CN102586023B - Method for extracting citrus pericarp essential oil - Google Patents
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Abstract
The invention discloses a method for extracting citrus pericarp essential oil, which comprises the following steps: selecting fresh citrus pericarps, removing the white pericarp layer until the pericarp thickness is 0.1-0.2cm, mincing, repeatedly freezing and thawing for 2-5 times, preparing a compound enzyme from pectinase and cellulose at a mass ratio of (1-6):1, preparing an enzyme solution, mixing the pretreated citrus pericarp particles with the compound enzyme solution, and performing enzymolysis in a dark place for 5-30min; and performing condensation and reflux extraction of the hydrolyzed citrus pericarps with n-hexane, and removing n-hexane to obtain essential oil. The method disclosed by the invention adopts a physical process of repeated freezing and thawing to conduct initial break of cell walls of citrus pericarps, and then performs enzymolysis of the citrus pericarps with the compound enzyme, so as to greatly increase the extraction rate of citrus pericarp essential oil. The method also has the following advantages: the extraction process is simple, the natural fragrance is less damaged, and the use value of the citrus processing byproduct - citrus pericarps - can be utilized to a maximum extent. The essential oil extracted using the method disclosed by the invention has pure texture and has the natural fragrance of citrus fruits.
Description
Technical field
The present invention relates to a kind of citrus pericarp essential oil, particularly relate to kind of a citrus pericarp extracts essential oil method.
Background technology
Tangerine essential oil is the spice oil that extracts from orange peel, has natural environmental-protective, and characteristics such as pleasant aroma are widely used in industries such as food, makeup, simultaneously as a kind of natural nonpoisonous organic solvent, is widely used in medicine, chemical industry.Studies show that, peel of Citrus reticulata Blanco oil have eliminate the phlegm, effects such as cough-relieving, promotion enterogastric peristalsis, the secretion of promoting digestion liquid, analgesia, dissolving gallbladdergallstonecholetithiasis and antiphlogistic antibacterial.
Producing at present the method for extraction of essential oil that goes up widespread use mainly contains: three kinds of steam distillations, milling process, solvent extration, supercritical fluid extraction is arranged in addition, but because higher to equipment requirements, reasons such as production cost height are almost seldom used in actual production.
1, steam distillation
Steam distillation is that the principle of utilizing water vapor to take away volatile oil prepares volatile oil.The volatile oil that obtains so also claims " deep fat ".Distillation method is the most frequently used method, can be divided into common hydrodistillation and steam distillation.This method operation is the simplest, and cost is lower, is the most frequently used extracting process.On the orange peel of fragmentation, add 3% solid NaCl equably, can improve oil yield about 20%.The shortcoming that this method exists is the inferior quality of gained essential oil, and subsequent disposal is trouble.
2, milling process
Essential oil in the citrus pericarp is positioned at the top layer of exocarp, and the oil sac diameter that contains essential oil generally can reach 0.4 ~ 0.6mm, and is bigger, and Ductless gland is formed by the cell accumulation encirclement of degenerating on every side.Milling process is with crunch squeezing peel of Citrus reticulata Blanco, and its oil cell is broken, and causes oil content to flow out, and then separates oilyly.Adopt this method obtain peel of Citrus reticulata Blanco oil yield about 0.3%, pressed oil fragrance is near the orange fruital, color is light yellow.The essential oil oil of this method gained is good, but the shortcoming of its existence is not thorough to the extraction of tangerine essential oil, and yield is lower.Residue after the squeezing can also adopt solvent extraction method to extract the tangerine essential oil that obtains part.
3, solvent extration
Thereby solvent-extraction process is to utilize lower boiling organic solvent such as hexane, ether, sherwood oil and ethanol to wait to soak peel of Citrus reticulata Blanco volatile oil is put forward.This method key is that selected solvent must have selectivity and lower viscosity preferably to effective constituent, selects performance to make effective constituent that big relatively solubleness be arranged preferably, and lower viscosity can make it bigger velocity of diffusion.This method is simple to operate, and gained essential oil quality is pure, but yield is lower.
Summary of the invention
The objective of the invention is provides a kind of yield height in order to overcome the defective that prior art exists, and essential oil extracts thoroughly, the citrus pericarp extracts essential oil method of essential oil quality better.
The present invention adopts the physical method of multigelation that the peel of Citrus reticulata Blanco cell walls is tentatively destroyed, combining pectin enzyme and cellulase are to the thorough enzymolysis of navel orange chrotoplast wall again, improve the leaching yield of tangerine essential oil, after adopt solvent extraction method to extract again, the navel orange essential oil quality that this method is extracted is pure, color and luster is shallow clearly, and the essential oil extraction thoroughly, and yield significantly improves.
Purpose of the present invention realizes by following proposal:
A kind of citrus pericarp extracts essential oil method comprises the steps and processing condition:
(1) citrus pericarp pre-treatment: choose fresh citrus pericarp, removing white cortex to peel thickness is 0.1 ~ 0.2cm, chopping, and the control particle diameter is 0.2 ~ 0.5cm, multigelation 2 ~ 5 times; Freeze thawing for the first time is citrus pericarp particle to be moved to thaw under 10 ℃ ~ 60 ℃ behind freezing 10 ~ 90min under-5 ℃ ~-30 ℃; Freeze thawing for the second time is that the citrus pericarp particle after thawing is thawed moving under 10 ℃ ~ 60 ℃ behind freezing 10 ~ 90min under-5 ℃ ~-30 ℃ again again; If carry out 3-5 freeze thawing, the 3-5 time freeze thawing is with freezing-thawing method is identical for the second time;
(2) preparation of enzyme liquid: prepare prozyme according to polygalacturonase and cellulase mass ratio 1:1 ~ 6:1, adding water preparation mass percent with prozyme again is 0.2% ~ 0.6% enzyme liquid, and the pH of regulatory enzyme liquid is 3.5 ~ 5.5;
(3) enzymolysis of peel of Citrus reticulata Blanco: with pretreated citrus pericarp particle and the enzyme liquid mixed according to mass ratio 1:1 ~ 1:6, at 25 ~ 60 ℃ of following lucifuge enzymolysis 5min ~ 30min;
(4) normal hexane extraction: adopt normal hexane to carry out condensing reflux the citrus pericarp particle behind the enzymolysis and extract 2 ~ 6 times; Extracting for the first time is to be that 1:5 ~ 1:30 mix with normal hexane by mass ratio with citrus pericarp particle, and the extraction temperature is 25 ~ 70 ℃, and the time is 0.5h ~ 2h; Extracting for the second time is after the extraction mixed solution is filtered, to get filter residue and mix according to mass ratio 1:5 ~ 1:30 with normal hexane again, and extracting temperature is 25 ~ 70 ℃, and the time is 0.5h ~ 2h; Extract if carry out the 3-6 time, the 3-6 time extracting method is with extracting for the second time;
(5) preparation of essential oil product: with extract centrifugal 5 ~ 30min under 4000 ~ 9000r/min condition of normal hexane extraction gained, get its supernatant liquor and rotate the evaporative removal normal hexane down at 20 ~ 75 ℃, namely get citrus pericarp essential oil.
Further, described citrus pericarp is the pericarp of orange class, shaddock class or lemon class.
Described pH value is regulated by citric acid-disodium hydrogen phosphate buffer solution.
The concentration of described citric acid solution is 0.1mol/L, and the concentration of disodium phosphate soln is 0.2mol/L.
With respect to prior art, the present invention has following advantage and beneficial effect:
(1) the present invention proposes physics-biology-solvent lixiviate three-step approach first and extracts tangerine essential oil: the first step multigelation tentatively destroys citrus pericarp membrane wall, second step thoroughly destroyed cell walls in conjunction with enzymolysis, the normal hexane solvent lixiviate of the 3rd step, the tangerine essential oil color and luster that extracts is shallow clearly, quality is pure, essential oil extracts thoroughly, and yield significantly improves.
(2) raw material of the present invention is cheap and easy to get, adopts physical method to handle the citrus pericarp first, by destroying the peel of Citrus reticulata Blanco cell walls, has promoted the leaching of essential oil.
(3) method of the present invention is simple to operate, to plant and instrument require lowly, reduced cost, improved benefit.
Embodiment
The present invention is further illustrated below in conjunction with embodiment, but the scope of protection of present invention is not limited to the scope of embodiment statement.
Embodiment 1
Choose fresh citrus fruit-navel orange, getting skin and removing white cortex to peel thickness is 0.1cm, and the navel orange skin after the processing is pulverized, and the diameter of pulverized particles is 0.2cm; To pulverize posterior umbilicus orange peel particle and move under 10 ℃ after freezing 10min under-5 ℃ and thaw, the navel orange skin particle after thawing moves under 10 ℃ after freezing 10min under-5 ℃ and thaws; Select polygalacturonase, cellulase for use, according to polygalacturonase and cellulase mass ratio 1:1 preparation prozyme, adding water preparation mass percent with prozyme again is the mass percent of 0.2%(prozyme in enzyme liquid) enzyme liquid, and be 3.5 with the pH of citric acid-disodium hydrogen phosphate buffer solution regulatory enzyme liquid, the volumetric molar concentration of citric acid solution is 0.1mol/L, and the volumetric molar concentration of disodium phosphate soln is 0.2mol/L; With navel orange skin and the prozyme liquid mixed according to mass ratio 1:1, at 25 ℃ of following lucifuge enzymolysis 5min; Adopt normal hexane to carry out condensing reflux the navel orange skin behind the enzymolysis and extract, the mass ratio of navel orange skin and normal hexane is 1:5, and extracting temperature is 25 ℃, time is 0.5h, after will extracting mixed solution and filtering, gets filter residue and mixes according to mass ratio 1:5 with normal hexane, extracting temperature is 25 ℃, and the time is 0.5h; With gained n-hexane extract centrifugal 5min under the 4000r/min condition, get its supernatant liquor and rotate the evaporative removal normal hexane down at 20 ℃, namely get essential oil.In the leaching process, thoroughly destroyed the cell walls of navel orange pericarp by the pre-treatment of physics-biological combination, the solubility rate of essential oil increases, and the essential oil yield is for being increased to the 6.92%(quality), and the yield of essential oil only is 1.0% ~ 3.0%(quality when adopting solvent extration to carry out the essential oil extraction at present).Essential oil residual quantity in the remaining residue is carried out normal hexane to be extracted again, and extracted amount detected, extraction conditions is: the residue normal hexane mixes according to mass ratio 1:5, extracting temperature is 25 ℃, time is 0.5h, and extraction time is 1 time, and the result shows: the residual quantity of essential oil is the 0.13%(quality), for extracting the 1.88%(quality of total amount), prove that this method is more thorough to the extraction of the essential oil in the navel orange skin.
Use GC-MS to analyze the composition of the navel orange peel essential oil that extracts, condition is: adopt chromatographic column (HPinnowax, 60m * 0.25mm * 0.25 μ m) to analyze.Carrier gas is helium, and flow velocity is 1mL/min; Column temperature keeps 2min for 50 ℃, is warming up to 220 ℃ with 3 ℃/min again, keeps 2min then; The vaporization room temperature is 220 ℃; Sample size is 0.2 μ L(volume), splitting ratio (volume) is 40:1.The main component that draws essential oil has: hesperidene, the D-limonene, the 1S-α-Pai Xi, β-phellandrene, beta-myrcene, 4-methyl isophthalic acid-(1-methyl ethylene)-two ring [3.1.0] hexane-2-alkene, (z)-3,7-dimethyl-1,3,6 sarohornenes, 3,7-dimethyl-6 octenal, capraldehyde, linalyl isobutyrate, 3,7 dimethyl-1,6 octadienes-3 alcohol, trans-8 sec.-propyls two rings [4,3,0] ninth of the ten Heavenly Stems-3-alkene, (R)-3,7-dimethyl-6-octen-1-ol, the 4-[1-methyl ethylene]-1-tetrahydrobenzene-1-formaldehyde, wherein, hesperidene accounts for the 81.23%(quality), the D-limonene accounts for the 15.67%(quality).
Embodiment 2
Choose fresh citrus fruit-shaddock, getting skin and removing white cortex to peel thickness is 0.15cm, and the shaddock ped after the processing is pulverized, and the diameter of pulverized particles is 0.3cm; Shaddock skin particle moves under 20 ℃ after freezing 30min under-15 ℃ and thaws after will pulverizing, and the shaddock ped particle after thawing moves under 20 ℃ after freezing 20min under-10 ℃ and thaws, and so multigelation amounts to freeze thawing 3 times; Select polygalacturonase, cellulase for use, according to polygalacturonase and cellulase mass ratio 1:3 preparation prozyme, adding water preparation mass percent with prozyme again is the mass percent of 0.35%(prozyme in enzyme liquid) enzyme liquid, and be 4.5 with the pH of citric acid-disodium hydrogen phosphate buffer solution regulatory enzyme liquid, the volumetric molar concentration of citric acid solution is 0.1mol/L, and the volumetric molar concentration of disodium phosphate soln is 0.2mol/L; With shaddock skin and the prozyme liquid mixed according to mass ratio 1:3, at 35 ℃ of following lucifuge enzymolysis 15min; Adopting normal hexane to carry out condensing reflux the shaddock skin behind the enzymolysis extracts, the mass ratio of shaddock skin and normal hexane is 1:15, extracting temperature is 35 ℃, time is 1h, after will extracting mixed solution and filtering, gets filter residue and mixes according to mass ratio 1:10 with normal hexane, extracting temperature is 35 ℃, time is 1h, extracts so repeatedly, extracts altogether 4 times; With centrifugal 15min under the n-hexane extract 5000r/min condition, get its supernatant liquor and rotate the evaporative removal normal hexane down at 35 ℃, namely get essential oil.In the leaching process, thoroughly destroyed the cell walls of navel orange pericarp by the pre-treatment of physics-biological combination, the solubility rate of essential oil increases, and the essential oil yield is increased to the 7.86%(quality), and adopt at present solvent extration carry out essential oil when extracting the yield of essential oil only be 1.0% ~ 3.0%(quality).Essential oil residual quantity in the remaining residue is carried out normal hexane to be extracted again, and extracted amount detected, extraction conditions is: the mass ratio of residue and normal hexane is 1:15, extracting temperature is 35 ℃, time is 1h, extracts 4 times, and the result shows: the residual quantity of essential oil is the 0.03%(quality), for extracting the 0.32%(quality of total amount), prove that this method is more thorough to the extraction of the essential oil in the shaddock skin.
Use GC-MS to analyze the composition of the shaddock peel essential oil that extracts, condition is: adopt chromatographic column (HPinnowax, 60m * 0.25mm * 0.25 μ m) to analyze.Carrier gas is helium, and flow velocity is 1mL/min; Column temperature keeps 2min for 50 ℃, is warming up to 220 ℃ with 3 ℃/min again, keeps 2min then; The vaporization room temperature is 220 ℃; Sample size is 0.2 μ L(volume), splitting ratio (volume) is 40:1.The main component that draws essential oil has: hesperidene, 1S-α-Pai Xi, β-phellandrene, beta-myrcene, 4-methyl isophthalic acid-(1-methyl ethylene)-two ring [3.1.0] hexane-2-alkene, (z)-3,7-dimethyl-1,3,6 sarohornenes, 3,7-dimethyl-6 octenal, capraldehyde, linalyl isobutyrate, 3,7 dimethyl-1,6 octadienes-3 alcohol, trans-8 sec.-propyls two rings [4,3,0] ninth of the ten Heavenly Stems-3-alkene, (R)-3,7-dimethyl-6-octen-1-ol, 4-[1-methyl ethylene]-1-tetrahydrobenzene-1-formaldehyde, wherein hesperidene accounts for the 92.9%(quality of total amount).
Embodiment 3
Choose fresh citrus fruit-lemon, get skin and remove white cortex, the lemon peel after the processing is pulverized, and the diameter of pulverized particles is 0.5cm; To pulverize posterior umbilicus orange peel particle and move under 60 ℃ after freezing 90min under-30 ℃ and thaw, the navel orange skin particle after thawing moves under 60 ℃ after freezing 90min under-30 ℃ and thaws, and so multigelation is 5 times; Select polygalacturonase, cellulase for use, according to polygalacturonase and cellulase mass ratio 6:1 preparation prozyme, adding water preparation massfraction with prozyme again is the mass percent of 0.6%(prozyme in enzyme liquid) enzyme liquid, and be 5.5 with the pH of citric acid-disodium hydrogen phosphate buffer solution regulatory enzyme liquid, the volumetric molar concentration of citric acid solution is 0.1mol/L, and the volumetric molar concentration of disodium phosphate soln is 0.2mol/L; With lemon peel and the prozyme liquid mixed according to mass ratio 1:6, at 60 ℃ of following lucifuge enzymolysis 30min; Adopting normal hexane to carry out condensing reflux the lemon peel behind the enzymolysis extracts, the mass ratio of lemon peel and normal hexane is 1:30, extracting temperature is 70 ℃, time is 2.0h, after will extracting the mixed solution filtration, get filter residue and mix according to mass ratio 1:30 with normal hexane, extracting temperature is 70 ℃, time is 2.0h, extracts so repeatedly 6 times; With centrifugal 30min under the n-hexane extract 9000r/min condition, get its supernatant liquor and rotate the evaporative removal normal hexane down at 75 ℃, namely get essential oil.In the leaching process, thoroughly destroyed the cell walls of lemon pericarp by the pre-treatment of physics-biological combination, the solubility rate of essential oil increases, and the essential oil yield is increased to the 7.16%(quality), and adopt at present solvent extration carry out essential oil when extracting the yield of essential oil only be 1.0% ~ 3.0%(quality).Essential oil residual quantity in the remaining residue is carried out normal hexane to be extracted again, and extracted amount detected, extraction conditions is: residue with mix according to mass ratio 1:30 with normal hexane, extracting temperature is 70 ℃, time is 2.0h, and extraction time is 1 time, and the result shows: the residual quantity of essential oil is the 0.08%(quality), for extracting the 1.12%(quality of total amount), prove that this method is more thorough to the extraction of the essential oil in the lemon peel.
Use GC-MS to analyze the composition of the lemon peel essential oil that extracts, condition is: adopt chromatographic column (HPinnowax, 60m * 0.25mm * 0.25 μ m) to analyze.Carrier gas is helium, and flow velocity is 1mL/min; Column temperature keeps 2min for 50 ℃, is warming up to 220 ℃ with 3 ℃/min again, keeps 2min then; The vaporization room temperature is 220 ℃; Sample size is 0.2 μ L(volume), splitting ratio (volume) is 40:1.The main component that draws essential oil has D-hesperidene, 1S-α-Pai Xi, β-phellandrene, beta-myrcene, 4-methyl isophthalic acid-(1-methyl ethylene)-two ring [3.1.0] hexane-2-alkene, (z)-3,7-dimethyl-1,3,6 sarohornenes, 3,7-dimethyl-6 octenal, capraldehyde, linalyl isobutyrate, 3,7 dimethyl-1,6 octadienes-3 alcohol, trans-8 sec.-propyls two rings [4,3,0] ninth of the ten Heavenly Stems-3-alkene, (R)-3,7-dimethyl-6-octen-1-ol, 4-[1-methyl ethylene]-1-tetrahydrobenzene-1-formaldehyde, wherein the D-hesperidene accounts for the 93.6%(quality).
Embodiment 4
Choose fresh citrus fruit-navel orange, shaddock, lemon, three kinds of fruit are got skin by mass ratio 1:1:1 and are removed white cortex, and the mixing skin after the processing is pulverized, and the diameter of pulverized particles is 0.4cm; To pulverize posterior umbilicus orange peel particle and move under 40 ℃ after freezing 40min under-20 ℃ and thaw, the navel orange skin particle after thawing moves under 40 ℃ after freezing 40min under-20 ℃ and thaws, and so multigelation is 4 times; Select polygalacturonase, cellulase for use, according to polygalacturonase and cellulase mass ratio 4:1 preparation prozyme, adding water preparation massfraction with prozyme again is the mass percent of 0.4%(prozyme in enzyme liquid) enzyme liquid, and be 4.5 with the pH of citric acid-disodium hydrogen phosphate buffer solution regulatory enzyme liquid, the volumetric molar concentration of citric acid solution is 0.1mol/L, and the volumetric molar concentration of disodium phosphate soln is 0.2mol/L; With peel of Citrus reticulata Blanco and the prozyme liquid mixed according to mass ratio 1:4, at 40 ℃ of following lucifuge enzymolysis 20min; Adopting normal hexane to carry out condensing reflux the peel of Citrus reticulata Blanco behind the enzymolysis extracts, the mass ratio of peel of Citrus reticulata Blanco and normal hexane is 1:20, extracting temperature is 45 ℃, time is 1h, after will extracting mixed solution and filtering, gets filter residue and mixes according to mass ratio 1:25 with normal hexane, extracting temperature is 45 ℃, time is 1h, extracts so repeatedly, extracts altogether 4 times; With centrifugal 20min under the n-hexane extract 7000r/min condition, get its supernatant liquor and rotate the evaporative removal normal hexane down at 45 ℃, namely get essential oil.In the leaching process, thoroughly destroyed the cell walls of navel orange pericarp by the pre-treatment of physics-biological combination, the solubility rate of essential oil increases, and the volatile oil yield is increased to the 8.92%(quality), and adopt at present solvent extration carry out essential oil when extracting the yield of essential oil only be 1.0% ~ 3.0%(quality).Essential oil residual quantity in the remaining residue is carried out normal hexane to be extracted again, and extracted amount detected, extraction conditions is: normal hexane mixes according to mass ratio 1:25, extracting temperature is 45 ℃, time is 1h, and extraction time is 1 time, and the result shows: the residual quantity of essential oil is the 0.02%(quality), for extracting the 0.22%(quality of total amount), prove that this method is more thorough to the extraction of the essential oil in the navel orange skin.
Use GC-MS to analyze the composition of the navel orange peel essential oil that extracts, condition is: adopt chromatographic column (HPinnowax, 60m * 0.25mm * 0.25 μ m) to analyze.Carrier gas is helium, and flow velocity is 1mL/min; Column temperature keeps 2min for 50 ℃, is warming up to 220 ℃ with 3 ℃/min again, keeps 2min then; The vaporization room temperature is 220 ℃; Sample size is 0.2 μ L(volume), splitting ratio (volume) is 40:1.The main component that draws essential oil has: D-hesperidene, 1S-α-Pai Xi, β-phellandrene, beta-myrcene, 4-methyl isophthalic acid-(1-methyl ethylene)-two ring [3.1.0] hexane-2-alkene, (z)-3,7-dimethyl-1,3,6 sarohornenes, 3,7-dimethyl-6 octenal, capraldehyde, linalyl isobutyrate, 3,7 dimethyl-1,6 octadienes-3 alcohol, trans-8 sec.-propyls two rings [4,3,0] ninth of the ten Heavenly Stems-3-alkene, (R)-3,7-dimethyl-6-octen-1-ol, 4-[1-methyl ethylene]-1-tetrahydrobenzene-1-formaldehyde, wherein the D-hesperidene accounts for the 97.3%(quality).
Claims (4)
1. citrus pericarp extracts essential oil method is characterized in that comprising the steps and processing condition:
(1) citrus pericarp pre-treatment: choose fresh citrus pericarp, removing white cortex to peel thickness is 0.1～0.2cm, chopping, and the control particle diameter is 0.2～0.5cm, multigelation 2～5 times; Freeze thawing for the first time is citrus pericarp particle to be moved to thaw under 10 ℃～60 ℃ behind freezing 10～90min under-5 ℃～-30 ℃; Freeze thawing for the second time is that the citrus pericarp particle after thawing is thawed moving under 10 ℃～60 ℃ behind freezing 10～90min under-5 ℃～-30 ℃ again again; If carry out 3-5 freeze thawing, the 3-5 time freeze thawing is with freezing-thawing method is identical for the second time;
(2) preparation of enzyme liquid: according to polygalacturonase and cellulase mass ratio preparation in 1: 1～6: 1 prozyme, adding water preparation mass percent with prozyme again is 0.2%～0.6% enzyme liquid, and the pH of regulatory enzyme liquid is 3.5～5.5;
(3) enzymolysis of peel of Citrus reticulata Blanco: with pretreated citrus pericarp particle and enzyme liquid according to 1: 1～1: 6 mixed of mass ratio, at 25～60 ℃ of following lucifuge enzymolysis 5min～30min;
(4) normal hexane extraction: adopt normal hexane to carry out condensing reflux the citrus pericarp particle behind the enzymolysis and extract 2～6 times; Extracting for the first time is to be to mix in 1: 5～1: 30 citrus pericarp particle and normal hexane by mass ratio, and the extraction temperature is 25～70 ℃, and the time is 0.5h～2h; Extracting for the second time is after the extraction mixed solution is filtered, to get filter residue and mixed in 1: 5～1: 30 according to mass ratio with normal hexane again, and extracting temperature is 25～70 ℃, and the time is 0.5h～2h; Extract if carry out the 3-6 time, the 3-6 time extracting method is with extracting for the second time;
(5) preparation of essential oil product: with extract centrifugal 5～30min under 4000～9000r/min condition of normal hexane extraction gained, get its supernatant liquor and rotate the evaporative removal normal hexane down at 20～75 ℃, namely get citrus pericarp essential oil.
2. citrus pericarp extracts essential oil method according to claim 1 is characterized in that, described citrus pericarp is the pericarp of orange class, shaddock class or lemon class.
3. citrus pericarp extracts essential oil method according to claim 1 is characterized in that, described pH value is regulated by citric acid-disodium hydrogen phosphate buffer solution.
4. citrus pericarp extracts essential oil method according to claim 3 is characterized in that the concentration of described citric acid solution is 0.1mol/L, and the concentration of disodium phosphate soln is 0.2mol/L.
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| CN100480364C (en) * | 2005-04-05 | 2009-04-22 | 张劲松 | Technique for separating essential oil of spiceberry by method for breaking cell wall under normal temperature (or low temperature) and normal pressure |
| CN101928639B (en) * | 2010-08-20 | 2012-10-03 | 遵义陆圣康源科技开发有限责任公司 | Natural tea essence prepared by using tea and preparation method thereof |
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