CN103897805B - A kind of solvent-free extracting method of lemon - Google Patents
A kind of solvent-free extracting method of lemon Download PDFInfo
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- CN103897805B CN103897805B CN201410133030.XA CN201410133030A CN103897805B CN 103897805 B CN103897805 B CN 103897805B CN 201410133030 A CN201410133030 A CN 201410133030A CN 103897805 B CN103897805 B CN 103897805B
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Abstract
A solvent-free extracting method for lemon, comprises the steps: that (1) pulverize clean fresh lemon pericarp successively, or by clean lemon dry fruit skin with pulverizing after water-wet, obtain lemon pericarp fragment; (2) lemon pericarp fragment is placed in to microwave extracting apparatus, lemon pericarp fragment is applied to microwave, collect the essential oil steam the condensation that produce, obtain thick lemon; The mode that applies microwave is batch (-type), and its process is: carry out after a microwave radiation processing intermittently, then carry out microwave radiation processing next time, repeat operation; (3) isolate the impurity in thick lemon, obtain lemon. Extracting method of the present invention has green, the advantage such as quick and energy-conservation, and less to the pollution of environment, raw material is easy to get, and technique is simple, easy to operate, consumes energy low, and cost is low, and efficiency is high; The lemon organic solvent-free making is residual, and quality better, purity are high, and keeps the natural quality of lemon.
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, under condition of no solvent, from lemon pericarp, extract the method for lemon.
Background technology
The bioactive ingredients natural environmental-protective extracting from plant, long-term use 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 cosmetics, plant source active component 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 active ingredient in plant extracts to carry out the research and development of cosmetics, 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 extracts 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 extracts 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, production 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 extracting from lemon pericarp, Nantural non-toxic side effect. The main chemical compositions of lemon is sobrerone or firpene, amphene, sabinene, bay (spiceleaf) alkene, dipentene, linalool, bisabolene, limonene, nerol and neral. Lemon, for cosmetics, 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, flat wart 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 that research is reclaimed in lemon pericarp is used for cosmetics, is a very promising technology.
Traditional method of extracting lemon 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 extract cost is high and technical requirement 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, this method is under condition of no solvent, from lemon pericarp, extract lemon by intermittent type microwave radiation effects, have technique simple, easy to operate, consume energy low, cost is low, efficiency advantages of higher, and the lemon quality better making. The technical scheme adopting is as follows:
A solvent-free extracting method for lemon, is characterized in that comprising the steps: successively
(1) pretreatment of raw material: 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, collects the essential oil steam the condensation that produce, obtains thick lemon;
The mode that applies microwave is batch (-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, obtain lemon.
Preferably, in above-mentioned steps (1), the moisture content 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 in step (2) is batch (-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 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. 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 moisture content, microwave irradiation time is slightly short; For the lower lemon pericarp fragment of moisture content, 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 nonmetallic vessel, then lemon pericarp fragment is placed in to microwave extracting apparatus together with nonmetallic vessel. Above-mentioned nonmetallic vessel can be glass container (as flask, beaker), ceramic vessel or plastic ware (container of making as polytetrafluoroethylmaterial material). For improving extraction efficiency, can multiple nonmetallic vessels that lemon pericarp fragment is housed be put into microwave extracting apparatus simultaneously.
Impurity in thick lemon is mainly pericarp wax. Preferably, in above-mentioned steps (3), by thick lemon 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 radiation treatment lemon pericarp fragment, adopt the fresh lemon pericarp of carry out microwave radiation heating or the dry lemon pericarp through wettability treatment, make Lemon fruit skin internal moisture Quick-gasifying, the essential oil of Lemon fruit intracutaneous is taken out of, after condensation, separation, obtain lemon. Compared with prior art, the present invention has following beneficial effect: (1) not with an organic solvent, lemon organic solvent-free is residual; (2) firing rate is fast, lemon heated time is short, reduce lemon 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 to cause local temperature too high and destroy the quality of lemon, keep the natural quality of lemon; (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 recovery rate of the present invention is up to 2.23%, and the lemon making is transparency liquid faint yellow, that have citris aromas, and quality better, purity are high, can be widely used in the fields such as food, cosmetics, medicine.
Detailed description of the invention
Embodiment 1
In the present embodiment, the solvent-free extracting method of lemon comprises the steps: successively
(1) pretreatment of raw material: clean lemon dry fruit skin, with pulverizing after water-wet, is obtained to lemon pericarp fragment; The moisture content 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, collect the essential oil steam the condensation that produce, obtain thick lemon;
The mode that applies microwave is batch (-type), its process is: microwave radiation processing 2.5 minutes (power of microwave is 250 watts), intermittently 6 minutes, microwave radiation processing 2.5 minutes (power of microwave is 250 watts) again, intermittently 6 minutes, microwave radiation processing 2.5 minutes (power of microwave is 250 watts) again, intermittently 6 minutes, microwave radiation processing 2.5 minutes (power of microwave is 250 watts) again, intermittently 6 minutes, then microwave radiation processing 2.5 minutes (power of microwave 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, obtain lemon.
In this step (3), by thick lemon at 5 DEG C cooling and standing 3 hours, refilter and remove impurity (being mainly pericarp wax).
The present embodiment gained lemon is light yellow transparent liquid, has obvious citris aromas, and through measuring and calculating, its recovery rate 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 comprises the steps: successively
(1) pretreatment of raw material: clean lemon dry fruit skin, with pulverizing after water-wet, is obtained to lemon pericarp fragment; The moisture content 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, collect the essential oil steam the condensation that produce, obtain thick lemon;
The mode that applies microwave is batch (-type), its process is: microwave radiation processing 40 seconds (power of microwave is 360 watts), intermittently 5 minutes, microwave radiation processing 60 seconds (power of microwave is 360 watts) again, intermittently 6 minutes, then microwave radiation processing 80 seconds (power of microwave 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, obtain lemon.
In this step (3), by thick lemon at 5 DEG C cooling and standing 2.5 hours, refilter and remove impurity (being mainly pericarp wax).
The present embodiment gained lemon is light yellow transparent liquid, has obvious citris aromas, and through measuring and calculating, its recovery rate 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 comprises the steps: successively
(1) pretreatment of raw material: clean fresh lemon pericarp is pulverized, obtained lemon pericarp fragment; The moisture content 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, collect the essential oil steam the condensation that produce, obtain thick lemon;
The mode that applies microwave is batch (-type), its process is: microwave radiation processing 90 seconds (power of microwave is 360 watts), intermittently 4 minutes, microwave radiation processing 30 seconds (power of microwave is 400 watts) again, intermittently 5 minutes, then microwave radiation processing 20 seconds (power of microwave 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, obtain lemon.
In this step (3), by thick lemon at 6 DEG C cooling and standing 2 hours, refilter and remove impurity (being mainly pericarp wax).
The present embodiment gained lemon is light yellow transparent liquid, has obvious citris aromas, and through measuring and calculating, its recovery rate 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 comprises the steps: successively
(1) pretreatment of raw material: clean lemon dry fruit skin, with pulverizing after water-wet, is obtained to lemon pericarp fragment; The moisture content 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, collect the essential oil steam the condensation that produce, obtain thick lemon;
The mode that applies microwave is batch (-type), its process is: microwave radiation processing 50 seconds (power of microwave is 300 watts), intermittently 5 minutes, microwave radiation processing 50 seconds (power of microwave is 300 watts) again, intermittently 5 minutes, microwave radiation processing 50 seconds (power of microwave is 300 watts) again, intermittently 5 minutes, then microwave radiation processing 50 seconds (power of microwave 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, obtain lemon.
In this step (3), by thick lemon at 5 DEG C cooling and standing 2.5 hours, refilter and remove impurity (being mainly pericarp wax).
The present embodiment gained lemon is yellow transparent liquid, has obvious citris aromas, and through measuring and calculating, its recovery rate 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 comprises the steps: successively
(1) pretreatment of raw material: clean fresh lemon pericarp is pulverized, obtained lemon pericarp fragment; The moisture content 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, collect the essential oil steam the condensation that produce, obtain thick lemon;
The mode that applies microwave is batch (-type), its process is: microwave radiation processing 30 seconds (power of microwave is 400 watts), intermittently 5 minutes, microwave radiation processing 30 seconds (power of microwave is 400 watts) again, intermittently 5 minutes, then microwave radiation processing 30 seconds (power of microwave 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, obtain lemon.
In this step (3), by thick lemon at 8 DEG C cooling and standing 4 hours, refilter and remove impurity (being mainly pericarp wax).
The present embodiment gained lemon is light yellow transparent liquid, has obvious citris aromas, and through measuring and calculating, its recovery rate 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 nonmetallic vessel and carry out splendid attire lemon pericarp fragment, as beaker, ceramic vessel, 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:
Recovery rate=(essential oil quality/lemon pericarp dry mass) × 100%.
The method of test lemon fragrance is: lemon sample is poured in 150mL beaker, and water-bath is slowly heated to 5min, utilizes glass bar to stir rapidly, smells the smell that it volatilizes.
Acid number computational methods are: demarcate the free fatty in lemon with potassium hydroxide standard liquid, every gram of lemon can consume the amount of substance of potassium hydroxide. Country-level standard: acid number≤0.2.
Peroxide value computational methods are titrations: the peroxide that lemon grease produces in oxidizing process, peroxide and KI 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 (1)
1. a solvent-free extracting method for lemon, is characterized in that comprising the steps: successively
(1) pretreatment of raw material: clean lemon dry fruit skin, with pulverizing after water-wet, is obtained to lemon pericarp fragment; The moisture content of above-mentioned lemon pericarp fragment is 26wt%;
(2) the lemon pericarp fragment 200 grams of steps (1) being obtained is placed in microwave extracting apparatus, and lemon pericarp fragment is applied to microwave, collects the essential oil steam the condensation that produce, obtains thick lemon;
In this step (2), lemon pericarp fragment is placed in flask, then lemon pericarp fragment is placed in to microwave extracting apparatus together with flask;
The mode that applies microwave is batch (-type), its process is: microwave radiation processing 2.5 minutes, the power of microwave is 250 watts, then 6 minutes intermittences, microwave radiation processing 2.5 minutes again, the power of microwave is 250 watts, then at 2.5 minutes 6 minutes intermittences, then microwave radiation processing, the power of microwave is 250 watts, then 6 minutes intermittences, microwave radiation processing 2.5 minutes again, the power of microwave is 250 watts, then 6 minutes intermittences, microwave radiation processing 2.5 minutes again, the power of microwave 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, obtain lemon;
In this step (3), by thick lemon at 5 DEG C cooling and standing 3 hours, refilter and remove impurity.
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| 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 |
| CN105713726A (en) * | 2016-03-31 | 2016-06-29 | 李颖 | Method and device for rapidly extracting natural plant essential oil and hydrolat without solvents |
| 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 |
| 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 |
| CN111448290B (en) * | 2017-12-20 | 2022-06-24 | 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 |
| 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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