CN106433985B - A kind of ginger essential oil and preparation method thereof - Google Patents
A kind of ginger essential oil and preparation method thereof Download PDFInfo
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- CN106433985B CN106433985B CN201610891592.XA CN201610891592A CN106433985B CN 106433985 B CN106433985 B CN 106433985B CN 201610891592 A CN201610891592 A CN 201610891592A CN 106433985 B CN106433985 B CN 106433985B
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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
- C11B9/025—Recovery by solvent extraction
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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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Abstract
The present invention provides a kind of preparation method of ginger essential oil, includes the following steps：The preparation of ginger powder：Ginger is cleaned, remove seed dry, pulverize, and obtain ginger powder；The preparation of oil of ginger crude product：The ginger powder that step S1 is obtained is packed into extraction kettle, supercritical CO2Entered in extraction kettle by extraction kettle bottom end, extracted through first time extraction and second, collect and merge the CO containing extract2, detached through first time parsing separation and second of parsing, collect separating liquid I and separating liquid II, merge, obtain oil of ginger crude product；The preparation of ginger essential oil：The oil of ginger crude product that step S2 is obtained under water bath condition is stirred, water-oil separating is carried out, oil phase is filtered by vacuum, collection obtains ginger essential oil.The invention belongs to technical field of food additives, method provided by the invention has many advantages, such as that high income, preparation time are short, and ginger essential oil obtained is high-quality, long shelf-life.
Description
Technical field
The invention belongs to technical field of food additives more particularly to a kind of ginger essential oil and preparation method thereof.
Background technology
Ginger is the fresh rhizome of Zingiber herbaceos perennial ginger (Zingiber officinale Roscoe), is one
The time-honored pungent and fragrant flavorings of kind belong to the plant of medicine-food two-purpose, have diverging, preventing or arresting vomiting, cough-relieving and other effects.Ginger essential oil is
Refer to the volatile oil extracted from ginger rhizome, be a kind of brown oil liquid, including sesquialter mushroom alkenes carbon hydrate
The main components such as object, oxidation sesquialter mushroom ene compound and single mushroom alkenes carbohydrate, have strong aromatic odor.It is existing to grind
Study carefully and show that ginger essential oil has anticoagulation, antibacterial, preventing thrombosis, prevention atherosclerosis and other effects, can be used as food, daily use chemicals are used
The additive of product etc..
Existing ginger essential oil preparation method is mainly steam distillation and solvent extraction method.Used in steam distillation
Solvent is water, environmental-friendly, easy to operate, but the distillation time of this method is long, and extraction efficiency is relatively low, and treating capacity is relatively low, such as
Chinese patent application CN 102443487A disclose a kind of preparation method of ginger essential oil, after being heated by microwave irradiation
Distillation extraction, after standing water-oil separating obtain ginger essential oil.Solvent extraction method makes ginger essential oil, can possess ginger simultaneously
Fragrance and peculiar taste, but there are dissolvent residual (ethyl alcohol, ether etc.) flavor can be influenced, and in product impurity it is more (wax,
Resinous matter etc.), aftertreatment technology is complicated.
Supercritical CO2Extraction is the environmentally protective extracting process of rising in recent years, has extraction efficiency height, production week
Phase is short, it is simple for process, there is no the advantages that dissolvent residual, be widely used in the fields such as food processing, pharmaceuticals and health food.
Existing supercritical extraction generally requires higher pressure to improve extraction efficiency, therefore, to the more demanding of equipment,
And the ingredient that part is unfavorable for flavor is also extracted while flavor components are extracted.
102965190 A of Chinese patent application CN disclose a kind of ginger method of extraction of essential oil, ginger grain are placed in overcritical
CO2In extraction equipment, supercritical CO is carried out under the conditions of 30MPa, 60 DEG C2Extraction, extraction time are controlled in 120min, then will
Obtained first product ginger essential oil is sent into molecular distillation tank and carries out vacuum distillation purifying condensation, finished product ginger essential oil, although in ginger oil
Major terpene class carbohydrate content it is high, but yield is relatively low, about 3% or so.
Invention content
To solve problems of the prior art, inventor is by a large number of experiments to the supercritical extract condition of ginger powder
It is studied, unexpected discovery：By the extraction and parsing of secondary different pressures, flavor components extract yield is being improved
While reduce the extraction for being unfavorable for flavor components, obtained oil of ginger crude yield is high, conducive to subsequent purifying, through simple
After purification, you can obtain ginger essential oil, the acid value and peroxide value of ginger essential oil are low, state transparent and homogeneous, good fluidity, flavor
It is good.Based on above-mentioned discovery, thereby completing the present invention.
The purpose of the present invention will be further described in detail below reflect and description.
The present invention provides a kind of preparation method of ginger essential oil, includes the following steps：
The preparation of S1 ginger powders：Ginger is cleaned, remove seed, drying to water content is 5~14%, crushes, obtains ginger powder；
The preparation of S2 oil of ginger crude products：The ginger powder that step S1 is obtained is packed into extraction kettle, supercritical CO2By extraction kettle
Bottom end enters in extraction kettle, is extracted through first time extraction and second, collects and merge the CO containing extract2, solved through first time
Analysis separation and second of parsing separation, collect separating liquid I and separating liquid II, merge, obtain oil of ginger crude product；
The preparation of S3 ginger essential oils：The oil of ginger crude product that step S2 is obtained under water bath condition is stirred, carries out grease point
From, oil phase is filtered by vacuum, vacuum degree be -0.07Mpa~-0.1Mpa, collection obtain ginger essential oil.
Preferably, the condition of the first time extraction is：10~16MPa, temperature are 40~60 DEG C, CO2Flow velocity for 200~
500L/h, time are 30~60min.It is highly preferred that pressure is 14MPa, temperature is 52 DEG C, CO2Flow velocity is 400L/h, the time is
45min。
Preferably, the condition of second of extraction is：20~28MPa, temperature are 50~60 DEG C, CO2Flow velocity for 300~
500L/h, time are 20~60min.It is highly preferred that pressure is 24MPa, temperature is 55 DEG C, CO2Flow velocity is 400L/h, the time is
30min.Supercritical CO2To polarity, the extraction efficiency of smaller substance is often higher than the larger substance of polarity to fluid, and solute is super
Critical CO2Solubility in fluid is easily influenced by pressure and temperature, and different solutes are in supercritical CO2Solubility in fluid
It may also influence each other.The present invention passes through the CO containing extract that is obtained to different extraction conditions2Analytical analysis is carried out, is expected not
It is found to ground：Supercritical CO2Fluid is 40~60 DEG C, CO in 10~16MPa, temperature2Under conditions of flow velocity is 200~500L/h
30~60min is first extracted, then again in 20~28MPa, 50~60 DEG C, CO2Flow velocity extracts 20 under conditions of being 300~500L/h
~60min, by the cooperation of different extraction conditions twice, the high income of oil of ginger crude product, pressure is not very high, extraction time
Short, the whole flavor after refined is good.
Preferably, the condition of the first time parsing separation is：40~55 DEG C of 5~10MPa of pressure, temperature.It is highly preferred that
Pressure is 8MPa, temperature is 50 DEG C.
Preferably, the condition of second of parsing separation is：40~55 DEG C of 5~7MPa of pressure, temperature.It is highly preferred that
Pressure is 6MPa, temperature is 48 DEG C.
By elder generation under the conditions of 5~10MPa, 40~55 DEG C of temperature for the first time parsing separation, then again pressure 5~
Second parsing separation, can realize the abundant parsing of flavor components under the conditions of 7MPa, 40~55 DEG C of temperature, at the same reduce it is unfavorable
In the parsing of flavor components (low grade aldehyde etc.).
Preferably, in the S1, drying to water content is 6~12%, is crushed to 30~60 mesh.
Preferably, in the S3, the temperature of water-bath is 45~60 DEG C, and the time is 10~20min；The rotating speed of stirring is 200
~500rpm, time are 5~10min.
Preferably, the extraction kettle includes the extraction column equipped with filler.
It is highly preferred that the filler is the western tower ring filler of stainless steel.
Correspondingly, the present invention also provides a kind of ginger essential oils, are made by the preparation method of above-mentioned ginger essential oil.Ginger extract
The good product quality of oil, acid value and peroxide value are low, and whole flavor is good, long shelf-life.
Compared with prior art, the beneficial effects of the invention are as follows：The present invention by the extraction and parsing of secondary different pressures,
The use of high pressure is avoided, extraction time is short, improves production efficiency, and obtained oil of ginger crude yield is high, conducive to follow-up
Purifying；Oil of ginger purifying crude method provided by the invention is simple, and the active ingredient loss in purification process is few, high income,
The good product quality of obtained ginger essential oil, acid value and peroxide value are low, and whole flavor is good, long shelf-life.
Specific embodiment
Below by specific embodiment, the present invention is described in further detail.
In the embodiment of the present invention, the detection of acid value is with reference to GB/T 5530-2005 (animal and plant fats：Acid value and acidity are surveyed
It is fixed), the detection of peroxide value is with reference to GB/T 5538-2005 (animal and plant fats：Peroxide value).
The preparation of one ginger powder of embodiment
Ginger is cleaned, remove seed, drying to water content is 7.5%, is crushed to 30~60 mesh, obtains ginger powder.
The preparation of two oil of ginger crude product of embodiment
Ginger powder 12.0kg made from Example one is packed into the extraction kettle (extraction including being equipped with the western tower ring filler of stainless steel
Take column) in, supercritical CO2Entered in extraction kettle by extraction kettle bottom end, extracted through first time extraction and second, collect and merge
CO containing extract2, detached through first time parsing separation and second of parsing, collect separating liquid I and separating liquid II, merge, obtain
To oil of ginger crude product；The pressure of extraction is 14MPa for the first time, temperature is 52 DEG C, CO2Flow velocity is 400L/h, time 45min；
The pressure of second of extraction is 24MPa, temperature is 55 DEG C, CO2Flow velocity is 400L/h, time 30min；Parsing separation for the first time
Pressure be 8MPa, temperature is 50 DEG C；The pressure of second of parsing separation is 6MPa, temperature is 48 DEG C.
In terms of ginger powder, the mass yield of oil of ginger crude product is 5.53%.
The preparation of three oil of ginger crude product of embodiment
Ginger powder 12.0kg made from Example one is packed into the extraction kettle (extraction including being equipped with the western tower ring filler of stainless steel
Take column) in, supercritical CO2Entered in extraction kettle by extraction kettle bottom end, extracted through first time extraction and second, collect and merge
CO containing extract2, detached through first time parsing separation and second of parsing, collect separating liquid I and separating liquid II, merge, obtain
To oil of ginger crude product；The pressure of extraction is 12MPa for the first time, temperature is 50 DEG C, CO2Flow velocity is 400L/h, time 45min；
The pressure of second of extraction is 26MPa, temperature is 55 DEG C, CO2Flow velocity is 400L/h, time 30min；Parsing separation for the first time
Pressure be 8MPa, temperature is 50 DEG C；The pressure of second of parsing separation is 6MPa, temperature is 48 DEG C.
In terms of ginger powder, the mass yield of oil of ginger crude product is 5.29%.
The preparation of one oil of ginger crude product of comparative example
Ginger powder 6.0kg made from Example one is packed into the extraction kettle (extraction including being equipped with the western tower ring filler of stainless steel
Column) in, supercritical CO2Entered in extraction kettle by extraction kettle bottom end, extracted through first time extraction and second, collected and merge and contain
The CO of extract2, detached through first time parsing separation and second of parsing, collect separating liquid I and separating liquid II, merge, obtain
Oil of ginger crude product；The pressure of extraction is 14MPa for the first time, temperature is 52 DEG C, CO2Flow velocity is 400L/h, time 45min；The
The pressure of reextraction is 18MPa, temperature is 55 DEG C, CO2Flow velocity is 400L/h, time 30min；Parsing separation for the first time
Pressure is 8MPa, temperature is 50 DEG C；The pressure of second of parsing separation is 6MPa, temperature is 48 DEG C.
Comparative example one and embodiment two difference lies in：The pressure of second of extraction becomes 18MPa from 24MPa.
In terms of ginger powder, the mass yield of oil of ginger crude product is 4.38%.
The preparation of two oil of ginger crude product of comparative example
Ginger powder 12.0kg made from Example one is packed into the extraction kettle (extraction including being equipped with the western tower ring filler of stainless steel
Take column) in, supercritical CO2Entered in extraction kettle by extraction kettle bottom end, extracted through first time extraction and second, collect and merge
CO containing extract2, detached through first time parsing separation and second of parsing, collect separating liquid I and separating liquid II, merge, obtain
To oil of ginger crude product；The pressure of extraction is 14MPa for the first time, temperature is 52 DEG C, CO2Flow velocity is 400L/h, time 45min；
The pressure of second of extraction is 30MPa, temperature is 55 DEG C, CO2Flow velocity is 400L/h, time 30min；Parsing separation for the first time
Pressure be 8MPa, temperature is 50 DEG C；The pressure of second of parsing separation is 6MPa, temperature is 48 DEG C.
Comparative example two and embodiment two difference lies in：The pressure of second of extraction becomes 30MPa from 24MPa.
In terms of ginger powder, the mass yield of oil of ginger crude product is 5.17%.Increase the pressure of second of extraction, not into one
Step improves the yield of oil of ginger crude product, with difference desired in advance.
The preparation of example IV ginger essential oil
Oil of ginger crude product 0.5kg made from Example two, the water-bath 15min under the conditions of 50 DEG C, stirring, 400rpm, when
Between be 6min.After standing, water-oil separating is carried out, oil phase is filtered by vacuum, vacuum degree is -0.08Mpa, and collection obtains ginger
Essential oil 0.459kg.Water-bath is the speed in order to accelerate grease layering, but temperature cannot be too high.
Ginger essential oil stable homogeneous, it is limpid transparent, it is not stratified after centrifugation.Constituent analysis, α-zingiberene are carried out to ginger essential oil
Content be the content of 28.5%, β-sesquiphellandrene be 9.1%, the content of farnesene is 6.7%, and the content of 6-gingerol is
The content of 5.0%, 6- zingiberol is 6.2%, and the content of water is 3.7%.
The preparation of five ginger essential oil of embodiment
Oil of ginger crude product 0.5kg made from Example three, the water-bath 15min under the conditions of 50 DEG C, stirring, 400rpm, when
Between be 6min.After standing, water-oil separating is carried out, oil phase is filtered by vacuum, vacuum degree is -0.08Mpa, and collection obtains ginger
Essential oil 0.453kg.
Ginger essential oil stable homogeneous, it is limpid transparent, it is not stratified after centrifugation.Constituent analysis, α-zingiberene are carried out to ginger essential oil
Content be 26.3%, β-sesquiphellandrene content 8.8%, the content of farnesene is 7.2%, and the content of 6-gingerol is
The content of 5.4%, 6- zingiberol is 4.9%, the content 3.5% of water.
The preparation of three ginger essential oil of comparative example
Oil of ginger crude product 0.5kg made from comparative example one is taken, the water-bath 15min under the conditions of 50 DEG C, stirring, 400rpm, when
Between be 6min.After standing, water-oil separating is carried out, oil phase is filtered by vacuum, vacuum degree is -0.08Mpa, and collection obtains ginger
Essential oil 0.461kg.
Constituent analysis is carried out to ginger essential oil, the content of α-zingiberene is the content 7.9% of 28.0%, β-sesquiphellandrene,
The content of farnesene is 7.1%, and the content of 6-gingerol is that the content of 3.5%, 6- zingiberols is 1.8%, the content 3.8% of water.
The preparation of four ginger essential oil of comparative example
Oil of ginger crude product 0.5kg made from comparative example two is taken, the water-bath 15min under the conditions of 50 DEG C, stirring, 400rpm, when
Between be 6min.After standing, water-oil separating is carried out, as a result：Oil phase is filtered by vacuum, vacuum degree is -0.08Mpa, is collected
To ginger essential oil 0.448kg.
Constituent analysis is carried out to ginger essential oil, the content of α-zingiberene is the content 8.5% of 29.3%, β-sesquiphellandrene,
The content of farnesene is 4.6%, and the content of 6-gingerol is that the content of 6.0%, 6- zingiberols is 6.9%, the content 4.1% of water.
The evaluation of test example ginger essential oil
Respectively to ginger essential oil and commercially available ginger made from example IV, embodiment five, comparative example three and comparative example four
Essential oil carries out the detection of acid value and peroxide value, at the same convene 10 flavour of food products evaluations professional person carry out fragrance level and
The scoring (full marks are 10 points) of preference degree, the results are shown in Table 1.
The evaluation of the different ginger essential oils of table 1
As known from Table 1, ginger essential oil made from preparation method of the present invention is high-quality, and acid value and peroxide value are low, total ceramide
Content is high, and fragrance flavor is good.The comprehensive performance of wherein example IV is best, and by specialty evaluation, personage is liked.
Study on the stability is carried out to ginger essential oil made from example IV and embodiment five, as a result：Long shelf-life is up to 18
Month.
In conclusion preparation method provided by the invention, when there is the high income of oil of ginger crude product and ginger essential oil, preparing
Between it is short the advantages that, ginger essential oil obtained is high-quality, and acid value and peroxide value are low, and fragrance flavor is good, long shelf-life.
Claims (4)
1. a kind of preparation method of ginger essential oil, it is characterised in that：Include the following steps：
The preparation of S1 ginger powders：It is 6 ~ 12% by ginger cleaning, drying to water content, is crushed to 30 ~ 60 mesh, obtains ginger powder；
The preparation of S2 oil of ginger crude products：The ginger powder that step S1 is obtained is packed into extraction kettle, supercritical CO2By extraction kettle bottom end
Into in extraction kettle, extracted through first time extraction and second, collect and merge the CO containing extract2, through first time parsing point
Oil of ginger crude product is obtained from second of parsing separation, collection separating liquid I and separating liquid II, merging；The first time extraction
Condition is：Pressure is 14MPa, temperature is 52 DEG C, CO2Flow velocity is 400L/h, time 45min；The item of second of extraction
Part is：Pressure is 24MPa, temperature is 55 DEG C, CO2Flow velocity is 400L/h, time 30min；The first time parsing separation
Condition is：Pressure 8MPa, temperature 50 C；The condition of the second parsing separation is：48 DEG C of pressure 6MPa, temperature；
The preparation of S3 ginger essential oils：The oil of ginger crude product that step S2 is obtained under water bath condition is stirred, carries out water-oil separating,
Oil phase is filtered by vacuum, vacuum degree is -0.07Mpa ~ -0.1Mpa, and collection obtains ginger essential oil；The temperature of water-bath for 45 ~
60 DEG C, the time is 10 ~ 20min；The rotating speed of stirring is 200 ~ 500rpm, and the time is 5 ~ 10min.
2. the preparation method of ginger essential oil according to claim 1, it is characterised in that：The extraction kettle is included equipped with filler
Extraction column.
3. the preparation method of ginger essential oil according to claim 2, it is characterised in that：The filler is the western tower ring of stainless steel
Filler.
4. a kind of ginger essential oil, it is characterised in that：As the preparation method of the ginger essential oil described in any one of claims 1 to 3
It is made.
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| CN107432927A (en) * | 2017-08-30 | 2017-12-05 | 姚璐 | A kind of essential oil and preparation method |
| CN109645394A (en) * | 2018-12-20 | 2019-04-19 | 株洲千金药业股份有限公司 | A kind of preparation method and its healthcare applications of water solubility ginger powder |
| CN109852477A (en) * | 2019-01-17 | 2019-06-07 | 广东聿津食品有限公司 | A kind of preparation method of cinnamon essential oil |
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