CN103897805A - Solvent-free extraction method of lemon essential oil - Google Patents
Solvent-free extraction method of lemon essential oil Download PDFInfo
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Abstract
The invention relates to a solvent-free extraction method of lemon essential oil. The extraction method sequentially comprises the following steps: (1) crushing clean fresh lemon peel, or wetting clean dry lemon peel with water, and then, crushing, so as to obtain lemon peel debris; (2) putting the lemon peel debris into a microwave extraction device, applying microwave radiation to the lemon peel debris, and collecting generated essential oil vapor and condensing, so as to obtain crude lemon essential oil, wherein the manner of microwave radiation applying is intermittent and comprises the processes of carrying out one-time microwave radiation treatment, then, intermitting, and then, carrying out next-time microwave radiation treatment, and repetitively operating in such a manner; (3) separating impurities from the crude lemon essential oil, thereby obtaining the lemon essential oil. The extraction method disclosed by the invention has the advantages of environmental friendliness, rapidness, energy saving and the like, and is less in environmental pollution, easy in raw material obtaining, simple in process, convenient in operation, low in energy consumption, low in cost and high in efficiency; the prepared lemon essential oil is free from organic solvent residues and is high in quality and high in purity, and the natural quality of the lemon essential oil is kept.
Description
Technical field
The present invention relates to extract the method for essential oil from plant material, be specifically related to a kind of solvent-free extracting method of lemon quintessence oil, under condition of no solvent, from lemon pericarp, extract the method for lemon quintessence oil.
Background technology
The bioactive ingredients natural environmental-protective extracting from plant, life-time service have no side effect or side effect little, be successfully applied to skin care, whitening, the anti-ageing cosmetic field of waiting for a long time.Compare with traditional makeup, plant-sourced activeconstituents is more easily absorbed by the skin and digests, and curative effect is obvious, with strong points, and can not deposit in vivo.Utilizing the effective constituent in plant milk extract to carry out the research and development of makeup, is focus and the trend of current cosmetic industry, also will become the leading force of following cosmetic industry.
Chinese Plants resource is richly endowed, and plant milk extract industry development is more and more faster, has become independently new industry, is worldwide extensively approved.Along with the emergence in world wide implants extract market, the plant milk extract industry of China also will become the new strategic t shore industry of national economy and social development.
Lemon have the title of " beauty treatment fruit ", vegetal pole horn of plenty.In recent years, the fast development of lemon industry, plantation, industrial scale constantly expand, but the waste of lemon pericarp resource is day by day obvious, and environment is caused to day by day serious pollution.The comprehensive utilization that improves lemon pericarp, can reduce the waste of limited resources, can reduce again environmental pollution.
The lemon quintessence oil extracting from lemon pericarp, Nantural non-toxic side effect.The main chemical compositions of lemon quintessence oil is sobrerone or firpene, amphene, sabinene, bay (spiceleaf) alkene, Dipentine, phantol, bisabolene, Limonene, vernol and neral.Lemon quintessence oil, for makeup, has following effect: contribute to softening aging cutin, purify skin, convergence pore, improves the obscure colour of skin, and desalination pigment and acne print, and profit white muscle skin is had to splendid effect; Be used for removing corn, verruca plana and general wart all very effective; Can soften causes scar tissue, prevention nail trouble is split; Can be anti-ageing, prevent that wrinkle from producing, increase skin gloss, desalination freckle.Therefore, the lemon quintessence oil that research is reclaimed in lemon pericarp is used for makeup, is a very promising technology.
Traditional method of extracting lemon quintessence oil from lemon pericarp is mainly that cold-press, steam distillation, solvent method, supercritical extraction and above several different methods are combined use etc.Milling process purity is not high; Solvent method is used for scientific research; Supercritical extraction cost is high and technical requirements is high not easy to operate.Current most enterprise adopts steam distillation conventionally, by improving equipment, Optimized Extraction Process condition, can obtain the essential oil that purity is higher, and this method cost is low, simple to operate, but extraction efficiency is lower.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of solvent-free extracting method of lemon quintessence oil, this method is under condition of no solvent, from lemon pericarp, extract lemon quintessence oil by intermittent type microwave radiation effect, have technique simple, easy to operate, consume energy low, cost is low, efficiency advantages of higher, and the lemon quintessence oil quality better making.The technical scheme adopting is as follows:
A solvent-free extracting method for lemon quintessence oil, is characterized in that comprising the steps: successively
(1) raw materials pretreatment: clean fresh lemon pericarp is pulverized, or by clean lemon dry fruit skin with pulverizing after water-wet, obtain lemon pericarp fragment;
(2) lemon pericarp fragment step (1) being obtained is placed in microwave extracting apparatus, and lemon pericarp fragment is applied to microwave radiation, collects the essential oil steam the condensation that produce, obtains thick lemon quintessence oil;
The mode that applies microwave radiation is intermittent type, and its process is: carry out after a microwave radiation processing intermittently, then carry out microwave radiation processing next time, repeat operation, carry out repeatedly microwave radiation processing;
(3) isolate the impurity in thick lemon quintessence oil, obtain lemon quintessence oil.
Preferably, in above-mentioned steps (1), the water ratio of lemon pericarp fragment is 20-70%(weight).
Preferably, in above-mentioned steps (2), the temperature in microwave extracting apparatus is controlled at 90-120 DEG C.Before essential oil volatilization, can adopt Electric heating to assist lemon pericarp fragment is heated.
The mode that applies microwave radiation in step (2) is intermittent type, can avoid lemon pericarp local heating excess Temperature to affect essential oil quality and extraction efficiency.Preferably, in above-mentioned steps (2), the power of microwave radiation is 200-500 watt, and the time of each microwave radiation processing is 20 seconds-3 minutes, and the intermittent time is 3-8 minute.Under above-mentioned suitable microwave irradiation power (being 200-500 watt) effect, can promote effective volatilization of essential oil, can avoid again producing burned smell and impurity, thereby guarantee the fine quality of lemon quintessence oil.In the present invention, the selection of time scope of each microwave radiation processing was advisable with 20 seconds-3 minutes; For the higher lemon pericarp fragment of water ratio, microwave irradiation time is slightly short; For the lower lemon pericarp fragment of water ratio, microwave irradiation time is slightly long.Preferably, in above-mentioned steps (2), the number of times of microwave radiation processing is 2-5 time.
Preferably, in above-mentioned steps (2), lemon pericarp fragment is placed in non-metallic container, then lemon pericarp fragment is placed in to microwave extracting apparatus together with non-metallic container.Above-mentioned non-metallic container can be Glass Containers (as flask, beaker), earthenware porcelain receptacle or plastic ware (container of making as polytetrafluoroethylmaterial material).For improving extraction efficiency, can multiple non-metallic containers that lemon pericarp fragment is housed be put into microwave extracting apparatus simultaneously.
Impurity in thick lemon quintessence oil is mainly pericarp wax.Preferably, in above-mentioned steps (3), by thick lemon quintessence oil cooling and standing 2-4 hour at 4-8 DEG C, refilter and remove impurity (being mainly pericarp wax).
The present invention adopts intermittent type microwave radiotreatment lemon pericarp fragment, adopt the fresh lemon pericarp of carry out microwave radiation heating or the dry lemon pericarp through moist curing, make Lemon fruit skin internal moisture Quick-gasifying, the essential oil of Lemon fruit intracutaneous is taken out of, after condensation, separation, obtain lemon quintessence oil.Compared with prior art, the present invention has following beneficial effect: (1) not with an organic solvent, lemon quintessence oil organic solvent-free is residual; (2) rate of heating is fast, lemon quintessence oil heated time is short, reduce lemon quintessence oil and at high temperature cause the reactions such as oxygenatedchemicals generation pyrolysis, hydrolysis, oxidation through long-time extraction, fragrance loss is few, there is green, the advantage such as quick and energy-conservation, and, certain hour intermittently between adjacent twice microwave radiation processing, make the cooling of lemon pericarp material, can avoid long microwave radiation to cause local temperature too high and destroy the quality of lemon quintessence oil, keep the natural quality of lemon quintessence oil; (3) intermittent type microwave radiation is less to the pollution of environment; (4) raw material is easy to get, and technique is simple, easy to operate, consumes energy low, and cost is low, and efficiency is high, pollution-free, is easy to the marketization and industrial production.Lemon quintessence oil extraction yield of the present invention is up to 2.23%, and the lemon quintessence oil making is transparent liquid faint yellow, that have citris aromas, and quality better, purity are high, can be widely used in the fields such as food, makeup, medicine.
Embodiment
Embodiment 1
In the present embodiment, the solvent-free extracting method of lemon quintessence oil comprises the steps: successively
(1) raw materials pretreatment: clean lemon dry fruit skin, with pulverizing after water-wet, is obtained to lemon pericarp fragment; The water ratio of above-mentioned lemon pericarp fragment is 26%(weight);
(2) the lemon pericarp fragment 200 grams of steps (1) being obtained is placed in microwave extracting apparatus (can be placed into flask by lemon pericarp fragment, again lemon pericarp fragment is placed in to microwave extracting apparatus together with flask), lemon pericarp fragment is applied to microwave radiation, collect the essential oil steam the condensation that produce, obtain thick lemon quintessence oil;
The mode that applies microwave radiation is intermittent type, its process is: microwave radiation processing 2.5 minutes (power of microwave radiation is 250 watts), intermittently 6 minutes, microwave radiation processing 2.5 minutes (power of microwave radiation is 250 watts) again, intermittently 6 minutes, microwave radiation processing 2.5 minutes (power of microwave radiation is 250 watts) again, intermittently 6 minutes, microwave radiation processing 2.5 minutes (power of microwave radiation is 250 watts) again, intermittently 6 minutes, then microwave radiation processing 2.5 minutes (power of microwave radiation is 250 watts);
In this step (2), the temperature in microwave extracting apparatus is controlled at 108-112 DEG C.
(3) isolate the impurity in thick lemon quintessence oil, obtain lemon quintessence oil.
In this step (3), by thick lemon quintessence oil at 5 DEG C cooling and standing 3 hours, refilter and remove impurity (being mainly pericarp wax).
The present embodiment gained lemon quintessence oil is light yellow transparent liquid, has obvious citris aromas, and through measuring and calculating, its extraction yield is 2.23%, and acid number is 0.12, and peroxide value is 3.13mmol/kg.
Embodiment 2
In the present embodiment, the solvent-free extracting method of lemon quintessence oil comprises the steps: successively
(1) raw materials pretreatment: clean lemon dry fruit skin, with pulverizing after water-wet, is obtained to lemon pericarp fragment; The water ratio of above-mentioned lemon pericarp fragment is 35%(weight);
(2) the lemon pericarp fragment 40 grams of steps (1) being obtained is placed in microwave extracting apparatus (can be placed into flask by lemon pericarp fragment, again lemon pericarp fragment is placed in to microwave extracting apparatus together with flask), lemon pericarp fragment is applied to microwave radiation, collect the essential oil steam the condensation that produce, obtain thick lemon quintessence oil;
The mode that applies microwave radiation is intermittent type, its process is: microwave radiation processing 40 seconds (power of microwave radiation is 360 watts), intermittently 5 minutes, microwave radiation processing 60 seconds (power of microwave radiation is 360 watts) again, intermittently 6 minutes, then microwave radiation processing 80 seconds (power of microwave radiation is 360 watts);
In this step (2), the temperature in microwave extracting apparatus is controlled at 108-112 DEG C.
(3) isolate the impurity in thick lemon quintessence oil, obtain lemon quintessence oil.
In this step (3), by thick lemon quintessence oil at 5 DEG C cooling and standing 2.5 hours, refilter and remove impurity (being mainly pericarp wax).
The present embodiment gained lemon quintessence oil is light yellow transparent liquid, has obvious citris aromas, and through measuring and calculating, its extraction yield is 1.73%, and acid number is 0.14, and peroxide value is 4.02mmol/kg.
Embodiment 3
In the present embodiment, the solvent-free extracting method of lemon quintessence oil comprises the steps: successively
(1) raw materials pretreatment: clean fresh lemon pericarp is pulverized, obtained lemon pericarp fragment; The water ratio of above-mentioned lemon pericarp fragment is 42%(weight).
(2) the lemon pericarp fragment 40 grams of steps (1) being obtained is placed in microwave extracting apparatus (can be placed into flask by lemon pericarp fragment, again lemon pericarp fragment is placed in to microwave extracting apparatus together with flask), lemon pericarp fragment is applied to microwave radiation, collect the essential oil steam the condensation that produce, obtain thick lemon quintessence oil;
The mode that applies microwave radiation is intermittent type, its process is: microwave radiation processing 90 seconds (power of microwave radiation is 360 watts), intermittently 4 minutes, microwave radiation processing 30 seconds (power of microwave radiation is 400 watts) again, intermittently 5 minutes, then microwave radiation processing 20 seconds (power of microwave radiation is 500 watts);
In this step (2), the temperature in microwave extracting apparatus is controlled at 105-110 DEG C.
(3) isolate the impurity in thick lemon quintessence oil, obtain lemon quintessence oil.
In this step (3), by thick lemon quintessence oil at 6 DEG C cooling and standing 2 hours, refilter and remove impurity (being mainly pericarp wax).
The present embodiment gained lemon quintessence oil is light yellow transparent liquid, has obvious citris aromas, and through measuring and calculating, its extraction yield is 2.18%, and acid number is 0.15, and peroxide value is 4.11mmol/kg.
Embodiment 4
In the present embodiment, the solvent-free extracting method of lemon quintessence oil comprises the steps: successively
(1) raw materials pretreatment: clean lemon dry fruit skin, with pulverizing after water-wet, is obtained to lemon pericarp fragment; The water ratio of above-mentioned lemon pericarp fragment is 68%(weight).
(2) the lemon pericarp fragment 80 grams of steps (1) being obtained is placed in microwave extracting apparatus (can be placed into flask by lemon pericarp fragment, again lemon pericarp fragment is placed in to microwave extracting apparatus together with flask), lemon pericarp fragment is applied to microwave radiation, collect the essential oil steam the condensation that produce, obtain thick lemon quintessence oil;
The mode that applies microwave radiation is intermittent type, its process is: microwave radiation processing 50 seconds (power of microwave radiation is 300 watts), intermittently 5 minutes, microwave radiation processing 50 seconds (power of microwave radiation is 300 watts) again, intermittently 5 minutes, microwave radiation processing 50 seconds (power of microwave radiation is 300 watts) again, intermittently 5 minutes, then microwave radiation processing 50 seconds (power of microwave radiation is 300 watts);
In this step (2), the temperature in microwave extracting apparatus is controlled at 90-95 DEG C.
(3) isolate the impurity in thick lemon quintessence oil, obtain lemon quintessence oil.
In this step (3), by thick lemon quintessence oil at 5 DEG C cooling and standing 2.5 hours, refilter and remove impurity (being mainly pericarp wax).
The present embodiment gained lemon quintessence oil is yellow transparent liquid, has obvious citris aromas, and through measuring and calculating, its extraction yield is 2.08%, and acid number is 0.18, and peroxide value is 4.22mmol/kg.
Embodiment 5
In the present embodiment, the solvent-free extracting method of lemon quintessence oil comprises the steps: successively
(1) raw materials pretreatment: clean fresh lemon pericarp is pulverized, obtained lemon pericarp fragment; The water ratio of above-mentioned lemon pericarp fragment is 42%(weight).
(2) lemon pericarp fragment step (1) being obtained is placed in microwave extracting apparatus (can be placed into flask by lemon pericarp fragment, again lemon pericarp fragment is placed in to microwave extracting apparatus together with flask), lemon pericarp fragment is applied to microwave radiation, collect the essential oil steam the condensation that produce, obtain thick lemon quintessence oil;
The mode that applies microwave radiation is intermittent type, its process is: microwave radiation processing 30 seconds (power of microwave radiation is 400 watts), intermittently 5 minutes, microwave radiation processing 30 seconds (power of microwave radiation is 400 watts) again, intermittently 5 minutes, then microwave radiation processing 30 seconds (power of microwave radiation is 400 watts);
In this step (2), the temperature in microwave extracting apparatus is controlled at 115-120 DEG C.
(3) isolate the impurity in thick lemon quintessence oil, obtain lemon quintessence oil.
In this step (3), by thick lemon quintessence oil at 8 DEG C cooling and standing 4 hours, refilter and remove impurity (being mainly pericarp wax).
The present embodiment gained lemon quintessence oil is light yellow transparent liquid, has obvious citris aromas, and through measuring and calculating, its extraction yield is 2.01%, and acid number is 0.17, and peroxide value is 4.45mmol/kg.
In above-described embodiment 1-5, also can substitute flask with other non-metallic container and carry out splendid attire lemon pericarp fragment, as beaker, earthenware porcelain receptacle, plastic ware (container of making as polytetrafluoroethylmaterial material) etc.; Or directly lemon pericarp fragment is placed in to microwave extracting apparatus.
In above embodiment 1-5:
Extraction yield=(essential oil quality/lemon pericarp dry mass) × 100%.
The method of test lemon quintessence oil fragrance is: lemon quintessence oil sample is poured in 150mL beaker, and water-bath is slowly heated to 5min, utilizes glass stick to stir rapidly, smells the smell that it volatilizes.
Acid number method of calculation are: demarcate the free fatty acids in lemon quintessence oil with potassium hydroxide standardized solution, every gram of lemon quintessence oil can consume the amount of substance of potassium hydroxide.Country-level standard: acid number≤0.2.
Peroxide value method of calculation are volumetrys: the superoxide that lemon quintessence oil grease produces in oxidising process, superoxide and potassiumiodide effect generate free-iodine, then use the sodium thiosulfate solution titrated of preparation, calculate its content.Country-level standard: peroxide value≤5.0mmol/kg.
Claims (7)
1. a solvent-free extracting method for lemon quintessence oil, is characterized in that comprising the steps: successively
(1) raw materials pretreatment: clean fresh lemon pericarp is pulverized, or by clean lemon dry fruit skin with pulverizing after water-wet, obtain lemon pericarp fragment;
(2) lemon pericarp fragment step (1) being obtained is placed in microwave extracting apparatus, and lemon pericarp fragment is applied to microwave radiation, collects the essential oil steam the condensation that produce, obtains thick lemon quintessence oil;
The mode that applies microwave radiation is intermittent type, and its process is: carry out after a microwave radiation processing intermittently, then carry out microwave radiation processing next time, repeat operation, carry out repeatedly microwave radiation processing;
(3) isolate the impurity in thick lemon quintessence oil, obtain lemon quintessence oil.
2. the solvent-free extracting method of lemon quintessence oil according to claim 1, is characterized in that: in described step (2), the power of microwave radiation is 200-500 watt, and the time of each microwave radiation processing is 20 seconds-3 minutes, and the intermittent time is 3-8 minute.
3. the solvent-free extracting method of lemon quintessence oil according to claim 1 and 2, is characterized in that: in described step (2), the number of times of microwave radiation processing is 2-5 time.
4. the solvent-free extracting method of lemon quintessence oil according to claim 1 and 2, is characterized in that: in described step (1), the water ratio of lemon pericarp fragment is 20-70%(weight).
5. the solvent-free extracting method of lemon quintessence oil according to claim 1 and 2, is characterized in that: in described step (2), the temperature in microwave extracting apparatus is controlled at 90-120 DEG C.
6. the solvent-free extracting method of lemon quintessence oil according to claim 1 and 2, it is characterized in that: in described step (2), lemon pericarp fragment is placed in non-metallic container, then lemon pericarp fragment is placed in to microwave extracting apparatus together with non-metallic container.
7. the solvent-free extracting method of lemon quintessence oil according to claim 1 and 2, is characterized in that: in described step (3), by thick lemon quintessence oil cooling and standing 2-4 hour at 4-8 DEG C, refilter and remove impurity.
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| CN105647649A (en) * | 2016-03-31 | 2016-06-08 | 李颖 | Preparation method and device using microwave and gravity to extract natural plant essential oil and hydrolat |
| CN105713726A (en) * | 2016-03-31 | 2016-06-29 | 李颖 | Method and device for rapidly extracting natural plant essential oil and hydrolat without solvents |
| CN106281704A (en) * | 2016-08-26 | 2017-01-04 | 广西灏源盛世生物科技有限公司 | A kind of extracting method of Fructus Citri Limoniae quintessence oil |
| CN111448290A (en) * | 2017-12-20 | 2020-07-24 | 盐田生命科学株式会社 | Method for producing antioxidant or hair growth promoter, and antioxidant or hair growth promoter produced by the production method |
| CN112980585A (en) * | 2021-03-26 | 2021-06-18 | 江西科技师范大学 | Method for extracting orange peel essential oil |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105219526A (en) * | 2015-09-25 | 2016-01-06 | 四川省林业科学研究院 | A kind of yusho oil microwave extraction device and method |
| CN105647649A (en) * | 2016-03-31 | 2016-06-08 | 李颖 | Preparation method and device using microwave and gravity to extract natural plant essential oil and hydrolat |
| CN105713726A (en) * | 2016-03-31 | 2016-06-29 | 李颖 | Method and device for rapidly extracting natural plant essential oil and hydrolat without solvents |
| CN106281704A (en) * | 2016-08-26 | 2017-01-04 | 广西灏源盛世生物科技有限公司 | A kind of extracting method of Fructus Citri Limoniae quintessence oil |
| CN111448290A (en) * | 2017-12-20 | 2020-07-24 | 盐田生命科学株式会社 | Method for producing antioxidant or hair growth promoter, and antioxidant or hair growth promoter produced by the production method |
| 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 |
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