CN108251215A - A kind of extracting method of cinnamon essential oil for mite killing - Google Patents
A kind of extracting method of cinnamon essential oil for mite killing Download PDFInfo
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- CN108251215A CN108251215A CN201711433785.1A CN201711433785A CN108251215A CN 108251215 A CN108251215 A CN 108251215A CN 201711433785 A CN201711433785 A CN 201711433785A CN 108251215 A CN108251215 A CN 108251215A
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—Refining
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
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Abstract
The present invention provides a kind of extracting method of the cinnamon essential oil for mite killing, including：(1) Chinese cassia tree raw material is taken, Chinese cassia tree raw material is subjected to freeze-drying process；(2) it after step (1) Chinese cassia tree raw material is crushed, adds in solvent and complex enzyme is digested, obtain enzymolysis liquid, filtered after enzyme deactivation, collect filtrate and filter residue；Filtrate obtains extracting solution A after centrifugation；(3) surfactant is added in filter residue, then carries out heating distillation, collection obtains condensate liquid, by condensate liquid centrifugation, crude product is obtained after water-oil separating；(4) crude product and extracting solution A are mixed, organic phase is taken after extraction, is dissolved in buffer solution after organic phase is evaporated, obtains crude extract, gained crude extract using macroreticular resin is adsorbed, is then eluted using eluent, obtains crude extract；(5) crude extract is obtained into cinnamon essential oil using chromatogram purification.The extracting method extraction efficiency of cinnamon essential oil of the present invention is higher, and the cinnamon essential oil quality extracted is preferable.
Description
Technical field
The present invention relates to the extraction fields of plants essential oil, and in particular to a kind of extraction side of cinnamon essential oil for mite killing
Method.
Background technology
In recent years, the incidence of anaphylactia (such as bronchial asthma, rhinitis) is in the world and increases year by year
Trend, serious threat people's health and life security.Research shows that dust mite is to cause anaphylactia main
One of inhalant allergens.Therefore, the dissipation of dust mite has great importance for the prevention of anaphylactia.
Existing acaricide is mainly using chemical substances such as Ergols as principle active component, and be often used in agriculture evil mite
Dissipation and prevention.Although these chemicals can preferably controlling dust mite, need to be used for a long time just effective, and toxicity
By force, residual is long, side effect is big, has large effect to environment, is unsuitable for indoor use.Therefore, research it is quick, efficiently, low toxicity,
Environmentally safe novel acaricide becomes one of emphasis of current anaphylactia study on prevention work.
In this regard, it has been proposed that using cinnamomum cassia extract or cinnamon essential oil for mite killing, but the extraction of cinnamon essential oil at present
Method is generally there are the defects of extraction effect is bad, recovery rate is not high, therefore, it is necessary to provide a kind of carrying for new cinnamon essential oil
Take method.
Invention content
To solve the above problems, the present invention provides a kind of extracting methods of the cinnamon essential oil for mite killing.Meat of the present invention
The extracting method extraction efficiency of osmanthus essential oil is higher.
The present invention provides a kind of extracting methods of the cinnamon essential oil for mite killing, include the following steps：
(1) Chinese cassia tree raw material is taken, the Chinese cassia tree raw material is subjected to freeze-drying process；
(2) it after step (1) treated Chinese cassia tree raw material is crushed, adds in solvent and complex enzyme is digested, digested
Liquid filters after enzyme deactivation, collects filtrate and filter residue；The filtrate obtains extracting solution A after centrifugation；
(3) surfactant is added in the filter residue, then carries out heating distillation, collection obtains condensate liquid, will condense
Liquid centrifugation obtains crude product after water-oil separating；
(4) crude product and the extracting solution A are mixed, organic phase is taken after extraction, after the organic phase is evaporated
It is dissolved in buffer solution, obtains crude extract, gained crude extract using macroreticular resin is adsorbed, is then carried out using eluent
Elution, obtains crude extract；
(5) crude extract is obtained into the cinnamon essential oil for mite killing using chromatogram purification.
Wherein, complex enzyme described in step (2) includes cellulase, pectase and zytase, wherein, the cellulose
The weight ratio of enzyme, the pectase and the zytase is 1-5:1-5:1, the addition weight of the complex enzyme is the Chinese cassia tree
The 0.1%-0.5% of raw material weight.
Wherein, surfactant described in step (3) includes C8-C20Cationic surfactant, C8-C20Anion
Surfactant and C8-C20Nonionic surfactant in it is one or more, the addition weight of the surfactant is
The 0.1%-10% of the filter residue weight.
Wherein, the surfactant includes neopelex, Tween-80, sldium lauryl sulfate, dodecyl
It is one or more in sodium sulfonate, hexadecyltrimethylammonium chloride, octadecyltrimethylammonium chloride and odium stearate.
Wherein, between step (3) and step (4), by the progress of at least one of the crude product and the extracting solution A
High-pressure pulse electric processing, the high-pressure pulse electric processing carry out in accordance with the following methods：
At least one of the crude product and the extracting solution A are added in isometric ethyl alcohol, carry out high-tension pulse
Electric field treatment, electric field strength 20-40kV/cm are rushed, umber of pulse is 5-8, and supernatant is taken to continue step (4) after centrifugation
Operation.
Wherein, in step (4), the macroreticular resin is included in polarity, middle polarity, low pole and non-polar macroporous resin
It is one or more.
Wherein, the macroreticular resin is HPD500 or AB-8 macroreticular resins.
Wherein, using the time that the macroreticular resin is adsorbed, the dosage of the macroreticular resin was by such as 0.5-2 hours
Lower ratio addition：1g macroreticular resins/20-50mL crude extracts.
Wherein, in step (5), the method for the chromatogram purification includes high-speed countercurrent chromatography, the high speed adverse current chromatogram
Condition is as follows：Rotating speed is 500-1200rpm；Temperature is 16-34 DEG C；Flow velocity is 1-3ml/min；Separation solvent is A-B- water bodys
System, the A are chloroform, dichloromethane, dichloroethanes or tetrachloromethane；The B is methanol or ethyl alcohol；In the separation solvent,
The volumn concentration of the A is 20%-70%；The volumn concentration of the B is 5%-60%；The volume basis of the water
Content is 5%-50%.
Wherein, in step (1), the freeze-drying process operates in accordance with the following methods：
(1) eutectic point of Chinese cassia tree raw material is measured, is filled in material disc after measure；
(2) material disc is put into cool chamber, cool chamber temperature is adjusted to pre-freeze junction temperature, kept for 3.5-5 hours, in advance
Solidification point is less than 10-20 DEG C of the eutectic temperature；
(3) lyophilization will be carried out in prefreezing treated Chinese cassia tree raw material merging dry vacuum container, dry vacuum container is true
Reciprocal of duty cycle maintains 0.3-0.4KPa, the heat supply into dry vacuum container, and maximum temperature is controlled at 50 DEG C, when temperature of charge reaches setting
During maximum temperature, stop heating；
(4) vacuum of breaking vacuum dryness storehouse takes out Chinese cassia tree raw material.
Higher, the cinnamon spirit extracted provided by the present invention for the extracting method extraction efficiency of the cinnamon essential oil of mite killing
Oil quality is preferable, is effectively used for mite killing.
Description of the drawings
Fig. 1 is the extracting method flow chart of the cinnamon essential oil for mite killing that an embodiment of the present invention provides.
Specific embodiment
As described below is the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also considered as
Protection scope of the present invention.
Refering to Fig. 1, an embodiment of the present invention provides a kind of extracting method of the cinnamon essential oil for mite killing, including following step
Suddenly：
S01, Chinese cassia tree raw material is taken, the Chinese cassia tree raw material is subjected to freeze-drying process；
S02, it after step S01 treated Chinese cassia tree raw materials are crushed, adds in solvent and complex enzyme is digested, digested
Liquid filters after enzyme deactivation, collects filtrate and filter residue；The filtrate obtains extracting solution A after centrifugation；
S03, surfactant is added in the filter residue, then carries out heating distillation, collection obtains condensate liquid, will condense
Centrifugation after liquid cooling, crude product is obtained after water-oil separating；
S04, the crude product and the extracting solution A are mixed, organic phase is taken after extraction, after the organic phase is evaporated
It is dissolved in buffer solution, obtains crude extract, gained crude extract using macroreticular resin is adsorbed, is then carried out using eluent
Elution, obtains crude extract；
S05, the crude extract is used into chromatogram purification, obtains the cinnamon essential oil for mite killing.
In the embodiment of the present invention, in step S01, the Chinese cassia tree raw material is cassia.
In step S01, the freeze-drying process operates in accordance with the following methods：
(1) eutectic point of Chinese cassia tree raw material is measured, is filled in material disc after measure；
(2) material disc is put into cool chamber, cool chamber temperature is adjusted to pre-freeze junction temperature, kept for 3.5-5 hours, in advance
Solidification point is less than 10-20 DEG C of the eutectic temperature；
(3) lyophilization will be carried out in prefreezing treated Chinese cassia tree raw material merging dry vacuum container, dry vacuum container is true
Reciprocal of duty cycle maintains 0.3-0.4KPa, the heat supply into dry vacuum container, and maximum temperature is controlled at 50 DEG C, when temperature of charge reaches setting
During maximum temperature, stop heating；
(4) vacuum of breaking vacuum dryness storehouse takes out Chinese cassia tree raw material.
Step of embodiment of the present invention S01 is handled Chinese cassia tree raw material using freeze-drying, after freeze-drying, it is easier to carry
Take the active ingredient in Chinese cassia tree raw material.
In the embodiment of the present invention, in step S02, after the Chinese cassia tree raw material is crushed, 80-100 mesh sieve is crossed.
In step S02, the complex enzyme includes cellulase, pectase and zytase, wherein, the cellulase,
The weight ratio of pectase and zytase is 1-5:1-5:1.The unit of activity of the complex enzyme is 4000-7000U/g.It is optional
Ground, the weight ratio of the cellulase, pectase and zytase is 4:2:1.Optionally, the addition weight of the complex enzyme is
The 0.1%-0.5% of the Chinese cassia tree raw material weight.
In step S02, the solvent includes water.The addition weight of the solvent is 3-6 times of Chinese cassia tree raw material weight.
In step S02, it is molten that Chinese cassia tree raw material and complex enzyme can be added to acetic acid/sodium acetate buffer that pH is 4.0-6.0
In liquid.
In step S02, the hydrolysis temperature is 55-60 DEG C, and the enzymolysis time is 0.5-2h.
In step S02, the filtrate obtains extracting solution A after centrifugation, and the centrifugal force is 4000-6000g, centrifugation time
For 5-8min.
Step of embodiment of the present invention S02 is effectively improved the yield of Cortex Cinnamomi volatile oil, and help using the technique of enzymolysis
Continue to extract in subsequent.
In the embodiment of the present invention, in step S03, the surfactant includes C8-C20Cationic surfactant,
C8-C20Anion surfactant and C8-C20Nonionic surfactant in it is one or more.Optionally, it is described non-
Ionic surface active agent includes fatty alcohol polyethenoxy ether class, sorbitan fatty acid ester class, polyoxyethylene sorbitan
Fatty acid ester, polyethylene glycol, alkyl polyglycoside or sucrose-fatty esters；The anion surfactant includes aliphatic acid
Sodium salt, fatty acid potassium salt, sulfonate surfactant, sulfuric acid ester surfactant, phosphate ester surfactant or amber
Amber acid ester sulfonates class；The cationic surface include quaternary ammonium salt cationic surfactant, heterocyclic cationic surfactant or
Polyethylene polyamines salt.Still optionally further, the surfactant includes neopelex, Tween-80, laruyl alcohol
In sodium sulphate, dodecyl sodium sulfate, hexadecyltrimethylammonium chloride, octadecyltrimethylammonium chloride and odium stearate
It is at least one.
In step S03, the addition weight of the surfactant is the 0.1%-10% of the filter residue weight.Optionally,
The addition weight of the surfactant is the 0.5%-1.0% of the filter residue weight.
In step S03, in addition to adding in surfactant, it is also added into water.The addition weight of the water is the filter residue weight
10-15 times of amount.
In step S03, vapo(u)rizing temperature is makes system boil, distillation time 1-3h.
In step S03, cinnamon oil crude product is obtained after removing moisture removal after water-oil separating.
Using the distillating method of step S03, using the wetting of surfactant, infiltration, solubilising, foaming characteristic, shorten distillation
Time improves oil yield, reduces energy consumption, accelerates water-oil separating, improves utilization rate of equipment and installations, substantially reduces production cost.
It, can be by the crude product and the extracting solution A after step S03 and before step S04 in the embodiment of the present invention
At least one of carry out high-pressure pulse electric processing, processing operation carries out in accordance with the following methods：
At least one of the crude product and the extracting solution A are added in isometric ethyl alcohol, through high-voltage pulse
It is centrifuged after electric field treatment, electric field strength 20-40kV/cm, umber of pulse is 5-8, and supernatant is taken to carry out the operation of step S04.
It in the embodiment of the present invention, is handled using high-pressure pulse electric, can fully extract the cinnamon essential oil in Chinese cassia tree raw material,
Realize the efficient utilization of Chinese cassia tree raw material.
In the embodiment of the present invention, in step S04, the solvent for extracting use includes ethyl alcohol, methanol, acetone, n-butanol and stone
At least one of oily ether, the time of repose of extraction is 10-30min.Optionally, the number of extraction is 2-4 times, repeatedly after extraction
Merge organic phase.Optionally, the volume of the solvent used is extracted as the crude product and the 1/4- of the extracting solution A mixed volumes
2 times, it is chosen as 1/4.
In step S04, the pH of the buffer solution is 6.0-7.0；It is preferred that the acidic buffer that it is 6.0 that the buffer solution, which is pH,
Liquid.The buffer solution that the present invention uses can be acid-base buffer conventional in industry, acid condition optimization citric acid buffer solution
Or acetate buffer solution, but not limited to this.Optionally, the buffer solution can be in industry conventional acid-base buffer with it is organic molten
Mixed solution (the volume ratio 1 of agent:1-1:4, preferably 3:7).Wherein, organic solvent is preferably in methanol, ethyl alcohol or acetone
It is one or more, but not limited to this.
In step S04, the macroreticular resin includes one kind in polarity, middle polarity, low pole and non-polar macroporous resin
It is or a variety of.Optionally, the polar macroporous resin is preferably one or more in NKA-9, S8 and HPD500.The middle polarity
Macroreticular resin polarity be preferably it is one or more in HPD850, HPD750 and HPD400A, but not limited to this.Preferably, it is described
Low pole macroreticular resin polarity be preferably it is one or more in AB-8, HPD450 and HPD722, but not limited to this.The non-pole
Property macroreticular resin polarity be preferably it is one or more in D3520, D4020, X-5 and NKA, but not limited to this.Optionally, it is described
Macroreticular resin is HPD500 or AB-8 macroreticular resins.
In step S04, the time that macroreticular resin is used to be adsorbed is 0.5-2 hour.Described uses macropore
When resin is adsorbed, the dosage of the macroreticular resin is added in following ratio：1g macroreticular resins/20-50mL crude extracts.
In step S04, the eluent includes the buffer solution that pH is 3.0-10.0, and further preferably pH is 9.0
Alkaline buffer solution.The eluent that the present invention uses can be acid-base buffer conventional in industry, the preferred lemon of acid condition
Acid buffering solution or acetate buffer solution, but not limited to this；Alkaline condition is preferably buffered using ammonia-ammonium chloride buffer or sodium carbonate
Liquid, but not limited to this.
In step S04, the time of elution is 2-4h.
By the extracting method of the macroreticular resin of step (4), the cinnamon essential oil that purity is up to more than 70% can be obtained, it can
Convenient for follow-up further purification process.
In the embodiment of the present invention, in step S05, the method for the chromatogram purification includes high-speed countercurrent chromatography.Can carry out
High-speed countercurrent chromatography carries out chromatogram purification twice.Optionally, the high speed adverse current chromatogram condition is as follows：Rotating speed is 500-
1200rpm；Temperature is 16-34 DEG C；Flow velocity is 1-3ml/min；Separation solvent is A-B- aqueous systems, and the A is chloroform, dichloromethane
Alkane, dichloroethanes or tetrachloromethane；The B is methanol or ethyl alcohol；In the separation solvent, the volumn concentration of the A is
The volumn concentration of 20%-70%, the B are 5%-60%, and the volumn concentration of the water is 5%-50%.
The cinnamon essential oil that method through the embodiment of the present invention is extracted be deep yellow brown oil fluid, good fluidity,
Fragrance and taste are strong.The cinnamon essential oil quality illustrated is preferable.Meanwhile in cinnamon essential oil made from the embodiment of the present invention
Main mite killing ingredient eugenol kind compound content is higher, can perform well in mite-killing preparation.Therefore, the embodiment of the present invention
The extracting method extraction efficiency of the cinnamon essential oil of offer is higher.
Embodiment 1：
A kind of extracting method of cinnamon essential oil for mite killing, includes the following steps：
(1) Chinese cassia tree raw material is taken, Chinese cassia tree raw material is subjected to freeze-drying process, concrete operations include：
(a) eutectic point of Chinese cassia tree raw material is measured, is filled in material disc after measure；
(b) and then by material disc it is put into cool chamber, cool chamber temperature is adjusted to pre-freeze junction temperature, is kept for 3.5 hours,
Pre-freeze junction temperature is less than 10 DEG C of eutectic temperature；
(c) lyophilization will be carried out in prefreezing treated Chinese cassia tree raw material merging dry vacuum container, dry vacuum container is true
Reciprocal of duty cycle maintains 0.3KPa, the heat supply into dry vacuum container, and maximum temperature is controlled at 50 DEG C, when temperature of charge reaches setting highest
During temperature, stop heating；
(d) vacuum of breaking vacuum dryness storehouse takes out Chinese cassia tree raw material.
(2) after step (1) treated Chinese cassia tree raw material is crushed, 80 mesh sieve is crossed, water is added in and complex enzyme is digested, obtain
It to enzymolysis liquid, is filtered after enzyme deactivation, collects filtrate and filter residue；Filtrate obtains extracting solution A after centrifugation；Complex enzyme is including weight ratio
4:2:1 cellulase, pectase and zytase, the addition weight of complex enzyme are the 0.5% of Chinese cassia tree raw material weight, and water adds
Add weight is 3 times of Chinese cassia tree raw material weight；Hydrolysis temperature is 55 DEG C, and enzymolysis time 2h, filtrate obtains extracting solution after centrifugation
A, centrifugal force 4000g, centrifugation time 8min.
(3) neopelex and water are added in filter residue, then carries out being heated to boiling being distilled, during distillation
Between for 1h, collection obtains condensate liquid, and by condensate liquid centrifugation, crude product is obtained after water-oil separating；The addition of surfactant
Weight is the 0.5% of filter residue weight, and the addition weight of water is 10 times of filter residue weight.
(4) crude product and extracting solution A are mixed, is extracted using ethyl alcohol, extraction times are 2 times, during the standing extracted every time
Between for 10min, merge organic phase, be dissolved in after organic phase is evaporated in the citric acid solution that pH is 6.0, slightly carried
Liquid adsorbs gained crude extract using HPD500 macroreticular resins, and the time of macroporous resin adsorption is 0.5 hour.Macropore tree
The dosage of fat is added in following ratio：1g macroreticular resins/20mL crude extracts.Then it is eluted using eluent, is slightly carried
Take object；Eluent is ammonia-ammonium chloride buffer that pH is 9.0, and the time of elution is 2h.
(5) crude extract using high-speed countercurrent chromatography is purified, obtains the cinnamon essential oil for mite killing.High-speed counter-current color
Spectral condition is as follows：Rotating speed is 500rpm；Temperature is 16 DEG C；Flow velocity is 1ml/min；Separation solvent is A-B- aqueous systems, and A is chlorine
It is imitative；B is methanol；The volumn concentration of A is 20%；The volumn concentration of B is 60%；The volumn concentration of water is
20%.
Embodiment 2：
A kind of extracting method of cinnamon essential oil for mite killing, includes the following steps：
(1) Chinese cassia tree raw material is taken, Chinese cassia tree raw material is subjected to freeze-drying process, concrete operations include：
(a) eutectic point of Chinese cassia tree raw material is measured, is filled in material disc after measure；
(b) and then by material disc it is put into cool chamber, cool chamber temperature is adjusted to pre-freeze junction temperature, kept for 5 hours, in advance
Solidification point is less than 20 DEG C of eutectic temperature；
(c) lyophilization will be carried out in prefreezing treated Chinese cassia tree raw material merging dry vacuum container, dry vacuum container is true
Reciprocal of duty cycle maintains 0.4KPa, the heat supply into dry vacuum container, and maximum temperature is controlled at 50 DEG C, when temperature of charge reaches setting highest
During temperature, stop heating；
(d) vacuum of breaking vacuum dryness storehouse takes out Chinese cassia tree raw material.
(2) it after step (1) treated Chinese cassia tree raw material is crushed, sieves with 100 mesh sieve, adds in water and complex enzyme is digested,
Enzymolysis liquid is obtained, is filtered after enzyme deactivation, collects filtrate and filter residue；Filtrate obtains extracting solution A after centrifugation；Complex enzyme includes weight ratio
It is 5:5:1 cellulase, pectase and zytase, the addition weight of complex enzyme are the 0.1% of Chinese cassia tree raw material weight, water
Add 6 times that weight is Chinese cassia tree raw material weight；Hydrolysis temperature is 60 DEG C, and enzymolysis time 0.5h, filtrate is carried after centrifugation
Take liquid A, centrifugal force 6000g, centrifugation time 5min.
(3) neopelex and water are added in filter residue, then carries out being heated to boiling being distilled, during distillation
Between for 3h, collection obtains condensate liquid, and by condensate liquid centrifugation, crude product is obtained after water-oil separating；The addition of surfactant
Weight is the 1.0% of filter residue weight, and the addition weight of water is 15 times of filter residue weight.
(4) crude product and extracting solution A are mixed, is extracted using ethyl alcohol, extraction times are 2 times, during the standing extracted every time
Between for 30min, merge organic phase, be dissolved in after organic phase is evaporated in the citric acid solution that pH is 6.0, slightly carried
Liquid adsorbs gained crude extract using AB-8 macroreticular resins, and the time of macroporous resin adsorption is 2 hours.Macroreticular resin
Dosage is added in following ratio：1g macroreticular resins/50mL crude extracts.Then it is eluted using eluent, obtains crude extract；
Eluent is ammonia-ammonium chloride buffer that pH is 9.0, and the time of elution is 4h.
(5) crude extract using high-speed countercurrent chromatography is purified, obtains the cinnamon essential oil for mite killing.High-speed counter-current color
Spectral condition is as follows：Rotating speed is 1200rpm；Temperature is 34 DEG C；Flow velocity is 3ml/min；Separation solvent is A-B- aqueous systems, and A is chlorine
It is imitative；B is methanol；The volumn concentration of A is 70%；The volumn concentration of B is 10%；The volumn concentration of water is
20%.
Embodiment 3：
A kind of extracting method of cinnamon essential oil for mite killing, includes the following steps：
(1) Chinese cassia tree raw material is taken, Chinese cassia tree raw material is subjected to freeze-drying process, concrete operations include：
(a) eutectic point of Chinese cassia tree raw material is measured, is filled in material disc after measure；
(b) and then by material disc it is put into cool chamber, cool chamber temperature is adjusted to pre-freeze junction temperature, kept for 4 hours, in advance
Solidification point is less than 15 DEG C of eutectic temperature；
(c) lyophilization will be carried out in prefreezing treated Chinese cassia tree raw material merging dry vacuum container, dry vacuum container is true
Reciprocal of duty cycle maintains 0.35KPa, the heat supply into dry vacuum container, and maximum temperature is controlled at 50 DEG C, when temperature of charge reaches setting most
During high-temperature, stop heating；
(d) vacuum of breaking vacuum dryness storehouse takes out Chinese cassia tree raw material.
(2) after step (1) treated Chinese cassia tree raw material is crushed, 90 mesh sieve is crossed, water is added in and complex enzyme is digested, obtain
It to enzymolysis liquid, is filtered after enzyme deactivation, collects filtrate and filter residue；Filtrate obtains extracting solution A after centrifugation；Complex enzyme is including weight ratio
1:1:1 cellulase, pectase and zytase, the addition weight of complex enzyme are the 0.1% of Chinese cassia tree raw material weight, and water adds
Add weight is 4 times of Chinese cassia tree raw material weight；Hydrolysis temperature is 56 DEG C, and enzymolysis time 1h, filtrate obtains extracting solution after centrifugation
A, centrifugal force 7000g, centrifugation time 7min.
(3) neopelex and water are added in filter residue, then carries out being heated to boiling being distilled, during distillation
Between for 2h, collection obtains condensate liquid, and by condensate liquid centrifugation, crude product is obtained after water-oil separating；The addition of surfactant
Weight is the 5.0% of filter residue weight, and the addition weight of water is 12 times of filter residue weight.
(4) crude product and extracting solution A are mixed, adds in isometric ethyl alcohol, centrifuged after high-pressure pulse electric is handled, electricity
Field intensity is 20kV/cm, and umber of pulse is 8, takes supernatant.
(5) supernatant is extracted using ethyl alcohol, extraction times are 3 times, and the time of repose extracted every time is 20min, is merged
Organic phase is dissolved in the citric acid solution that pH is 6.0 after organic phase is evaporated, crude extract is obtained, by gained crude extract
It is adsorbed using AB-8 macroreticular resins, the time of macroporous resin adsorption is 2 hours.The dosage of macroreticular resin is added in following ratio
Add：1g macroreticular resins/30mL crude extracts.Then it is eluted using eluent, obtains crude extract；Eluent is that pH is 9.0
Ammonia-ammonium chloride buffer, time of elution is 3h.
(6) crude extract using high-speed countercurrent chromatography is purified, obtains the cinnamon essential oil for mite killing.High-speed counter-current color
Spectral condition is as follows：Rotating speed is 1000rpm；Temperature is 30 DEG C；Flow velocity is 2ml/min；Separation solvent is A-B- aqueous systems, and A is chlorine
It is imitative；B is methanol；The volumn concentration of A is 50%；The volumn concentration of B is 5%；The volumn concentration of water is 45%.
Embodiment described above only expresses the several embodiments of the present invention, and description is more specific and detailed, but simultaneously
Cannot the limitation to the scope of the claims of the present invention therefore be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect range.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. the extracting method of a kind of cinnamon essential oil for mite killing, which is characterized in that include the following steps：
(1) Chinese cassia tree raw material is taken, the Chinese cassia tree raw material is subjected to freeze-drying process；
(2) it after step (1) treated Chinese cassia tree raw material is crushed, adds in solvent and complex enzyme is digested, obtain enzymolysis liquid, go out
It is filtered after enzyme, collects filtrate and filter residue；The filtrate obtains extracting solution A after centrifugation；
(3) surfactant is added in the filter residue, then carries out heating distillation, collection obtains condensate liquid, by condensate liquid from
The heart precipitates, and crude product is obtained after water-oil separating；
(4) crude product and the extracting solution A are mixed, organic phase is taken after extraction, is dissolved after the organic phase is evaporated
In buffer solution, crude extract is obtained, gained crude extract using macroreticular resin is adsorbed, is then washed using eluent
It is de-, obtain crude extract；
(5) crude extract is obtained into the cinnamon essential oil for mite killing using chromatogram purification.
2. the extracting method of cinnamon essential oil as described in claim 1, which is characterized in that complex enzyme includes described in step (2)
Cellulase, pectase and zytase, wherein, the weight ratio of the cellulase, the pectase and the zytase
For 1-5:1-5:1, the addition weight of the complex enzyme is the 0.1%-0.5% of the Chinese cassia tree raw material weight.
3. the extracting method of cinnamon essential oil as described in claim 1, which is characterized in that surfactant described in step (3)
Including C8-C20Cationic surfactant, C8-C20Anion surfactant and C8-C20Nonionic surfactant
In it is one or more, the addition weight of the surfactant is the 0.1%-10% of the filter residue weight.
4. the extracting method of cinnamon essential oil as claimed in claim 3, which is characterized in that the surfactant includes dodecane
Base benzene sulfonic acid sodium salt, Tween-80, sldium lauryl sulfate, dodecyl sodium sulfate, hexadecyltrimethylammonium chloride, octadecyl
It is one or more in trimethyl ammonium chloride and odium stearate.
5. the extracting method of cinnamon essential oil as described in claim 1, which is characterized in that between step (3) and step (4),
At least one of the crude product and the extracting solution A are subjected to high-pressure pulse electric processing, at the high-pressure pulse electric
Reason carries out in accordance with the following methods：
At least one of the crude product and the extracting solution A are added in isometric ethyl alcohol, carry out high-voltage pulse electric
Field processing, electric field strength 20-40kV/cm, umber of pulse are 5-8, and supernatant is taken to continue the behaviour of step (4) after centrifugation
Make.
6. the extracting method of cinnamon essential oil as described in claim 1, which is characterized in that in step (4), the macroreticular resin packet
It includes one or more in polarity, middle polarity, low pole and non-polar macroporous resin.
7. the extracting method of cinnamon essential oil as claimed in claim 6, which is characterized in that the macroreticular resin for HPD500 or
AB-8 macroreticular resins.
8. the extracting method of cinnamon essential oil as described in claim 1, which is characterized in that adsorbed using the macroreticular resin
Time for 0.5-2 hours, the dosage of the macroreticular resin is added in following ratio：1g macroreticular resins/20-50mL crude extracts.
9. the extracting method of cinnamon essential oil as described in claim 1, which is characterized in that in step (5), the chromatogram purification
Method includes high-speed countercurrent chromatography, and the high speed adverse current chromatogram condition is as follows：Rotating speed is 500-1200rpm；Temperature is 16-34
℃；Flow velocity is 1-3ml/min；Separation solvent is A-B- aqueous systems, and the A is chloroform, dichloromethane, dichloroethanes or four chloromethanes
Alkane；The B is methanol or ethyl alcohol；In the separation solvent, the volumn concentration of the A is 20%-70%, the body of the B
Product percentage composition is 5%-60%, and the volumn concentration of the water is 5%-50%.
10. the extracting method of cinnamon essential oil as described in claim 1, which is characterized in that in step (1), the freeze-drying
Processing operates in accordance with the following methods：
(1) eutectic point of Chinese cassia tree raw material is measured, is filled in material disc after measure；
(2) material disc is put into cool chamber, the cool chamber temperature is adjusted to pre-freeze junction temperature, keep 3.5-5 small
When, the pre-freeze junction temperature is the temperature less than 10-20 DEG C of the eutectic temperature；
(3) lyophilization will be carried out in prefreezing treated Chinese cassia tree raw material merging dry vacuum container, the dry vacuum container is true
Reciprocal of duty cycle maintains 0.3-0.4KPa, the heat supply into dry vacuum container, and maximum temperature is controlled at 50 DEG C, when temperature of charge reaches setting
During maximum temperature, stop heating；
(4) vacuum of breaking vacuum dryness storehouse takes out Chinese cassia tree raw material.
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| CN116396802A (en) * | 2023-04-26 | 2023-07-07 | 广州华锦香料科技有限公司 | Production process for preparing essential oil by enzymolysis method |
| WO2024109436A1 (en) * | 2022-11-21 | 2024-05-30 | 华南理工大学 | Method for accurately-controlled fractional extraction of bioactive substances from kaempferia elegans by using high-voltage pulse electric field |
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