CN106833902A - A kind of Japan pepper essential oil and its extracting method - Google Patents
A kind of Japan pepper essential oil and its extracting method Download PDFInfo
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- CN106833902A CN106833902A CN201710177850.2A CN201710177850A CN106833902A CN 106833902 A CN106833902 A CN 106833902A CN 201710177850 A CN201710177850 A CN 201710177850A CN 106833902 A CN106833902 A CN 106833902A
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- essential oil
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0292—Treatment of the solvent
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
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- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
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- Medicines Containing Plant Substances (AREA)
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Abstract
The invention belongs to food ingredient deep process technology field, a kind of Japan pepper essential oil and its extracting method are disclosed.Extracting method of the present invention is extracted using subcritical methyl ether butane mixed solvent, is comprised the following steps：To be inserted in extractor by the Pricklyash peel of pretreatment, pressure inside the tank is down to 1.0 × 104Below Pa, subcritical methyl ether butane mixed solvent is injected to zanthoxylum powder is submerged, and adjustment extraction pressure inside the tank is 0.4~0.8MPa, extracts 40~60min, isolated leaching liquor, the degreasing Chinese prickly ash dregs of rice and the Japan pepper essential oil rich in numb monosodium glutamate are obtained after solvent recovery is carried out to it.Degreasing Chinese prickly ash dregs of rice oil content≤1.0%, residual solvent≤50mg/kg；Volatile oil extracting rate ＞ 98%, numb monosodium glutamate recovery rate ＞ 95%, total impurities ＜ 2.0%, while numb monosodium glutamate recovery rate in fully improving Chinese prickly ash, effectively controls impurity content in essential oil, at utmost retain the peculiar fragrance and numb taste of Chinese prickly ash, more local flavor.
Description
Technical field
The invention belongs to food ingredient deep process technology field, more particularly to a kind of Japan pepper essential oil and its extracting method.
Background technology
Chinese prickly ash is Rutaceae, Zanthoxylum machaka or dungarunga, and its pericarp can be as flavoring and extractable fragrant
Oil, can be used as medicine again, seed edible.Chinese prickly ash can remove the stink smell of various meats, and can provide the distinctive fragrance of Chinese prickly ash and numb taste, be
Food processing and the preferable blending raw material of fragrance industry.Chinese prickly ash also has anti-inflammation, analgesia, suppresses platelet aggregation, drop blood
The multiple pharmacological effects such as fat, ascarifuge, have very big developing and utilizingpotentiality and prospect in field of medicaments.
For a long time, the major product form of Chinese prickly ash is pepper grain or zanthoxylum powder, is restricted using scope, transports and protects
Hide relatively costly.Used as a kind of Chinese prickly ash deep processed product, Japan pepper essential oil application in the food industry is more and more.Japan pepper essential oil
In volatile oil and numb monosodium glutamate be the main component for producing Chinese prickly ash peculiar taste, volatile oil is by olefines, alcohols, ketone, aldehydes
Deng multiple compounds composition, with preferably fat-soluble, and the main component of numb monosodium glutamate is amides compound in Chinese prickly ash, is dissolved in
Hot ethanol, benzene, are slightly soluble in water, insoluble in petroleum ether, are primarily present in Chinese prickly ash pericarp, also have small part to be present in the flower of Chinese prickly ash
In leaf.
The extracting mode of the characteristic flavor on basis composition such as volatile oil and numb monosodium glutamate mainly has immersion method, organic solvent in current Chinese prickly ash
Extraction, supercritical extraction.Wherein can not be fully dissolved out for spicy component by immersion method, and Residual oil is more in material, cause to waste；
There is problem of solvent residual in conventional organic solvent extraction, influence the local flavor and quality of product；Supercritical extraction extracting pressure
Higher, the design and manufacture cost and operating cost of equipment are higher, and to introduce the entrainers such as ethanol and could effectively extract flower
The compositions such as the numb monosodium glutamate in green pepper, need to carry out desolventizing treatment to extraction product.
Additionally, the extraction that steam distillation and Subcritical Water Extraction method are used for Chinese prickly ash composition also has been reported that, both sides
The operation temperature of method is big compared with high, energy consumption, can cause characteristic chicken flavor and spicy component different degrees of loss or destruction in Chinese prickly ash, and
And it is relatively low to the extraction efficiency of liposoluble constituent in raw material, resource utilization is relatively low.
The content of the invention
In order to overcome the shortcomings and deficiencies of the prior art described above, primary and foremost purpose of the invention is to provide a kind of Japan pepper essential oil
Extracting method.The inventive method can simultaneously extract the validity feature composition, maximum journey such as volatile oil and numb monosodium glutamate in Chinese prickly ash
Retain the peculiar fragrance and numb taste of Chinese prickly ash on degree, be prevented effectively from the wasting of resources.
Another object of the present invention is to provide the Japan pepper essential oil that the above method is obtained.
The purpose of the present invention is realized by following proposal：
A kind of extracting method of Japan pepper essential oil, is extracted using subcritical methyl ether-butane mixed solvent, is comprised the following steps：
To be inserted in extractor by the Pricklyash peel of pretreatment, pressure inside the tank is down to 1.0 × 104Below Pa, injects subcritical first
To zanthoxylum powder is submerged, adjustment extraction pressure inside the tank is 0.4~0.8MPa to ether-butane mixed solvent, extracts 40~60min, is separated
Leaching liquor is obtained, the degreasing Chinese prickly ash dregs of rice and the Japan pepper essential oil rich in numb monosodium glutamate are obtained after solvent recovery is carried out to it.
The volume ratio of the mixed solvent Subcritical methyl ether and butane is preferably 1:1~1:19.Due to subcritical butane
There is extraction efficiency higher to the volatile oil in Chinese prickly ash, and the extraction efficiency of the pepper numb-taste component stronger to polarity is relatively low, institute
Using the present invention, the appropriate subcritical methyl ether of addition, as entrainer, takes full advantage of Asia and faces in conventional subcritical abstraction agent butane
The cooperative effect of boundary's methyl ether and butane makes numb monosodium glutamate dissolution, and two class flavor components in Chinese prickly ash are kept with extraction effect higher simultaneously
Rate, and controlled in reduced levels the stickiness resinous impurities in products obtained therefrom by suitable usage ratio, it is to avoid product
Sensory properties and application be affected.
The pretreatment includes the operations such as removal of impurities, drying, drying, remove seed, crushing.
The temperature of the extraction is preferably 20~40 DEG C.
The extraction is preferably carried out 2~5 times.
Merge after solvent recovery is carried out to extracted many times liquid, obtain the Japan pepper essential oil rich in numb monosodium glutamate.
The isolated leaching liquor is that leaching liquor is transferred into solvent recovery tank from extractor using pressure differential.
The solvent recovery, the solvent gasified in extractor and solvent recovery tank is pressurizeed by air compressor preferably is made
Solvent tank is flowed into after its liquefaction to realize.
Pressure in solvent recovery process in extractor and solvent recovery tank is gradually reduced, when pressure inside the tank close to atmospheric pressure
When, vavuum pump and air compressor tandem working are needed, pressure inside the tank is down to 1.0 × 10 under the conditions of 25~40 DEG C4Below Pa,
It is the degreasing Chinese prickly ash dregs of rice and Japan pepper essential oil that can obtain precipitation to maintain 20~40min.
The solvent that the solvent recovery is obtained can be recycled.
Extracting method running cost of the present invention is low, be easily achieved large-scale production, significantly improves numb monosodium glutamate recovery rate.
Oil content≤1.0% of the degreasing Chinese prickly ash dregs of rice that the inventive method is obtained, residual solvent≤50mg/kg；Japan pepper essential oil
In be more than 95% more than the recovery rate of 98%, numb monosodium glutamate, dissolved in gained essential oil rich in numb monosodium glutamate, the wherein recovery rate of volatile oil
Sticky solid material and the total amount of the impurity such as polysaccharide be less than 2.0%, while numb monosodium glutamate recovery rate in fully improving Chinese prickly ash,
The content of smart well cuts is effectively controlled, the peculiar fragrance and numb taste of Chinese prickly ash, more local flavor are retained to the full extent.
The present invention has the following advantages and beneficial effect relative to prior art：
(1) local flavor such as volatile oil and numb monosodium glutamate during the inventive method efficiently can extract Chinese prickly ash under relatively low pressure condition
Composition, simple to operate and with good stability, the design and manufacture cost and operating cost of equipment are low, easily realize scale
Production；
(2) the inventive method can be prevented effectively from the broken of product special flavour composition close to the extraction temperature and oxygen-free environment of room temperature
It is bad；
(3) the inventive method solvent for use is gas, i.e. liquefiable after appropriate pressurization, it is easy to return under normal temperature and pressure conditionses
Receive and in the absence of problem of solvent residual；
(4) impurity content is few in present invention gained Japan pepper essential oil.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, but embodiments of the present invention not limited to this.
The reagent used in the following example can be obtained from commercial channel.
Embodiment 1
Ten kilograms of pericarpium zanthoxyli schinifolii pericarps are crushed to below 40 mesh, are placed in batch extractor, dropped pressure inside the tank using vavuum pump
To 1.0 × 104Below Pa；To mixed solvent is injected in batch extractor, (subcritical methyl ether and subcritical butane volume ratio are 1:4) extremely
Material is flooded, extraction pressure is 0.4MPa, and the time is 40min；Mixed solvent is fully transferred to solvent recovery by extraction after terminating
Tank, using air compressor by solvent recovery to solvent tank, when solvent recovery pressure inside the tank is suitable with atmospheric pressure, starts vacuum
Pump and air compressor tandem working, make the pressure in solvent recovery tank be down to 1.0 × 104Below Pa simultaneously keeps 30min, molten
With recirculated water persistently to tank body heat supply during agent recovery, it is 40 DEG C to keep pot temperature.Repeat extracting operation 5 times, merge
Each extract is to obtain the common 1.65kg of Japan pepper essential oil rich in numb monosodium glutamate, and acid value is 5.16mgKOH/g, the extraction of volatile oil
Rate is 98.3%, and the recovery rate of numb monosodium glutamate is 96.0%, the impurity such as sticky solid material and polysaccharide being dissolved in Japan pepper essential oil
Total amount≤1.8% of composition.The degreasing Chinese prickly ash dregs of rice oil content obtained through solvent recovery is 0.53%, dissolvent residual≤20mg/kg.
Embodiment 2
40 mesh sieves after pericarpium zanthoxyli bungeani pericarp is crushed, take ten kilograms and are placed in batch extractor, are dropped pressure inside the tank using vavuum pump
To 1.0 × 104Below Pa；To mixed solvent is injected in batch extractor, (subcritical methyl ether and subcritical butane volume ratio are 1:9) extremely
Material is flooded, extraction pressure is 0.6MPa, and the time is 50min；Mixed solvent is fully transferred to solvent recovery by extraction after terminating
Tank, using air compressor by solvent recovery to solvent tank, when solvent recovery pressure inside the tank is suitable with atmospheric pressure, starts vacuum
Pump and air compressor tandem working, make the pressure in solvent recovery tank be down to 1.0 × 104Below Pa simultaneously keeps 30min, molten
With recirculated water persistently to tank body heat supply during agent recovery, it is 35 DEG C to keep pot temperature.Repeat extracting operation 3 times, merge
Each extract is to obtain the common 1.36kg of Japan pepper essential oil rich in numb monosodium glutamate, and acid value is 3.61mgKOH/g, the extraction of volatile oil
Rate is 98.8%, and the recovery rate of numb monosodium glutamate is 95.5%, the impurity such as sticky solid material and polysaccharide being dissolved in Japan pepper essential oil
Total amount≤2.0% of composition.The degreasing Chinese prickly ash dregs of rice oil content obtained through solvent recovery is 0.61%, dissolvent residual≤25mg/kg.
Comparative example
Five kilograms of pericarpium zanthoxyli schinifolii pericarps are crushed to below 40 mesh, are placed in batch extractor, dropped pressure inside the tank using vavuum pump
To 1.0 × 104Below Pa；To liquid butane is injected in batch extractor to material is flooded, extraction pressure is 0.7MPa, and the time is
40min；Solvent is fully transferred to solvent recovery tank by extraction after terminating, using air compressor by solvent recovery to solvent tank,
When solvent recovery pressure inside the tank is suitable with atmospheric pressure, start vavuum pump and air compressor tandem working, make solvent recovery tank
Interior pressure is down to 1.0 × 104Below Pa simultaneously keeps 30min, and persistently tank body is supplied with recirculated water during solvent recovery
Heat, it is 30 DEG C to keep pot temperature.Repeat extracting operation 4 times, it is to obtain the Chinese prickly ash rich in numb monosodium glutamate to merge each extract
The common 0.84kg of essential oil, acid value is 4.91mgKOH/g, and the recovery rate of volatile oil is 98.5%, and the recovery rate of numb monosodium glutamate is 56.7%,
Total amount≤1.0% of the impurity components such as sticky solid material and the polysaccharide being dissolved in Japan pepper essential oil.Obtained through solvent recovery
Degreasing Chinese prickly ash dregs of rice oil content is 0.59%, dissolvent residual≤25mg/kg.
Above-described embodiment is the present invention preferably implementation method, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from Spirit Essence of the invention and the change, modification, replacement made under principle, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. a kind of extracting method of Japan pepper essential oil, it is characterised in that extracted using subcritical methyl ether-butane mixed solvent, including with
Lower step：To be inserted in extractor by the Pricklyash peel of pretreatment, pressure inside the tank is down to 1.0 × 104Below Pa, injection is sub-
Critical methyl ether-butane mixed solvent extracts pressure inside the tank for 0.4~0.8MPa to zanthoxylum powder, adjustment is submerged, and extraction 40~
60min, isolated leaching liquor obtains the degreasing Chinese prickly ash dregs of rice and the Japan pepper essential oil rich in numb monosodium glutamate after solvent recovery is carried out to it.
2. the extracting method of Japan pepper essential oil according to claim 1, it is characterised in that：The mixed solvent Subcritical first
The volume ratio of ether and butane is 1:1~1:19.
3. the extracting method of Japan pepper essential oil according to claim 1, it is characterised in that：The pretreatment includes removal of impurities, dries in the air
Solarization, drying, remove seed, pulverizing process.
4. the extracting method of Japan pepper essential oil according to claim 1, it is characterised in that：The temperature of the extraction is 20~40
℃。
5. the extracting method of Japan pepper essential oil according to claim 1, it is characterised in that：The extraction is carried out 2~5 times.
6. the extracting method of Japan pepper essential oil according to claim 1, it is characterised in that：The isolated leaching liquor is profit
Leaching liquor is transferred to solvent recovery tank from extractor with pressure differential.
7. the extracting method of Japan pepper essential oil according to claim 1, it is characterised in that：The solvent recovery passes through air pressure
Contracting machine makes it that solvent tank realization is flowed into after liquefying the solvent pressurization gasified in extractor and solvent recovery tank.
8. the extracting method of Japan pepper essential oil according to claim 7, it is characterised in that：Extracted in the solvent recovery process
Pressure in tank and solvent recovery tank is gradually reduced, and when pressure inside the tank is close to atmospheric pressure, vavuum pump is connected with air compressor
Work, 1.0 × 10 are down under the conditions of 25~40 DEG C by pressure inside the tank4Below Pa, it is to obtain taking off for precipitation to maintain 20~40min
The fat Chinese prickly ash dregs of rice and Japan pepper essential oil.
9. the extracting method of Japan pepper essential oil according to claim 1, it is characterised in that：The solvent that the solvent recovery is obtained
Recycle.
10. a kind of Japan pepper essential oil is it is characterized in that the extracting method according to any one of claim 1~9 is obtained.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710177850.2A CN106833902A (en) | 2017-03-23 | 2017-03-23 | A kind of Japan pepper essential oil and its extracting method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710177850.2A CN106833902A (en) | 2017-03-23 | 2017-03-23 | A kind of Japan pepper essential oil and its extracting method |
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| CN201710177850.2A Pending CN106833902A (en) | 2017-03-23 | 2017-03-23 | A kind of Japan pepper essential oil and its extracting method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107803049A (en) * | 2017-11-22 | 2018-03-16 | 中国科学院兰州化学物理研究所 | The method for preparing papper oil and pepper oleoresin using ultrasonic subcritical fluid extraction technology |
| CN111205923A (en) * | 2020-01-13 | 2020-05-29 | 四川嘉威德农业科技有限公司 | Processing technology of pure zanthoxylum oil rich in linolenic acid |
| CN111303999A (en) * | 2020-02-27 | 2020-06-19 | 营山椒宝宝花椒有限责任公司 | Extraction method of green pepper volatile oil |
| CN111621365A (en) * | 2020-06-04 | 2020-09-04 | 成都泰罗科技有限公司 | Zanthoxylum essential oil and extraction process thereof |
| CN112094697A (en) * | 2020-09-04 | 2020-12-18 | 北京中科环通工程科技有限公司 | Extraction method of citrus essential oil |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107803049A (en) * | 2017-11-22 | 2018-03-16 | 中国科学院兰州化学物理研究所 | The method for preparing papper oil and pepper oleoresin using ultrasonic subcritical fluid extraction technology |
| CN111205923A (en) * | 2020-01-13 | 2020-05-29 | 四川嘉威德农业科技有限公司 | Processing technology of pure zanthoxylum oil rich in linolenic acid |
| CN111303999A (en) * | 2020-02-27 | 2020-06-19 | 营山椒宝宝花椒有限责任公司 | Extraction method of green pepper volatile oil |
| CN111303999B (en) * | 2020-02-27 | 2020-10-27 | 营山椒宝宝花椒有限责任公司 | Extraction method of green pepper volatile oil |
| CN111621365A (en) * | 2020-06-04 | 2020-09-04 | 成都泰罗科技有限公司 | Zanthoxylum essential oil and extraction process thereof |
| CN112094697A (en) * | 2020-09-04 | 2020-12-18 | 北京中科环通工程科技有限公司 | Extraction method of citrus essential oil |
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Application publication date: 20170613 |