CN110041178A - The method of rectifying extraction isoesdragol - Google Patents
The method of rectifying extraction isoesdragol Download PDFInfo
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- CN110041178A CN110041178A CN201910338344.6A CN201910338344A CN110041178A CN 110041178 A CN110041178 A CN 110041178A CN 201910338344 A CN201910338344 A CN 201910338344A CN 110041178 A CN110041178 A CN 110041178A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/38—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/40—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/46—Use of additives, e.g. for stabilisation
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Abstract
The invention discloses a kind of methods that isoesdragol is extracted in rectifying, this method comprises: being uniformly mixed after salt is added into Chinese anise tender leaf, then through parch, immersion, filtering, obtain mixed liquor, then dry soya bean is added into mixed liquor, refilters, heat, refilter, obtain miscella, again by miscella through distillation, stratification, extract is obtained, then extract is placed in extractive distillation column and is handled, extract is obtained, extract is removed water, isoesdragol is obtained.Operation of the present invention method is simple, and organic reagent is not used in extracting method, to reduce the probability that organic reagent is mixed into isoesdragol, the present invention does not use recrystallizing technology, but uses rectifying extraction process, improves the yield of isoesdragol.
Description
Technical field
The present invention relates to field of agricultural products processing.It is more particularly related to which isoesdragol is extracted in a kind of rectifying
Method.
Background technique
Illiciumverum is the distinctive fragrant plant in China, is grown in the ground such as Guangxi, Guangdong, Yunnan, Fujian, Sichuan, mainly with wide
The yield in west is most, and quality is best, and the main place of production in Guangxi concentrates on south Guangxi and western part, including Chongzuo, Port of Fangcheng, admires
The cities such as state, Baise, Nanning, Yulin, Wuzhou are especially reached the clouds with Shiwan Dashan area, Debao best in quality, most famous.China
Octagonal annual output be 100,000 tons or so, account for Gross World Product 80~90%, and Guangxi accounts for national total output 85% or so, Guangxi
Township as qualified illiciumverum.It is octagonal also to export the ground such as the U.S., Europe, Japan, Southeast Asia in addition to meeting domestic demand
Area is always important traditional agricultural product that China's export is earned foreign exchange.By 2006, the cultivated area of Guangxi District illiciumverum was up to 1,530,000
Mu, becomes the maximum Chinese anise medicinal material in China and oil of badian distribution centre by 79679 tons of annual output.The Chinese anise in Guangxi
It at home and abroad enjoys high reputation in the market, is known as the laudatory title in " township of world's illiciumverum ".
Mature dry octagonal fruit contains aromatic oil, fat, protein, resin etc., is that important " medicine food is same in China
The industrial crops in source ", have appetizer under the gas, warm stomach cold dispelling and other effects, while be also common fragrance, be highclass perfumes, perfumed soap,
The indispensable important fragrance such as beverage, food, tobacco, toothpaste, cosmetics.The illiciumverum about 95% that China consumes at present is used for
Fragrance, 5% make it is medicinal.
The yield of octagonal effective component illiciumverum anise-oil is usually the 5~12% of anistree yield, and content and property are because of eight
Angle type, weather conditions, environmental factor, processing extraction technique are different and different.Octagonal anise-oil is in 20 DEG C or more Shi Weiwu
Color is transparent or faint yellow working fluid, the characteristic perfume fragrance with Chinese anise.Volatile flavor component master in octagonal anise-oil
It to be made of anethole, monoterpenes, monoterpene type oxide, sesquiterpenoids.It is trans-anethole that wherein content is highest,
Up to 80% or so, there are also limonene, carypohyllene, cis anethol, chavicol methyl ether, anisaldehyde, aromatic alcohol, pine tars for other ingredients
Alcohol, α~firpene, borneol etc., in addition to cis anethol, all ingredients are the effective and values of fragrance and food industry
Substance, together constitute the unique perfume and flavor of oil of badian.Cis anethol is that same point of trans-anethole is different
The component that must be limited and remove in structure body and isoesdragol product, the reason is that the component has certain toxicity, to human body
Health is unfavorable.Cis anethol content is no more than in existing isoesdragol product food additives national Specification product
0.2%.
The extraction raw material of oil of badian can be real for octagonal fruit, can also mention using pericarp, seed, branches and leaves as raw material
It takes.Currently, effective extracting method of oil of badian generally uses organic solvent extractionprocess, such as ethanol solution, methanol solution, third
Ketone etc., but there is the problem of solvent residual for being difficult to eliminate in organic solvent method, be not suitable for making fragrance and food addition uses.
Summary of the invention
It is an object of the invention to solve at least the above problems, and provide the advantages of at least will be described later.
It is an object of the present invention to provide a kind of methods that isoesdragol is extracted in rectifying, this method comprises: to Chinese anise
It is uniformly mixed after salt is added in tender leaf, then through parch, immersion, filtering, obtains mixed liquor, dry Huang is then added into mixed liquor
Beans are refiltered, heat, are refiltered, and are obtained miscella, then miscella is obtained extract through distillation, stratification, then will be extracted
Object is placed in extractive distillation column and handles, and obtains extract, and extract is removed water, and obtains isoesdragol.Operation of the present invention method is simple, mentions
It takes and organic reagent is not used in method, to reduce the probability that organic reagent is mixed into isoesdragol, the present invention is not used and tied again
Brilliant technique, but rectifying extraction process is used, improve the yield of isoesdragol.
In order to realize purposes and other advantages according to the present invention, a kind of method that isoesdragol is extracted in rectifying is provided,
Characterized by comprising the following steps:
S1, the cleaning of Chinese anise tender leaf, drying are taken, salt is then added and is uniformly mixed, then is placed in parch 10 at 80~90 DEG C
~15min is subsequently placed in 5~8min of parch at 120~135 DEG C, then is placed in 10~15min of parch at 100~120 DEG C, must dry
Object is fried, is soaked in water after parch object is crushed, then be placed in 4~6h of ultrasonication under 55~75 DEG C and 25~40KHz, then
It is placed in 40~60min of ultrasonication under 100~110 DEG C and 25~40kHz, obtains mixture, mixture is placed in 30~50 DEG C
After lower filtering, the lower object of filter is taken, mixed liquor is obtained, wherein the octagonal weight ratio with salt is 7:1；
S2, dry soya bean is added into mixed liquor, then be placed at 30~45 DEG C with the speed of 50~100r/min stirring 2~
Then 4h is filtered, take the lower object of filter, obtain treatment fluid, zeolite is added into treatment fluid, be placed at 105~125 DEG C and be heated to anhydrous steaming
After gas evolution, filtering takes the lower object of filter, obtains miscella, wherein the weight ratio of mixed liquor and dry soya bean is 9:4, treatment fluid and zeolite
Weight ratio be 9:2；
S3, miscella is placed under 100~130 DEG C and the vacuum degree of 8~10mmHg after 4~6h of distillation, collects vapor
After cool down, obtain distillate, salt be added into distillate and is placed on stratification at 25~30 DEG C, takes upper liquid dry, must mention
Take object, wherein the weight ratio of distillate and salt is 7:2；
S4, heating extractive distillation column to tower top temperature rise to 125~150 DEG C, and column bottom temperature rises to 125~150 DEG C, then will
Extract is fed from the middle part of extractive distillation column, and extractant is fed from the top of extractive distillation column, and the reflux ratio of extracting rectifying is 2
~4:1 obtains extract, extract is removed water, obtain isoesdragol, wherein the weight of extract and extractant after extracting 4~6h
Than for 1:3.
Preferably, the method that isoesdragol is extracted in the rectifying, drying course in step S1 are as follows: illiciumverum that will be clean
It is placed in 30~60min of placement under 70~85 DEG C and the wind speed of 5~8m/s, then is placed under 25~40 DEG C and the wind speed of 15~20m/s
After placing 10~20min, 20~30min is then placed at 5~10 DEG C, then be placed under 70~85 DEG C and the wind speed of 5~8m/s
10~20min is placed, is subsequently placed in after placing 10~15min at 110~125 DEG C, then be placed in 25~40 DEG C and 15~20m/s
10~20min is placed under wind speed.
Preferably, the method that isoesdragol is extracted in the rectifying, parch object after the pulverizing, is soaked in step S1
Cellulase and bamboo extractive are added before in water, wherein the weight ratio of parch object and cellulase, bamboo extractive is 8:
1:2, bamboo extractive the preparation method is as follows: the leaf of bamboo is taken to clean up after, cover wet cotton and be placed at 30~40 DEG C and place 1
~2h, then wet cotton is removed, it is subsequently placed in water and boils 2~4h, filter, take the lower object of filter, obtain filtered fluid, filtered fluid is placed in 45
It is concentrated under reduced pressure under~60 DEG C and 0.06~0.08Mpa, is dry, wherein wet cotton is immersed in 5 in rice washing water before covering the leaf of bamboo
After~8min, taking-up is wrung out to not dripping.
Preferably, the method that isoesdragol is extracted in the rectifying, cellulase are swashed before parch object is added
It is living, the concrete operations of activation are as follows: cellulase is placed at -20 DEG C and freezes 10-16h, then takes out and MgCl is added2Solid powder
End, then it is placed in 5~8min of water-bath at 45~50 DEG C, wherein cellulase and MgCl2The weight ratio of solid powder is 7:2.
Preferably, the method that isoesdragol is extracted in the rectifying, in S4 extractant include citric acid, sodium soap,
One or more of Epoxysuccinic acid potassium, sodium benzoate.
Preferably, the method that isoesdragol is extracted in the rectifying, extract liquor removal process in S4 are as follows: into extract liquor
The discoloration silica gel for accounting for extract liquor parts by weight 10~20% is added, then is placed at 30~40 DEG C and is stirred with the speed of 100~200r/min
30~60min is mixed, is then filtered, the lower object of filter is taken, obtains isoesdragol.
The present invention is include at least the following beneficial effects: it is uniformly mixed after salt is added into Chinese anise tender leaf in the present invention,
Again through parch, immersion, filtering, mixed liquor is obtained, dry soya bean is then added into mixed liquor, refilters, heat, refilter, is obtained mixed
Oil is closed, then miscella is obtained extract, then extract is placed in extractive distillation column and is handled, must extracted through distillation, stratification
Object is taken, extract is removed water, obtains isoesdragol.Operation of the present invention method is simple, and organic reagent is not used in extracting method, thus
Reduce the probability that organic reagent is mixed into isoesdragol, improve the use scope of isoesdragol, enhances the warp of isoesdragol
Ji value；It joined salt before parch Chinese anise tender leaf again in the present invention, can effectively destroy the cell of Chinese anise tender leaf, allow cell
Content evolution, improves subsequent extraction efficiency；Dry soya bean is added in the present invention into mixed liquor, can effectively remove in mixed liquor
Moisture, reduce distillation water removal and caused by mixed liquor effective component loss.
Further advantage, target and feature of the invention will be partially reflected by the following instructions, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Specific embodiment
The present invention will be further described in detail below with reference to the embodiments, to enable those skilled in the art referring to specification
Text can be implemented accordingly.
It should be noted that experimental method described in following embodiments is unless otherwise specified conventional method, it is described
Reagent and material commercially obtain unless otherwise specified.
Embodiment 1:
The method of rectifying extraction isoesdragol, comprising the following steps:
S1, the cleaning of Chinese anise tender leaf, drying are taken, salt are then added and is uniformly mixed, then is placed in parch 10min at 80 DEG C,
It is subsequently placed in parch 5min at 120 DEG C, then is placed in parch 10min at 100 DEG C, obtains parch object, is soaked in after parch object is crushed
In water, then it is placed in ultrasonication 4h under 55 DEG C and 25KHz, is subsequently placed in ultrasonication 40min under 100 DEG C and 25kHz, obtains
Mixture is placed at 30 DEG C after filtering by mixture, is taken the lower object of filter, is obtained mixed liquor, wherein the octagonal weight ratio with salt is 7:
1；
S2, dry soya bean is added into mixed liquor, then is placed at 30 DEG C and 2h is stirred with the speed of 50r/min, then filter, take
Lower object is filtered, treatment fluid is obtained, zeolite is added into treatment fluid, is placed at 105 DEG C after being heated to anhydrous steam evolution, filtering takes filter
Lower object, obtains miscella, wherein the weight ratio of mixed liquor and dry soya bean is 9:4, and the weight ratio for the treatment of fluid and zeolite is 9:2；
S3, miscella is placed under 100 DEG C and the vacuum degree of 8mmHg after distillation 4h, collects cooling after vapor, must distills
Liquid is added salt into distillate and is placed on stratification at 25 DEG C, takes upper liquid dry, obtain extract, wherein distillate with
The weight ratio of salt is 7:2；
S4, heating extractive distillation column to tower top temperature rise to 125 DEG C, and column bottom temperature rises to 125 DEG C, then by extract from extraction
The middle part of rectifying column is taken to feed, citric acid is fed from the top of extractive distillation column, and the reflux ratio of extracting rectifying is 2:1, extracts 4h
Afterwards, extract is obtained, extract is removed water, obtains isoesdragol, wherein the weight ratio of extract and citric acid is 1:3.
Embodiment 2:
The method of rectifying extraction isoesdragol, comprising the following steps:
S1, the cleaning of Chinese anise tender leaf, drying are taken, salt are then added and is uniformly mixed, then is placed in parch 15min at 90 DEG C,
It is subsequently placed in parch 8min at 135 DEG C, then is placed in parch 15min at 120 DEG C, obtains parch object, is soaked in after parch object is crushed
In water, then it is placed in ultrasonication 6h under 75 DEG C and 40KHz, is subsequently placed in ultrasonication 60min under 110 DEG C and 40kHz, obtains
Mixture is placed at 50 DEG C after filtering by mixture, is taken the lower object of filter, is obtained mixed liquor, wherein the octagonal weight ratio with salt is 7:
1；
S2, dry soya bean is added into mixed liquor, then is placed at 45 DEG C and 4h is stirred with the speed of 100r/min, then filter,
The lower object of filter is taken, treatment fluid is obtained, zeolite is added into treatment fluid, be placed at 125 DEG C after being heated to anhydrous steam evolution, filtering takes
Lower object is filtered, miscella is obtained, wherein the weight ratio of mixed liquor and dry soya bean is 9:4, and the weight ratio for the treatment of fluid and zeolite is 9:2；
S3, miscella is placed under 130 DEG C and the vacuum degree of 10mmHg after distillation 6h, collects cooling after vapor, must steams
Distillate is added salt into distillate and is placed on stratification at 30 DEG C, takes upper liquid dry, obtains extract, wherein distillate
Weight ratio with salt is 7:2；
S4, heating extractive distillation column to tower top temperature rise to 150 DEG C, and column bottom temperature rises to 150 DEG C, then by extract from extraction
The middle part of rectifying column is taken to feed, citric acid is fed from the top of extractive distillation column, and the reflux ratio of extracting rectifying is 4:1, extracts 6h
Afterwards, extract is obtained, extract is removed water, obtains isoesdragol, wherein the weight ratio of extract and citric acid is 1:3.
Embodiment 3:
The method of rectifying extraction isoesdragol, comprising the following steps:
S1, the cleaning of Chinese anise tender leaf, drying are taken, salt are then added and is uniformly mixed, then is placed in parch 12min at 85 DEG C,
It is subsequently placed in parch 6min at 128 DEG C, then is placed in parch 12min at 110 DEG C, obtains parch object, is soaked in after parch object is crushed
In water, then it is placed in ultrasonication 5h under 65 DEG C and 32KHz, is subsequently placed in ultrasonication 50min under 105 DEG C and 32kHz, obtains
Mixture is placed at 40 DEG C after filtering by mixture, is taken the lower object of filter, is obtained mixed liquor, wherein the octagonal weight ratio with salt is 7:
1；
S2, dry soya bean is added into mixed liquor, then is placed at 36 DEG C and 3h is stirred with the speed of 75r/min, then filter, take
Lower object is filtered, treatment fluid is obtained, zeolite is added into treatment fluid, is placed at 115 DEG C after being heated to anhydrous steam evolution, filtering takes filter
Lower object, obtains miscella, wherein the weight ratio of mixed liquor and dry soya bean is 9:4, and the weight ratio for the treatment of fluid and zeolite is 9:2；
S3, miscella is placed under 115 DEG C and the vacuum degree of 9mmHg after distillation 5h, collects cooling after vapor, must distills
Liquid is added salt into distillate and is placed on stratification at 28 DEG C, takes upper liquid dry, obtain extract, wherein distillate with
The weight ratio of salt is 7:2；
S4, heating extractive distillation column to tower top temperature rise to 136 DEG C, and column bottom temperature rises to 136 DEG C, then by extract from extraction
The middle part of rectifying column is taken to feed, citric acid is fed from the top of extractive distillation column, and the reflux ratio of extracting rectifying is 3:1, extracts 5h
Afterwards, extract is obtained, extract is removed water, obtains isoesdragol, wherein the weight ratio of extract and citric acid is 1:3.
Embodiment 4:
The method of rectifying extraction isoesdragol, comprising the following steps:
S1, the cleaning of Chinese anise tender leaf, drying are taken, salt are then added and is uniformly mixed, then is placed in parch 12min at 85 DEG C,
It is subsequently placed in parch 6min at 128 DEG C, then is placed in parch 12min at 110 DEG C, obtains parch object, is soaked in after parch object is crushed
In water, then it is placed in ultrasonication 5h under 65 DEG C and 32KHz, is subsequently placed in ultrasonication 50min under 105 DEG C and 32kHz, obtains
Mixture is placed at 40 DEG C after filtering by mixture, is taken the lower object of filter, is obtained mixed liquor, wherein the octagonal weight ratio with salt is 7:
1, drying course are as follows: clean illiciumverum is placed under 78 DEG C and 6m/s of wind speed and places 45min, then be placed in 32 DEG C and 18m/s
After placing 15min under wind speed, 25min is then placed at 8 DEG C, then is placed under 78 DEG C and 6m/s of wind speed and places 15min, then
It is placed at 118 DEG C after placing 12min, then is placed under 32 DEG C and 18m/s of wind speed and places 15min；
S2, dry soya bean is added into mixed liquor, then is placed at 36 DEG C and 3h is stirred with the speed of 75r/min, then filter, take
Lower object is filtered, treatment fluid is obtained, zeolite is added into treatment fluid, is placed at 115 DEG C after being heated to anhydrous steam evolution, filtering takes filter
Lower object, obtains miscella, wherein the weight ratio of mixed liquor and dry soya bean is 9:4, and the weight ratio for the treatment of fluid and zeolite is 9:2；
S3, miscella is placed under 115 DEG C and the vacuum degree of 9mmHg after distillation 5h, collects cooling after vapor, must distills
Liquid is added salt into distillate and is placed on stratification at 28 DEG C, takes upper liquid dry, obtain extract, wherein distillate with
The weight ratio of salt is 7:2；
S4, heating extractive distillation column to tower top temperature rise to 136 DEG C, and column bottom temperature rises to 136 DEG C, then by extract from extraction
The middle part of rectifying column is taken to feed, citric acid is fed from the top of extractive distillation column, and the reflux ratio of extracting rectifying is 3:1, extracts 5h
Afterwards, extract is obtained, extract is removed water, obtains isoesdragol, wherein the weight ratio of extract and citric acid is 1:3.
Embodiment 5:
The method of rectifying extraction isoesdragol, comprising the following steps:
S1, the cleaning of Chinese anise tender leaf, drying are taken, salt are then added and is uniformly mixed, then is placed in parch 12min at 85 DEG C,
It is subsequently placed in parch 6min at 128 DEG C, then is placed in parch 12min at 110 DEG C, obtains parch object, is added after parch object is crushed fine
Plain enzyme and bamboo extractive are tieed up, is then soaked in water, then is placed in ultrasonication 5h under 65 DEG C and 32KHz, is subsequently placed in 105
DEG C and 32kHz under ultrasonication 50min, obtain mixture, mixture be placed at 40 DEG C after filtering, take the lower object of filter, must mix
Liquid, wherein the octagonal weight ratio with salt is 7:1；Drying course are as follows: be placed in clean illiciumverum under 78 DEG C and 6m/s of wind speed
45min is placed, then is placed under 32 DEG C and 18m/s of wind speed after placement 15min, 25min is then placed at 8 DEG C, then be placed in 78
DEG C and the wind speed of 6m/s under place 15min, be subsequently placed in after placing 12min at 118 DEG C, then be placed in the wind speed of 32 DEG C He 18m/s
Lower placement 15min；The weight ratio of parch object and cellulase, bamboo extractive is 8:1:2, and the preparation method of bamboo extractive is such as
Under: after taking the leaf of bamboo to clean up, covers wet cotton and be placed at 35 DEG C and place 1.5h, then remove wet cotton, be subsequently placed in water
3h is boiled, is filtered, the lower object of filter is taken, obtains filtered fluid, filtered fluid is placed under 52 DEG C and 0.07Mpa and is concentrated under reduced pressure, is dry, wherein
Wet cotton is immersed in rice washing water after 7min before covering the leaf of bamboo, and taking-up is wrung out to not dripping；
S2, dry soya bean is added into mixed liquor, then is placed at 36 DEG C and 3h is stirred with the speed of 75r/min, then filter, take
Lower object is filtered, treatment fluid is obtained, zeolite is added into treatment fluid, is placed at 115 DEG C after being heated to anhydrous steam evolution, filtering takes filter
Lower object, obtains miscella, wherein the weight ratio of mixed liquor and dry soya bean is 9:4, and the weight ratio for the treatment of fluid and zeolite is 9:2；
S3, miscella is placed under 115 DEG C and the vacuum degree of 9mmHg after distillation 5h, collects cooling after vapor, must distills
Liquid is added salt into distillate and is placed on stratification at 28 DEG C, takes upper liquid dry, obtain extract, wherein distillate with
The weight ratio of salt is 7:2；
S4, heating extractive distillation column to tower top temperature rise to 136 DEG C, and column bottom temperature rises to 136 DEG C, then by extract from extraction
The middle part of rectifying column is taken to feed, citric acid is fed from the top of extractive distillation column, and the reflux ratio of extracting rectifying is 3:1, extracts 5h
Afterwards, extract is obtained, extract is removed water, obtains isoesdragol, wherein the weight ratio of extract and citric acid is 1:3.
Embodiment 6:
The method of rectifying extraction isoesdragol, comprising the following steps:
S1, the cleaning of Chinese anise tender leaf, drying are taken, salt are then added and is uniformly mixed, then is placed in parch 12min at 85 DEG C,
It is subsequently placed in parch 6min at 128 DEG C, then is placed in parch 12min at 110 DEG C, obtains parch object, is added after parch object is crushed fine
Plain enzyme and bamboo extractive are tieed up, is then soaked in water, then is placed in ultrasonication 5h under 65 DEG C and 32KHz, is subsequently placed in 105
DEG C and 32kHz under ultrasonication 50min, obtain mixture, mixture be placed at 40 DEG C after filtering, take the lower object of filter, must mix
Liquid, wherein the octagonal weight ratio with salt is 7:1；Drying course are as follows: be placed in clean illiciumverum under 78 DEG C and 6m/s of wind speed
45min is placed, then is placed under 32 DEG C and 18m/s of wind speed after placement 15min, 25min is then placed at 8 DEG C, then be placed in 78
DEG C and the wind speed of 6m/s under place 15min, be subsequently placed in after placing 12min at 118 DEG C, then be placed in the wind speed of 32 DEG C He 18m/s
Lower placement 15min；The weight ratio of parch object and cellulase, bamboo extractive is 8:1:2, and the preparation method of bamboo extractive is such as
Under: after taking the leaf of bamboo to clean up, covers wet cotton and be placed at 35 DEG C and place 1.5h, then remove wet cotton, be subsequently placed in water
3h is boiled, is filtered, the lower object of filter is taken, obtains filtered fluid, filtered fluid is placed under 52 DEG C and 0.07Mpa and is concentrated under reduced pressure, is dry, wherein
Wet cotton is immersed in rice washing water after 7min before covering the leaf of bamboo, and taking-up is wrung out to not dripping；Parch is being added in cellulase
It is activated before object, the concrete operations of activation are as follows: cellulase is placed at -20 DEG C and freezes 13h, then takes out addition
MgCl2Solid powder, then it is placed in water-bath 7min at 48 DEG C, wherein cellulase and MgCl2The weight ratio of solid powder is 7:2；
S2, dry soya bean is added into mixed liquor, then is placed at 36 DEG C and 3h is stirred with the speed of 75r/min, then filter, take
Lower object is filtered, treatment fluid is obtained, zeolite is added into treatment fluid, is placed at 115 DEG C after being heated to anhydrous steam evolution, filtering takes filter
Lower object, obtains miscella, wherein the weight ratio of mixed liquor and dry soya bean is 9:4, and the weight ratio for the treatment of fluid and zeolite is 9:2；
S3, miscella is placed under 115 DEG C and the vacuum degree of 9mmHg after distillation 5h, collects cooling after vapor, must distills
Liquid is added salt into distillate and is placed on stratification at 28 DEG C, takes upper liquid dry, obtain extract, wherein distillate with
The weight ratio of salt is 7:2；
S4, heating extractive distillation column to tower top temperature rise to 136 DEG C, and column bottom temperature rises to 136 DEG C, then by extract from extraction
The middle part of rectifying column is taken to feed, citric acid is fed from the top of extractive distillation column, and the reflux ratio of extracting rectifying is 3:1, extracts 5h
Afterwards, extract is obtained, extract is removed water, obtains isoesdragol, wherein the weight ratio of extract and citric acid is 1:3.
Embodiment 7:
The method of rectifying extraction isoesdragol, comprising the following steps:
S1, the cleaning of Chinese anise tender leaf, drying are taken, salt are then added and is uniformly mixed, then is placed in parch 12min at 85 DEG C,
It is subsequently placed in parch 6min at 128 DEG C, then is placed in parch 12min at 110 DEG C, obtains parch object, is added after parch object is crushed fine
Plain enzyme and bamboo extractive are tieed up, is then soaked in water, then is placed in ultrasonication 5h under 65 DEG C and 32KHz, is subsequently placed in 105
DEG C and 32kHz under ultrasonication 50min, obtain mixture, mixture be placed at 40 DEG C after filtering, take the lower object of filter, must mix
Liquid, wherein the octagonal weight ratio with salt is 7:1；Drying course are as follows: be placed in clean illiciumverum under 78 DEG C and 6m/s of wind speed
45min is placed, then is placed under 32 DEG C and 18m/s of wind speed after placement 15min, 25min is then placed at 8 DEG C, then be placed in 78
DEG C and the wind speed of 6m/s under place 15min, be subsequently placed in after placing 12min at 118 DEG C, then be placed in the wind speed of 32 DEG C He 18m/s
Lower placement 15min；The weight ratio of parch object and cellulase, bamboo extractive is 8:1:2, and the preparation method of bamboo extractive is such as
Under: after taking the leaf of bamboo to clean up, covers wet cotton and be placed at 35 DEG C and place 1.5h, then remove wet cotton, be subsequently placed in water
3h is boiled, is filtered, the lower object of filter is taken, obtains filtered fluid, filtered fluid is placed under 52 DEG C and 0.07Mpa and is concentrated under reduced pressure, is dry, wherein
Wet cotton is immersed in rice washing water after 7min before covering the leaf of bamboo, and taking-up is wrung out to not dripping；Parch is being added in cellulase
It is activated before object, the concrete operations of activation are as follows: cellulase is placed at -20 DEG C and freezes 13h, then takes out addition
MgCl2Solid powder, then it is placed in water-bath 7min at 48 DEG C, wherein cellulase and MgCl2The weight ratio of solid powder is 7:2；
S2, dry soya bean is added into mixed liquor, then is placed at 36 DEG C and 3h is stirred with the speed of 75r/min, then filter, take
Lower object is filtered, treatment fluid is obtained, zeolite is added into treatment fluid, is placed at 115 DEG C after being heated to anhydrous steam evolution, filtering takes filter
Lower object, obtains miscella, wherein the weight ratio of mixed liquor and dry soya bean is 9:4, and the weight ratio for the treatment of fluid and zeolite is 9:2；
S3, miscella is placed under 115 DEG C and the vacuum degree of 9mmHg after distillation 5h, collects cooling after vapor, must distills
Liquid is added salt into distillate and is placed on stratification at 28 DEG C, takes upper liquid dry, obtain extract, wherein distillate with
The weight ratio of salt is 7:2；
S4, heating extractive distillation column to tower top temperature rise to 136 DEG C, and column bottom temperature rises to 136 DEG C, then by extract from extraction
The middle part of rectifying column is taken to feed, citric acid is fed from the top of extractive distillation column, and the reflux ratio of extracting rectifying is 3:1, extracts 5h
Afterwards, extract is obtained, the discoloration silica gel for accounting for extract liquor parts by weight 15% is added into extract liquor, then be placed at 35 DEG C with 150r/min
Speed stir 45min, then filter, take the lower object of filter, obtain isoesdragol, wherein the weight ratio of extract and citric acid is 1:
3。
Comparative example 1:
Preparation method is the same as embodiment 3, wherein unlike: mixed liquor is placed at 100 DEG C in S2 and is distilled to anhydrous steam
Evolution, obtains miscella.
Comparative example 2:
Preparation method is the same as embodiment 3, wherein unlike: miscella is placed in the vacuum degree of 115 DEG C He 9mmHg in S2
After lower distillation 5h, cooling after vapor is collected, distillate is obtained, distillate is placed in stratification at 28 DEG C, takes upper liquid dry,
Obtain extract.
Structural analysis:
Comparative example 1, comparative example 2, embodiment 3, the resulting isoesdragol of embodiment 7 are carried out to the ratio of organoleptic quality and yield
Compared with, wherein yield=m'/m of isoesdragol, m' are the weight of isoesdragol, and m is the weight of Chinese anise tender leaf, be the results are shown in Table
1。
The sense organ and yield of 1 isoesdragol of table
As known from Table 1, comparative example 1, comparative example 2, embodiment 3, the organoleptic quality of the resulting isoesdragol of embodiment 7 accord with
Market demands are closed, and the resulting isoesdragol of embodiment 7 is higher than other groups, has reached 13.5%, and dry Huang is not added in comparative example 1
Beans water removal, directly carries out distillation water removal, and vapor can take away effective component in distillation process, causes isoesdragol yield obtained
It is relatively low；Salt is not added in comparative example 2, distillate is directly placed in stratification at 28 DEG C, the similar density of distillate and water,
It is layered unobvious, middle layer is unobvious, removes middle layer during taking upper liquid, will cause the upper liquid liquid measure of acquirement
It is few, cause isoesdragol yield obtained relatively low；Embodiment 3 compared to the plain enzyme without added fiber of embodiment 7, octagonal tender leaf it is thin
Cell wall is thicker, and cellulase is needed to dissolve, and escapes cellular content, and cellulase is not used in embodiment 3, causes step S1
Obtained in mixed liquor effective component it is relatively low, the isoesdragol yield prepared by is relatively low.
In conclusion isoesdragol made from embodiment 3 and embodiment 7 meets market demands, compared to embodiment 3,
The yield with higher of embodiment 7.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details.
Claims (6)
1. the method for rectifying extraction isoesdragol, which comprises the following steps:
S1, take Chinese anise tender leaf cleaning, drying, then be added salt be uniformly mixed, then be placed in parch 10 at 80~90 DEG C~
15min is subsequently placed in 5~8min of parch at 120~135 DEG C, then is placed in 10~15min of parch at 100~120 DEG C, obtains parch
Object is soaked in water after crushing parch object, then is placed in 4~6h of ultrasonication under 55~75 DEG C and 25~40KHz, then sets
40~60min of ultrasonication, obtains mixture under 100~110 DEG C and 25~40kHz, and mixture is placed at 30~50 DEG C
After filtering, the lower object of filter is taken, mixed liquor is obtained, wherein the octagonal weight ratio with salt is 7:1；
S2, dry soya bean is added into mixed liquor, then is placed at 30~45 DEG C and 2~4h is stirred with the speed of 50~100r/min, so
After filter, take the lower object of filter, obtain treatment fluid, zeolite is added into treatment fluid, be placed at 105~125 DEG C and be heated to anhydrous steam ease
After out, filtering takes the lower object of filter, obtains miscella, wherein the weight ratio of mixed liquor and dry soya bean is 9:4, the weight for the treatment of fluid and zeolite
Amount is than being 9:2；
S3, miscella is placed under 100~130 DEG C and the vacuum degree of 8~10mmHg after 4~6h of distillation, it is cold after collection vapor
But, distillate is obtained, salt is added into distillate and is placed on stratification at 25~30 DEG C, takes upper liquid dry, obtains extract,
Wherein, the weight ratio of distillate and salt is 7:2；
S4, heating extractive distillation column to tower top temperature rise to 125~150 DEG C, and column bottom temperature rises to 125~150 DEG C, then will extract
Object is fed from the middle part of extractive distillation column, and extractant is fed from the top of extractive distillation column, and the reflux ratio of extracting rectifying is 2~4:
1, after extracting 4~6h, extract is obtained, extract is removed water, obtains isoesdragol, wherein the weight ratio of extract and extractant is
1:3。
2. the method that isoesdragol is extracted in rectifying as described in claim 1, which is characterized in that drying course in step S1 are as follows:
Clean illiciumverum is placed under 70~85 DEG C and the wind speed of 5~8m/s and places 30~60min, then be placed in 25~40 DEG C and 15~
After placing 10~20min under the wind speed of 20m/s, 20~30min is then placed at 5~10 DEG C, then be placed in 70~85 DEG C and 5~
10~20min is placed under the wind speed of 8m/s, is subsequently placed in after placing 10~15min at 110~125 DEG C, then be placed in 25~40 DEG C
With 10~20min of placement under the wind speed of 15~20m/s.
3. the method that isoesdragol is extracted in rectifying as claimed in claim 2, which is characterized in that parch object is crushing in step S1
Later, cellulase and bamboo extractive are added before being soaked in water, wherein parch object and cellulase, bamboo extractive
Weight ratio be 8:1:2, bamboo extractive the preparation method is as follows: the leaf of bamboo is taken to clean up after, cover wet cotton and be placed in 30
1~2h is placed at~40 DEG C, then removes wet cotton, is subsequently placed in water and boils 2~4h, is filtered, and is taken the lower object of filter, is obtained filtered fluid,
Filtered fluid is placed under 45~60 DEG C and 0.06~0.08Mpa and is concentrated under reduced pressure, is dry, wherein wet cotton is before covering the leaf of bamboo
It is immersed in rice washing water after 5~8min, taking-up is wrung out to not dripping.
4. the method that isoesdragol is extracted in rectifying as claimed in claim 3, which is characterized in that parch object is being added in cellulase
It is activated before, the concrete operations of activation are as follows: cellulase is placed at -20 DEG C and freezes 10-16h, then takes out addition
MgCl2Solid powder, then it is placed in 5~8min of water-bath at 45~50 DEG C, wherein cellulase and MgCl2The weight ratio of solid powder
For 7:2.
5. the method that isoesdragol is extracted in rectifying as described in claim 1, which is characterized in that extractant includes lemon in S4
One or more of acid, sodium soap, Epoxysuccinic acid potassium, sodium benzoate.
6. the method that isoesdragol is extracted in rectifying as described in claim 1, which is characterized in that extract liquor removal process in S4
Are as follows: it is added into extract liquor and accounts for the discoloration silica gel of extract liquor parts by weight 10~20%, then be placed at 30~40 DEG C with 100~
The speed of 200r/min stirs 30~60min, then filters, and takes the lower object of filter, obtains isoesdragol.
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| CN113501751A (en) * | 2021-08-18 | 2021-10-15 | 南宁市和昇香料香精有限公司 | Method for preparing high-purity cinnamaldehyde by efficiently rectifying and purifying cinnamon oil |
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| CN105713732A (en) * | 2016-04-29 | 2016-06-29 | 山东农业大学 | Extraction method of star anise oil |
| CN107098797A (en) * | 2017-06-23 | 2017-08-29 | 广西万山香料有限责任公司 | A kind of extracting method of chavicol methyl ether |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105713732A (en) * | 2016-04-29 | 2016-06-29 | 山东农业大学 | Extraction method of star anise oil |
| CN107098797A (en) * | 2017-06-23 | 2017-08-29 | 广西万山香料有限责任公司 | A kind of extracting method of chavicol methyl ether |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113501751A (en) * | 2021-08-18 | 2021-10-15 | 南宁市和昇香料香精有限公司 | Method for preparing high-purity cinnamaldehyde by efficiently rectifying and purifying cinnamon oil |
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