CN105713730B - Extracting method of citrus essential oil - Google Patents
Extracting method of citrus essential oil Download PDFInfo
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- CN105713730B CN105713730B CN201610121908.7A CN201610121908A CN105713730B CN 105713730 B CN105713730 B CN 105713730B CN 201610121908 A CN201610121908 A CN 201610121908A CN 105713730 B CN105713730 B CN 105713730B
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- 241000207199 Citrus Species 0.000 title claims abstract description 66
- 235000020971 citrus fruits Nutrition 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims abstract description 45
- 239000000341 volatile oil Substances 0.000 title claims abstract description 34
- 238000000605 extraction Methods 0.000 claims abstract description 78
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims abstract description 58
- 239000000284 extract Substances 0.000 claims abstract description 41
- 239000000843 powder Substances 0.000 claims abstract description 41
- 235000007586 terpenes Nutrition 0.000 claims abstract description 39
- XMGQYMWWDOXHJM-UHFFFAOYSA-N limonene Chemical compound CC(=C)C1CCC(C)=CC1 XMGQYMWWDOXHJM-UHFFFAOYSA-N 0.000 claims abstract description 28
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003960 organic solvent Substances 0.000 claims abstract description 17
- 235000001510 limonene Nutrition 0.000 claims abstract description 14
- 229940087305 limonene Drugs 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000005684 electric field Effects 0.000 claims abstract description 10
- 150000003505 terpenes Chemical class 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 239000003921 oil Substances 0.000 claims description 43
- 235000019198 oils Nutrition 0.000 claims description 43
- 238000001556 precipitation Methods 0.000 claims description 18
- 241001672694 Citrus reticulata Species 0.000 claims description 16
- -1 terpene compound Chemical class 0.000 claims description 11
- 235000019476 oil-water mixture Nutrition 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 239000001273 butane Substances 0.000 claims description 7
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 claims description 7
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 7
- 229910018503 SF6 Inorganic materials 0.000 claims description 6
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 claims description 6
- 229960000909 sulfur hexafluoride Drugs 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims 1
- 238000000638 solvent extraction Methods 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 8
- 239000007788 liquid Substances 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- NNPPMTNAJDCUHE-UHFFFAOYSA-N trimethylmethane Natural products CC(C)C NNPPMTNAJDCUHE-UHFFFAOYSA-N 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract 1
- 238000009210 therapy by ultrasound Methods 0.000 abstract 1
- 239000002904 solvent Substances 0.000 description 13
- 239000004519 grease Substances 0.000 description 10
- 239000003205 fragrance Substances 0.000 description 9
- 238000002156 mixing Methods 0.000 description 9
- 238000002137 ultrasound extraction Methods 0.000 description 8
- 238000009833 condensation Methods 0.000 description 5
- 230000005494 condensation Effects 0.000 description 5
- 230000006837 decompression Effects 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000002309 gasification Methods 0.000 description 5
- 239000000523 sample Substances 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 239000006187 pill Substances 0.000 description 4
- 238000013517 stratification Methods 0.000 description 4
- 150000001299 aldehydes Chemical class 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- 238000002386 leaching Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000004448 titration Methods 0.000 description 3
- 238000003809 water extraction Methods 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 239000002537 cosmetic Substances 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000199 molecular distillation Methods 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 238000000194 supercritical-fluid extraction Methods 0.000 description 2
- 238000005292 vacuum distillation Methods 0.000 description 2
- 235000019499 Citrus oil Nutrition 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000010500 citrus oil Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000013355 food flavoring agent Nutrition 0.000 description 1
- 238000004508 fractional distillation Methods 0.000 description 1
- 210000004907 gland Anatomy 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 239000003495 polar organic solvent Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
- 230000003248 secreting effect Effects 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 230000008542 thermal sensitivity Effects 0.000 description 1
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
- 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
- C11B9/022—Refining
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to the technical field of bioseparation and particularly discloses an extracting method of citrus essential oil. The method comprises the following steps that citrus peels are dried in the shade and smashed into powder, an extracting agent composed of dimethyl ether and ethane is added, and the mixture is extracted ultrasonically; the feed liquid mixture subjected to ultrasonic treatment is placed into a high-voltage pulse electric field to be extracted; the feed liquid mixture subjected to treatment in the high-voltage pulse electric field is subjected to subcritical extraction with organic solvent and water as extracting agents, and the extracting agents are removed, so that the citrus terpene removal essential oil is obtained. According to the extracting method of the citrus essential oil, in the extracting process, the required temperature and pressure are low, it can be ensured that aroma components in the essential oil are not damaged while the good terpene substance removal effect is achieved, the essential oil extracting yield is high, the technology is simple, and the equipment cost is low; the extract liquor obtained after subcritical solvent extraction has recycling value and can be widely used for preparing limonene.
Description
Technical field
The present invention relates to technical field of bioseparation, more particularly to a kind of extracting method of Citrus essential oil.
Background technology
Citrus essential oil is present in peel of Citrus reticulata Blanco or Citrus secreting gland, is the significant by-products of Citrus procession, with Citrus day
So, pure and fresh pleasant fragrance, is widely used in the production of food, flavoring agent, medicine, cosmetics and beverage.Its main component
It is terpene compound, accounts for more than the 90% of Citrus essential oil total amount, the wherein content of limonene at most, can be used as cosmetic, soap
And household chemicalss essence, but which contributes less to mandarin orange fragrance, and quality that is oxidizable rotten and reducing quintessence oil；Aldehydes, alcohol
Class, lipid and ketone equal size are less than 5%, are but the main sources of Citrus essential oil fragrance.Organic solvent is adopted in production typically
Extraction, vacuum distillation, molecular distillation, continuous countercurrent technique, solvent extraction and supercritical extraction etc. are smart to obtain the de- terpene of Citrus
Oil.Vacuum distillation and molecular distillation are carried out at high temperature so that in quintessence oil, thermal sensitivity fragrance component decomposes, and reduce quintessence oil quality；
Continuous countercurrent technique removes the less efficient of terpene compound, and contributes larger aldehydes to be also removed Citrus essential oil fragrance
, affect quintessence oil quality；Supercritical extraction operating pressure is big, high to equipment requirements, relatively costly, it is difficult to large-scale production；One
As to extract the conventional method of the de- terpene quintessence oil of Citrus in production be organic solvent extraction, the quintessence oil yield that the method is obtained is high, takes off terpene
Effect is good, and pigment is few, has the disadvantage that the solvent residual amount of quintessence oil is higher, and extraction time is long, and trivial operations, efficiency are low.
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 Citrus essential oil extracts yield
Height, fragrance component loss is less and because going terpene Citrus essence containing the subcritical fluid extraction that terpene compound is few, product quality is stable
The method of oil.
To solve above-mentioned technical problem, there is provided a kind of extracting method of Citrus essential oil, comprise the following steps：
(1) peel of Citrus reticulata Blanco is dried in the shade, is ground into powder, added the extractant of dimethyl ether and organic solvent composition, carry out ultrasound
Extraction obtains sonicated extract；
(2) sonicated extract is carried out into high-voltage pulse extraction and obtains high-voltage pulse extract；
(3) the high-voltage pulse extract is carried out into subcritical abstraction and obtains miscella and Citrus powder for 1～3 time；
(4) by the Citrus powder, subcritical abstraction 1～3 time is carried out by extractant of water, obtain oil water mixture；
(5) oil water mixture is stood, is layered profit, oil phase is Citrus essential oil.
Above-mentioned extracting method, it is preferred that peel of Citrus reticulata Blanco described in the step (1) is surpassed for 10 DEG C in ﹣ using super micron mill
Crushing of Ultrafine 5min～30min, obtains powder, and the particle diameter of the powder is 1mm～10mm.
Above-mentioned extracting method, it is preferred that powder with the mass volume ratio of the extractant is described in the step (1)
1g: 8mL～1g: 25mL.
Above-mentioned extracting method, it is preferred that current intensity 1.0A/25w of the supersound extraction～1.5A/275w, ultrasound
Extraction time is 10～15min.
Above-mentioned extracting method, it is preferred that the extractant of the dimethyl ether of the step (1) and organic solvent composition
In, organic solvent and dimethyl ether volume ratio are 1: 1～15: 1.
Above-mentioned extracting method, it is preferred that organic solvent described in the step (1) is ethane, sulfur hexafluoride and butane
In one kind.
Above-mentioned extracting method, it is preferred that in the step (2), the electric field intensity in the high-voltage pulse extraction process
20KV/cm～50KV/cm, 400 μ s～600 μ s of burst length, pulse frequency 200Hz～450Hz；The extraction time is
15min～40min.
Above-mentioned extracting method, it is preferred that the subcritical abstraction of the step (3) is specially：By the high-tension pulse
The batch extractor that extract is added to subcritical abstraction equipment is rushed, 3h～12h is infiltrated；Then extracting pressure be 0.2Mpa～
6Mpa, extraction temperature obtain miscella and Citrus powder to carry out subcritical abstraction 0.1h～2h under conditions of 15 DEG C～60 DEG C.
Above-mentioned extracting method, it is preferred that mix oil extract limonene, concrete extracting method described in the step (3)
For：By the miscella, steam oil tank is imported, ﹣ 0.08MPa precipitations is decompressed to and is obtained terpene compound, by the terpene compound
It is placed in depressurized system, is 85 DEG C in temperature, pressure is 4KPa environment, under pressure fractional distillation, collects fraction, obtains limonene.
Above-mentioned extracting method, it is preferred that during the step (4) subcritical abstraction, extracting pressure is
0.2Mpa～6Mpa, extraction temperature are 15 DEG C～60 DEG C, and extraction time is 0.1h～2h.
Above-mentioned extracting method, it is preferred that during the step (4) subcritical abstraction, Citrus powder and water
Volume ratio is 1: 5～20.
Compared with prior art, it is an advantage of the current invention that：
(1) the invention provides a kind of extracting method of Citrus essential oil, by high-voltage pulse electric field technology, ultrasound assisted extraction technique
It is combined with sub-critical extraction technology, not only increases the leaching rate of effective ingredient, effectively removes in Citrus essential oil
Terpenoid substance, and pigment residue is less, the method provided using the present invention reaches can the de- terpene rate of Citrus essential oil
93.26%, improve the purity of quintessence oil.Meanwhile, the present invention extracts quintessence oil under lower temperature and pressure, is conducive to keeping Citrus
Quintessence oil fresh degree of fragrance, and flow process is simple, extraction time is short, and energy resource consumption is relatively low, is easy to industrialized production, before good market
Scape.
(2) the invention provides a kind of extracting method of Citrus essential oil, using low-temperature grinding, not only can improve peel of Citrus reticulata Blanco
The extraction ratio of effective ingredient, while avoiding because of the loss for crushing the high temperature for producing to peel of Citrus reticulata Blanco effective ingredient.
(3) the invention provides a kind of extracting method of Citrus essential oil, the extractant for being constituted with dimethyl ether and ethane first
Extracted, then extracted using ultrasonic in combination high-pressure pulse electric, drastically increase de- terpene efficiency.
(4) the invention provides a kind of extracting method of Citrus essential oil, it is extractant to carrying with dimethyl ether and organic solvent
Taking liquid carries out subcritical abstraction, and the subcritical abstraction advantage time is shorter, and extraction temperature is low, can protective ingredient be not destroyed, extract
Efficiency high；Compared with subcritical, the pressure that supercritical needs is much bigger, and energy expenditure is big.Dimethyl ether has low pole, has excellent
Compatibility, can be miscible with most of polarity and non-polar organic solvent, organic solvent be preferably ethane, sulfur hexafluoride or fourth
Alkane, the ethane of present invention employing, sulfur hexafluoride, dimethyl ether equal solvent low boiling point are gas, at reduced pressure conditions, essence under room temperature
In oil, solvent is more easy to removing, and in finished product quintessence oil, total solvent residual is less than 30ppm；Solvent recovery, can be recycled, will not be to environment
Pollute；Extract can be further purified, and extract limonene, reduce wastage of material.
(5) the invention provides a kind of extracting method of Citrus essential oil, in peel of Citrus reticulata Blanco alcohols, aldehydes and ketone isopolarity into
Divide fragrance threshold value low, it is big to the contribution of quintessence oil fragrance, and water is polar substancess, carries out second subcritical extraction by extractant of water
Take, the polar component in peel of Citrus reticulata Blanco can effectively be extracted.
Description of the drawings
To make purpose, technical scheme and the advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention
In accompanying drawing, clear, complete description is carried out to the technical scheme in the embodiment of the present invention.
Extraction flow charts of the Fig. 1 for Citrus essential oil.
Specific embodiment
Below in conjunction with Figure of description and concrete preferred embodiment, the invention will be further described, but not therefore and
Limit the scope of the invention.
Embodiment
Material and instrument employed in following examples is commercially available.
Embodiment 1
Referring to Fig. 1, a kind of extracting method of the Citrus essential oil of the present invention, following steps are specifically included：
(1) take 200g drying peel of Citrus reticulata Blanco, using super micron mill in the case where 10 DEG C of ﹣ micronizing 5min, obtaining particle diameter is
The powder of 2mm.
(2) powder of step (1) is placed in pill tank, by 1g: 15mL addition extractant, (extractant is ethane and diformazan
The mixed solution of ether, wherein ethane and dimethyl ether volume ratio are 8: 1), when being slowly stirred with probe type ultrasonic extraction apparatus in electricity
Supersound extraction 15min is carried out under the conditions of intensity of flow 1.2A/45w and obtains sonicated extract.
(3) sonicated extract in step (2) is placed in into high-pressure pulse electric, electric field intensity 25KV/cm is set, during pulse
Between 500 μ s, pulse frequency 240Hz, extract 20min, obtain high-voltage pulse extract.
(4) the high-voltage pulse extract in the step of taking 3L (3) is added to the 5L batch extractors of subcritical abstraction complete set of equipments
In, infiltrate 3h (infiltrating time can be implemented for 3h～12h)；It is 0.6Mpa in extracting pressure, extraction temperature is 30 DEG C, during extraction
Between to carry out subcritical solvent extraction under conditions of 45min, obtain miscella and Citrus powder.
(5) miscella taken in step (4) is imported in precipitation tank, and being decompressed to ﹣ 0.08MPa carries out precipitation tank decompression separation,
It is terpene compound to obtain grease.Grease is inserted in depressurized system, 85 DEG C of temperature, pressure is 4KPa, collects fraction,
Obtain limonene；Organic solvent after gasification is compressed, after condensation liquefaction, collect solvent, and tank is recycled.
(6) the Citrus powder in step (4) is taken, is added the water of 8 times of volumes as extractant, is carried out Subcritical Water Extraction,
Setting extracting pressure is 0.5Mpa, and extraction temperature is 40 DEG C, and extraction time is 30min, obtains oil water mixture.
(7) repeat step (6) 2 times, after extracting every time are transferred to extract in precipitation tank, are decompressed to normal pressure, by gained
Extract stratification, oil phase are the de- terpene quintessence oil of Citrus, and yield is 4.21%, and it is 93.26% to take off terpene rate.
Embodiment 2
Referring to Fig. 1, a kind of extracting method of the Citrus essential oil of the present invention, comprise the steps：
(1) take 200g drying peel of Citrus reticulata Blanco, using super micron mill in the case where 10 DEG C of ﹣ micronizing 5min, obtaining particle diameter is
The powder of 2mm.
(2) powder of step (1) is placed in pill tank, by 1g: 10mL addition extractant, (extractant is ethane and diformazan
The mixed solution of ether, wherein ethane and dimethyl ether volume ratio are 8: 1), when being slowly stirred with probe type ultrasonic extraction apparatus in electricity
Supersound extraction 10min is carried out under the conditions of intensity of flow 1A/25w and obtains sonicated extract.
(3) sonicated extract in step (2) is placed in into high-pressure pulse electric, electric field intensity 25KV/cm is set, during pulse
Between 500 μ s, pulse frequency 240Hz, extraction time 20min obtain high-voltage pulse extract.
(4) the high-voltage pulse extract in the step of taking 3L step (3) is added to the 5L leachings of subcritical abstraction complete set of equipments
Go out in tank, infiltrate 3h；Then extracting pressure be 5Mpa, extraction temperature be 50 DEG C, extraction time be 30min under the conditions of carry out Asia
Critical solvent is extracted, and obtains miscella and Citrus powder.
(5) miscella taken in step (4) is imported in precipitation tank, and being decompressed to ﹣ 0.08MPa carries out precipitation tank decompression separation,
It is terpene compound to obtain grease.Grease is inserted in depressurized system, 85 DEG C of temperature, pressure is 4KPa, collects fraction,
Obtain limonene；Organic solvent after gasification is compressed, after condensation liquefaction, collect solvent, and tank is recycled.
(6) the Citrus powder in step (4) is taken, is added the water of 8 times of volumes as extractant, is carried out subcritical abstraction, if
It is 1.5Mpa to put extracting pressure, and extraction temperature is 50 DEG C, and extraction time is 20min, that is, obtain oil water mixture.
(7) repeat step (6) 2 times, after extracting every time are transferred to extract in precipitation tank, are decompressed to normal pressure, by gained
Extract stratification, oil phase are the de- terpene quintessence oil of Citrus, and yield is 3.47%, and it is 84.63% to take off terpene rate.
Embodiment 3
Referring to Fig. 1, a kind of extracting method of the Citrus essential oil of the present invention, comprise the steps：
(1) take 200g drying peel of Citrus reticulata Blanco, using super micron mill in the case where 10 DEG C of ﹣ micronizing 5min, obtaining particle diameter is
The powder of 2mm.
(2) powder of step (1) is placed in the 5L batch extractors of subcritical abstraction complete set of equipments, is extracted by 1g: 10mL addition
(extractant is that the mixed solution of ethane and dimethyl ether, wherein ethane and dimethyl ether volume ratio are 8: 1), infiltrates 3h to take agent；Then
It is 15Mpa in extracting pressure, extraction temperature is 40 DEG C, carries out subcritical solvent extraction, obtain miscella under the conditions of extraction 30min
With Citrus powder.
(3) miscella taken in step (2) is imported in precipitation tank, and being decompressed to ﹣ 0.08MPa carries out precipitation tank decompression separation,
It is terpene compound to obtain grease.Grease is inserted in depressurized system, 85 DEG C of temperature, pressure is 4KPa, collects fraction,
Obtain limonene；Organic solvent after gasification is compressed, after condensation liquefaction, collect solvent, and tank is recycled.
(4) the Citrus powder in step (2) is taken, is added the water of 8 times of volumes as extractant, is carried out subcritical abstraction, if
It is 5Mpa to put extracting pressure, and extraction temperature is 60 DEG C, and extraction time obtains oil water mixture for 50min.
(5) repeat step (4) 2 times, after extracting every time are transferred to extract in precipitation tank, are decompressed to normal pressure, by gained
Extract stratification, oil phase are the de- terpene quintessence oil of Citrus, and yield is 2.59%, and it is 73.40% to take off terpene rate.
Embodiment 4
Referring to Fig. 1, the impact that extractant is extracted to Citrus essential oil is investigated：
(1) take dry peel of Citrus reticulata Blanco, using super micron mill in the case where 10 DEG C of ﹣ micronizing 5min, obtain particle diameter for 2mm
Powder.
(2) every part of powder 200g is taken, and extractant 1～7 is separately added into by 1g: 8mL addition：
Extractant 1：Butane and dimethyl ether are 4: 1 mixing according to volume ratio.
Extractant 2：Butane and dimethyl ether are 8: 1 mixing according to volume ratio.
Extractant 3：Butane and dimethyl ether are 16: 1 mixing according to volume ratio.
Extractant 4：Sulfur hexafluoride and dimethyl ether are 4: 1 mixing according to volume ratio.
Extractant 5：Sulfur hexafluoride and dimethyl ether are 8: 1 mixing according to volume ratio.
Extractant 6：Ethane and dimethyl ether are 4: 1 mixing according to volume ratio.
Extractant 7：Ethane and dimethyl ether are 8: 1 mixing according to volume ratio.
Supersound extraction 15min current intensity 1A/25w under the conditions of is carried out with probe type ultrasonic extraction apparatus when being slowly stirred
Obtain sonicated extract.
(3) sonicated extract that extraction in step (2) is obtained is placed in into high-pressure pulse electric, electric field intensity 25KV/ is set
Cm, 450 μ s of burst length, pulse frequency 260Hz, extraction time are 15min, obtain high-voltage pulse extract.
(4) the high-voltage pulse extract for obtaining is extracted in the step of taking 3L step (3) subcritical abstraction is added to into being arranged
In standby 5L batch extractors, 3h is soaked；Then extracting pressure be 0.6Mpa, extraction temperature be 30 DEG C, extraction time be 40min bars
Subcritical solvent extraction is carried out under part, miscella and Citrus powder is obtained.
(5) miscella taken in step (4) is imported in precipitation tank, and being decompressed to ﹣ 0.08MPa carries out precipitation tank decompression separation,
It is terpene compound to obtain grease.Grease is inserted in depressurized system, 85 DEG C of temperature, pressure is 4KPa, collects fraction,
Obtain limonene；Organic solvent after gasification is compressed, after condensation liquefaction, collect solvent, and tank is recycled.
(6) the Citrus powder in step (4) is taken, is added the water of 8 times of volumes as extractant, is carried out subcritical abstraction, if
It is 1Mpa to put extracting pressure, and extraction temperature is 50 DEG C, and extraction time is 50min, obtains oil water mixture.
(7) repeat step (6) 2 times, after extracting every time are transferred to extract in precipitation tank, are decompressed to normal pressure, by gained
Extract stratification, oil phase are the de- terpene quintessence oil of Citrus, obtain final product the de- terpene quintessence oil of Citrus.
Calculate quintessence oil yield the content using titration measuring limonene.As a result referring to table 1.
Table 1：Impact of the different extractants to Citrus essential oil extraction effect
| Extractant | Proportioning | Quintessence oil yield | De- terpene rate |
| Butane-dimethyl ether | 4∶1 | 3.79% | 86.85% |
| Butane-dimethyl ether | 8∶1 | 4.05% | 91.10% |
| Butane-dimethyl ether | 16∶1 | 3.23% | 84.95% |
| Sulfur hexafluoride-dimethyl ether | 4∶1 | 3.86% | 72.37% |
| Sulfur hexafluoride-dimethyl ether | 8∶1 | 3.94% | 82.37% |
| Ethane-dimethyl ether | 4∶1 | 2.62% | 75.06% |
| Ethane-dimethyl ether | 8∶1 | 3.57% | 89.32% |
As can be known from Table 1：Mixed solution with butane and dimethyl ether as extractant, when the volume ratio of butane and dimethyl ether is
When 8: 1, quintessence oil yield reaches 4.05%, and de- terpene rate reaches 91.10%, and quintessence oil yield and de- terpene effect are substantially better than other extractions
Agent.
Embodiment 5
Referring to Fig. 1, the impact that subcritical solvent extraction is extracted to Citrus essential oil is investigated：
(1) take 200g drying peel of Citrus reticulata Blanco, using super micron mill in the case where 10 DEG C of ﹣ micronizing 5min, obtaining particle diameter is
The powder of 2mm.
(2) powder is placed in pill tank, by 1g: 8mL addition extractant, (extractant is molten for the mixing of ethane and dimethyl ether
Liquid, wherein ethane and dimethyl ether volume ratio are 8: 1), when being slowly stirred with probe type ultrasonic extraction apparatus in current intensity 1.2A/
Supersound extraction 15min is carried out under the conditions of 45w, then is placed in high-pressure pulse electric, electric field intensity 25KV/cm, 500 μ s of burst length,
Pulse frequency 240Hz, extraction time 20min obtain high-voltage pulse extract.
(3) the high-voltage pulse extract in the step of taking 3L (2) is poured into the 5L batch extractors of subcritical abstraction complete set of equipments
Middle extraction, soaks 3h, is then respectively 0.2,0.6,1.8Mpa in extracting pressure, and extraction time is respectively 20,45,60min, extraction
Taking carries out subcritical abstraction under conditions of temperature is respectively 30,40,50 DEG C and obtains miscella and Citrus powder.
Take miscella to import in precipitation tank, being decompressed to ﹣ 0.08MPa carries out precipitation tank decompression separation, obtain grease and be
Terpene compound.Grease is inserted in depressurized system, temperature is 85 DEG C, and pressure is 4KPa, collect fraction, obtain Fructus Citri Limoniae
Alkene；Organic solvent after gasification is compressed, after condensation liquefaction, collect solvent, and tank is recycled.
(4) Citrus powder is taken, the water for adding 8 times of volumes carries out subcritical abstraction, and setting extracting pressure is 1.0Mpa, is extracted
Temperature is taken for 60 DEG C, extraction time is 50min.Extract will be transferred in precipitation tank after extraction, be decompressed to normal pressure, rotation is steamed
Solvent is sent out, is filtered after standing, obtain final product the de- terpene quintessence oil of Citrus.
Quintessence oil yield the content using titration measuring limonene are calculated, as a result referring to table 2.
Table 2：Impact of the subcritical solvent extraction to Citrus essential oil extraction effect
| Extracting pressure/Mpa | Extraction time/min | Extraction temperature/DEG C | Quintessence oil yield/% | De- terpene rate/% |
| 0.2 | 20 | 30 | 1.57% | 64.80% |
| 0.2 | 60 | 40 | 2.87% | 86.74% |
| 0.2 | 45 | 50 | 2.04% | 78.39% |
| 0.6 | 20 | 40 | 3.65% | 86.82% |
| 0.6 | 60 | 50 | 3.15% | 77.30% |
| 0.6 | 45 | 30 | 3.87% | 90.42% |
| 1.8 | 20 | 50 | 2.53% | 73.21% |
| 1.8 | 60 | 30 | 3.60% | 83.92% |
| 1.8 | 45 | 40 | 3.58% | 81.54% |
As can be known from Table 2：With ethane and dimethyl ether (ethane and dimethyl ether volume ratio are as 8: 1) for subcritical abstraction agent, when
Extracting pressure is 0.6Mpa, and extraction time is 45min, and extraction temperature is 30 DEG C, and quintessence oil yield reaches 3.87%, and de- terpene rate reaches
90.42%, quintessence oil yield and de- terpene effect are substantially better than other extraction conditionss.
Embodiment 6
Referring to Fig. 1, the impact that Subcritical Water Extraction Citrus essential oil is extracted is investigated：
(1) take 200g drying peel of Citrus reticulata Blanco, using super micron mill in the case where 10 DEG C of ﹣ micronizing 5min, obtaining particle diameter is
The powder of 2mm.
(2) powder is placed in pill tank, by 1g: 8mL addition extractant, (extractant is molten for the mixing of ethane and dimethyl ether
Liquid, wherein ethane and dimethyl ether volume ratio are 8: 1), when being slowly stirred with probe type ultrasonic extraction apparatus in current intensity 1.2A/
Supersound extraction 15min is carried out under the conditions of 45w, then is placed in high-pressure pulse electric, electric field intensity 25KV/cm, 500 μ s of burst length,
Pulse frequency 240Hz, extraction time 20min obtain high-voltage pulse extract.
(3) the high-voltage pulse extract after the step of taking 3L (2) process is poured into the 5L leachings of subcritical abstraction complete set of equipments
Go out in tank, soak 3h；Then 0.6Mpa is respectively in extracting pressure, extraction time is respectively 45min, and extraction temperature is respectively 30
Subcritical solvent extraction is carried out under conditions of DEG C, miscella and Citrus powder is obtained.
(4) Citrus powder is taken, the water for adding 8 times of volumes carries out subcritical abstraction, extracting pressure is set and is respectively 0.2,
0.5,1.3,2.6Mpa, extraction temperature is respectively 30,40,50,60 DEG C, and extraction time is respectively 30,40,50min.After extracting
Extract is transferred in precipitation tank, normal pressure is decompressed to, rotary evaporation of solvent is filtered after standing, obtain final product the de- terpene quintessence oil of Citrus.
Quintessence oil yield the content using titration measuring limonene are calculated, as a result referring to table 3.
Table 3：Impact of the Subcritical Water Extraction to Citrus essential oil extraction effect
| Extracting pressure/Mpa | Extraction time/min | Extraction temperature/DEG C | Quintessence oil yield/% | De- terpene rate/% |
| 0.2 | 40 | 30 | 2.57% | 72.81% |
| 0.2 | 50 | 50 | 2.96% | 78.64% |
| 0.5 | 30 | 40 | 4.21% | 93.26% |
| 0.5 | 50 | 60 | 3.38% | 86.69% |
| 1.3 | 30 | 50 | 4.13% | 79.25% |
| 1.3 | 40 | 30 | 2.64% | 84.11% |
| 2.6 | 60 | 60 | 1.72% | 75.32% |
| 2.6 | 30 | 40 | 2.43% | 79.53% |
As can be known from Table 3：With water as subcritical abstraction agent, when extracting pressure is 0.5Mpa, extraction time is 30min, extraction
Temperature is taken for 40 DEG C, quintessence oil yield reaches 4.21%, de- terpene rate reaches 93.26%, and quintessence oil yield and de- terpene effect are substantially better than
Other extraction conditionss.
The above, is only presently preferred embodiments of the present invention, not makees any pro forma restriction to the present invention.Though
So the present invention is disclosed as above with preferred embodiment, but is not limited to the present invention.It is any to be familiar with those skilled in the art
Member, in the case of the spirit and technical scheme without departing from the present invention, all using in the methods and techniques of the disclosure above
Appearance makes many possible variations and modification, or the Equivalent embodiments for being revised as equivalent variations to technical solution of the present invention.Therefore,
Every content without departing from technical solution of the present invention, according to the technical spirit of the present invention to made for any of the above embodiments any simple
Modification, equivalent, equivalence changes and modification, still fall within the range of technical solution of the present invention protection.
Claims (7)
1. a kind of extracting method of Citrus essential oil, it is characterised in that comprise the following steps：
（1）Peel of Citrus reticulata Blanco is dried in the shade, powder is ground into, the extractant of dimethyl ether and organic solvent composition is added, is carried out supersound extraction
Obtain sonicated extract；The organic solvent and dimethyl ether volume ratio are 1: 1～15: 1；Organic solvent is ethane, sulfur hexafluoride
With the one kind in butane；
（2）The sonicated extract is carried out into high-voltage pulse extraction and obtains high-voltage pulse extract；
（3）The high-voltage pulse extract is carried out into subcritical abstraction and obtains miscella and Citrus powder for 1～3 time；
（4）By the Citrus powder, subcritical abstraction 1～3 time is carried out by extractant of water, obtain oil water mixture；Extraction pressure
Power is 0.2 Mpa～6 Mpa, and extraction temperature is 15 DEG C～60 DEG C, and extraction time is 0.1 h～2 h；
（5）The oil water mixture is stood, is layered profit, oil phase is Citrus essential oil.
2. extracting method according to claim 1, it is characterised in that the step（1）Described in peel of Citrus reticulata Blanco adopt ultra micro
Pulverizer obtains powder in 10 DEG C of micronizing of ﹣, 5 min～30 min, and the particle diameter of the powder is 1 mm～10 mm.
3. extracting method according to claim 1, it is characterised in that the step（1）Described in powder and the extraction
The mass volume ratio of agent is g: 25 mL of 1g: 8 mL～1；1.0 A/25 w～1.5 A/ of current intensity of the supersound extraction
275 w, supersound extraction time are 10～15 min.
4. extracting method according to claim 1, it is characterised in that the step（2）In, the high-voltage pulse was extracted
20 KV/cm～50 KV/cm of electric field intensity in journey, 400 μ s～600 μ s of burst length, 200 Hz～450 of pulse frequency
Hz；The extraction time is 15 min～40 min.
5. extracting method according to claim 1, it is characterised in that the step（3）The subcritical abstraction it is concrete
For：The high-voltage pulse extract is added to into the batch extractor of subcritical abstraction equipment, 3 h～12 h are infiltrated；Then in extraction
Pressure is 0.2 Mpa～6 Mpa, and extraction temperature is to carry out 0.1 h～2 h of subcritical abstraction and obtain under conditions of 15 DEG C～60 DEG C
To miscella and Citrus powder.
6. extracting method according to any one of claim 1 to 5, it is characterised in that the step（3）Described in mix
Oil extract limonene, concrete extracting method is：By the miscella, steam oil tank is imported, 0.08 MPa precipitations of ﹣ is decompressed to and is obtained terpene
Ene compound, the terpene compound is placed in depressurized system, is 85 DEG C in temperature, and pressure is 4 KPa environment, under pressure point
Evaporate, collect fraction, obtain limonene.
7. extracting method according to any one of claim 1 to 5, it is characterised in that the step（4）It is described subcritical
In extraction process, Citrus powder is 1: 5～20 with the volume ratio of water.
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