06 | Method for extracting essential oil from citrus peels |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610295597.6A CN105779131A (en) | 2016-05-06 | 2016-05-06 | Method for extracting essential oil from citrus peels |
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| CN105779131A true CN105779131A (en) | 2016-07-20 |
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| CN201610295597.6A Pending CN105779131A (en) | 2016-05-06 | 2016-05-06 | Method for extracting essential oil from citrus peels |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106281718A (en) * | 2016-10-30 | 2017-01-04 | 黄全 | The way of distillation extracts the method for Flos Rosae Rugosae quintessence oil from Cymbopogon martini |
| CN107307262A (en) * | 2017-08-14 | 2017-11-03 | 遵义医学院 | A kind of calamondin essential oil with bacteriostatic activity and preparation method and application |
| CN107699356A (en) * | 2017-11-07 | 2018-02-16 | 常州福隆工控设备有限公司 | A kind of extracting method of Peppermint essential oil |
| CN108208535A (en) * | 2017-12-29 | 2018-06-29 | 安徽九洲方圆制药有限公司 | A kind of method of Chinese medicine preparation aflatoxin degradation |
| CN112175735A (en) * | 2020-09-22 | 2021-01-05 | 广东华萃生物科技有限公司 | Extraction method of pericarp essential oil |
| CN112167317A (en) * | 2020-09-10 | 2021-01-05 | 长沙沃霖农副产品开发有限公司 | Aquatic product water-retaining preservative and freezing preservation method |
| CN112980585A (en) * | 2021-03-26 | 2021-06-18 | 江西科技师范大学 | Method for extracting orange peel essential oil |
| CN114149864A (en) * | 2021-12-14 | 2022-03-08 | 浙江工商大学 | Method for improving extraction rate of essential oil of citrus unshiu by using ultrasonic-assisted micro-cutting auxiliary agent and application |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106281718A (en) * | 2016-10-30 | 2017-01-04 | 黄全 | The way of distillation extracts the method for Flos Rosae Rugosae quintessence oil from Cymbopogon martini |
| CN107307262A (en) * | 2017-08-14 | 2017-11-03 | 遵义医学院 | A kind of calamondin essential oil with bacteriostatic activity and preparation method and application |
| CN107699356A (en) * | 2017-11-07 | 2018-02-16 | 常州福隆工控设备有限公司 | A kind of extracting method of Peppermint essential oil |
| CN108208535A (en) * | 2017-12-29 | 2018-06-29 | 安徽九洲方圆制药有限公司 | A kind of method of Chinese medicine preparation aflatoxin degradation |
| CN112167317A (en) * | 2020-09-10 | 2021-01-05 | 长沙沃霖农副产品开发有限公司 | Aquatic product water-retaining preservative and freezing preservation method |
| CN112175735A (en) * | 2020-09-22 | 2021-01-05 | 广东华萃生物科技有限公司 | Extraction method of pericarp essential oil |
| CN112980585A (en) * | 2021-03-26 | 2021-06-18 | 江西科技师范大学 | Method for extracting orange peel essential oil |
| CN112980585B (en) * | 2021-03-26 | 2022-08-26 | 江西科技师范大学 | Method for extracting orange peel essential oil |
| CN114149864A (en) * | 2021-12-14 | 2022-03-08 | 浙江工商大学 | Method for improving extraction rate of essential oil of citrus unshiu by using ultrasonic-assisted micro-cutting auxiliary agent and application |
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Application publication date: 20160720 |
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