CN106433985A - Fresh ginger essential oil and preparation method thereof - Google Patents
Fresh ginger essential oil and preparation method thereof Download PDFInfo
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- CN106433985A CN106433985A CN201610891592.XA CN201610891592A CN106433985A CN 106433985 A CN106433985 A CN 106433985A CN 201610891592 A CN201610891592 A CN 201610891592A CN 106433985 A CN106433985 A CN 106433985A
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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 invention provides a preparation method of fresh ginger essential oil. The preparation method comprises the following steps: preparing fresh ginger powder, namely cleaning fresh ginger, removing seeds, drying, and smashing to obtain the fresh ginger powder; preparing a fresh ginger oil crude product, namely putting the fresh ginger powder obtained in the step S1 into an extraction kettle, introducing supercritical CO2 from the bottom end of the extraction kettle, carrying out primary extraction and secondary extraction, collecting and mixing CO2 containing extracts, carrying out primary analysis and separation and secondary analysis and separation, collecting a separating medium I and a separating medium II, and mixing to obtain the fresh ginger oil crude product; and preparing the fresh ginger essential oil, namely stirring the fresh ginger oil crude product obtained in the step S2 under a water bath condition, carrying out oil-water separation, carrying out vacuum filtration on an oil phase, and collecting to obtain the fresh ginger essential oil. The invention belongs to the technical field of food additives. The preparation method provided by the invention has the advantages of high yield, short preparation time and the like, and the obtained fresh ginger essential oil is good in quality and long in quality guarantee period.
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
Rhizoma Zingiberis Recenss are the new fresh quench stems of Zingiberaceae herbaceos perennial Rhizoma Zingiberis Recens (Zingiber officinale Roscoe), are one
Time-honored pungent and fragrant flavorings are planted, belongs to the plant of medicine-food two-purpose, with the effects such as diverging, preventing or arresting vomiting, cough-relieving.Ginger essential oil is
Referring to the volatile oil for obtaining is extracted from Rhizoma Zingiberis Recenss rhizome, is a kind of brown oil liquid, including sesquialter mushroom alkenes carbon hydrate
The main component such as thing, oxidation sesquialter mushroom ene compound and single mushroom alkenes carbohydrate, with strong aromatic odor.Existing grind
Study carefully and show the effects such as ginger essential oil has anticoagulation, antibacterial, preventing thrombosis, prevents and treats atherosclerosiss, can be used as food, daily use chemicals and use
The additive of product etc..
Existing ginger essential oil preparation method is mainly steam distillation and solvent extraction method.Used by steam distillation
Solvent is water, and environmental friendliness is simple to operate, but the distillation time of the method is long, and extraction efficiency is relatively low, and treating capacity is relatively low, such as
Chinese patent application CN 102443487A discloses a kind of preparation method of ginger essential oil, after being heated by microwave irradiation
Distillation extraction, oil-water separation after standing obtains ginger essential oil.Solvent extraction method makes ginger essential oil, can possess Rhizoma Zingiberis Recenss simultaneously
Fragrance and peculiar taste, but can there is dissolvent residual (ethanol, ether etc.), impact local flavor, and product in impurity more (wax,
Resinous matter etc.), aftertreatment technology complexity.
Supercritical CO2Extraction is the extracting process of the environmental protection of rising in recent years, with extraction efficiency height, production week
Phase is short, process is simple, without dissolvent residual the advantages of, 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, and therefore, the requirement to equipment is higher,
And also extracted, while extraction flavor components, the composition that part is unfavorable for local flavor.
102965190 A of Chinese patent application CN discloses a kind of Rhizoma Zingiberis Recens method of extraction of essential oil, and Rhizoma Zingiberis Recens grain is placed in supercritical
CO2In extraction equipment, in 30MPa, supercritical CO under the conditions of 60 DEG C, is carried out2Extraction, then extraction time control will in 120min
The first product Rhizoma Zingiberis Recens quintessence oil for obtaining is sent into molecular distillation tank and carries out vacuum distilling purification condensation, finished product Rhizoma Zingiberis Recens quintessence oil, although in oil of ginger
Major terpene class carbohydrate content height, but yield is relatively low, about 3% or so.
Content of the invention
For solving problems of the prior art, inventor passes through supercritical extraction condition of the lot of experiments to Rhizoma Zingiberis Recens powder
Studied, unforeseeable discovery：By extraction and the parsing of secondary different pressures, flavor components extract yield is being improve
While reduce the extraction for being unfavorable for flavor components, the oil of Rhizoma Zingiberis Recens crude yield that obtains height, beneficial to follow-up purification, through simple
After purification, you can obtain ginger essential oil, the acid value of ginger essential oil and peroxide value are low, state transparent and homogeneous, good fluidity, local flavor
Good.Based on above-mentioned discovery, so as to complete 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, comprises the steps：
The preparation of S1 Rhizoma Zingiberis Recens powder：Rhizoma Zingiberis Recenss are cleaned, remove seed, it is 5～14%, to crush to dry to water content, obtains Rhizoma Zingiberis Recens powder；
The preparation of S2 oil of Rhizoma Zingiberis Recens crude product：The Rhizoma Zingiberis Recens powder that step S1 is obtained loads in extraction kettle, supercritical CO2By extraction kettle
Bottom is entered in extraction kettle, is extracted through first time extraction and second, is collected and merge the CO containing extract2, solve through first time
Analysis is separated and second parsing is separated, and collects separating liquid I and separating liquid II, is merged, is obtained oil of Rhizoma Zingiberis Recens crude product；
The preparation of S3 ginger essential oil：The oil of Rhizoma Zingiberis Recens crude product that step S2 is obtained is stirred under water bath condition, is carried out profit and is divided
From, vacuum filtration is carried out to oil phase, vacuum is -0.07Mpa～-0.1Mpa, collects and obtains ginger essential oil.
Preferably, the condition of the first time extraction is：10～16MPa, temperature are 40～60 DEG C, CO2Flow velocity be 200～
500L/h, time are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30～60min are 30.It is highly preferred that pressure be 14MPa, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO, temperature be 52 DEG C, CO2Flow velocity is 400L/h, the time is
45min.
Preferably, the condition of second extraction is：20～28MPa, temperature are 50～60 DEG C, CO2Flow velocity be 300～
500L/h, time are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20～60min are 20.It is highly preferred that pressure be 24MPa, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO, temperature be 55 DEG C, CO2Flow velocity is 400L/h, the time is
30min.Supercritical CO2Fluid is often higher than the larger material of polarity to the extraction efficiency of the less material of polarity, and solute is super
Critical CO2Dissolubility in fluid is easily stressed the impact with temperature, and different solutes are in supercritical CO2Dissolubility in fluid
It is likely to influence each other.The present invention is by the CO containing extract that different extraction conditionss are obtained2Analytical analysis are carried out, is expected not
Find to ground：Supercritical CO2Fluid is 40～60 DEG C, CO2Under conditions of flow velocity is 200～500L/h
First 30～60min is extracted, then again in 20～28MPa, 50～60 DEG C, CO2Flow velocity is extraction 20 under conditions of 300～500L/h
～60min, by the cooperation of different extraction conditionss twice, the high income of oil of Rhizoma Zingiberis Recens crude product, pressure is not very high, extraction time
Short, the overall local flavor after refining is good.
Preferably, the detached condition of the first time parsing 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, described parse detached condition for the second time and be：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, parsing for the first time is separated, then again pressure 5～
Under the conditions of 7MPa, 40～55 DEG C of temperature, second parsing is separated, it is possible to achieve the abundant parsing of flavor components, while minimizing is unfavorable
Parsing in flavor components (low grade aldehyde etc.).
Preferably, in the S1, it is 6～12%, to be crushed to 30～60 mesh to dry to water content.
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, the time is 5～10min.
Preferably, the extraction kettle includes the extraction column equipped with filler.
It is highly preferred that described filler is the western tower ring filler of rustless steel.
Correspondingly, the present invention also provides a kind of ginger essential oil, is obtained 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 overall local flavor is good, long shelf-life.
Compared with prior art, the invention has the beneficial effects as follows：Extraction and parsing of the present invention by secondary different pressures,
The use of high pressure is avoided, extraction time is short, and production efficiency is improve, the oil of Rhizoma Zingiberis Recens crude yield height for obtaining, beneficial to follow-up
Purification；The oil of Rhizoma Zingiberis Recens purifying crude method that the present invention is provided is simple, and the active ingredient loss in purge process is few, high income,
The good product quality of the ginger essential oil for obtaining, acid value and peroxide value are low, and overall local 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 number is with reference to GB/T 5530-2005 (animal and plant fat：Acid number and acidity are surveyed
Fixed), the detection of peroxide value is with reference to GB/T 5538-2005 (animal and plant fat：Peroxide value).
The preparation of one Rhizoma Zingiberis Recens powder of embodiment
Rhizoma Zingiberis Recenss are cleaned, remove seed, it is 7.5%, to be crushed to 30～60 mesh, obtain Rhizoma Zingiberis Recens powder to dry to water content.
The preparation of two oil of Rhizoma Zingiberis Recens crude product of embodiment
Rhizoma Zingiberis Recens powder 12.0kg obtained in Example one, loading extraction kettle (includes the extraction equipped with the western tower ring filler of rustless steel
Take post) in, supercritical CO2Entered in extraction kettle by extraction kettle bottom, extract through first time extraction and second, collect and merge
CO containing extract2, separate through first time parsing and second parsing separated, separating liquid I and separating liquid II is collected, is merged, obtain
To oil of Rhizoma Zingiberis Recens crude product；The pressure for extracting for the first time is 14MPa, temperature is 52 DEG C, CO2Flow velocity is 400L/h, the time is 45min；
The pressure of second extraction is 24MPa, temperature is 55 DEG C, CO2Flow velocity is 400L/h, the time is 30min；Parsing is separated for the first time
Pressure be 8MPa, temperature be 50 DEG C；Parse for the second time detached pressure for 6MPa, temperature be 48 DEG C.
In terms of Rhizoma Zingiberis Recens powder, the mass yield of oil of Rhizoma Zingiberis Recens crude product is 5.53%.
The preparation of three oil of Rhizoma Zingiberis Recens crude product of embodiment
Rhizoma Zingiberis Recens powder 12.0kg obtained in Example one, loading extraction kettle (includes the extraction equipped with the western tower ring filler of rustless steel
Take post) in, supercritical CO2Entered in extraction kettle by extraction kettle bottom, extract through first time extraction and second, collect and merge
CO containing extract2, separate through first time parsing and second parsing separated, separating liquid I and separating liquid II is collected, is merged, obtain
To oil of Rhizoma Zingiberis Recens crude product；The pressure for extracting for the first time is 12MPa, temperature is 50 DEG C, CO2Flow velocity is 400L/h, the time is 45min；
The pressure of second extraction is 26MPa, temperature is 55 DEG C, CO2Flow velocity is 400L/h, the time is 30min；Parsing is separated for the first time
Pressure be 8MPa, temperature be 50 DEG C；Parse for the second time detached pressure for 6MPa, temperature be 48 DEG C.
In terms of Rhizoma Zingiberis Recens powder, the mass yield of oil of Rhizoma Zingiberis Recens crude product is 5.29%.
The preparation of one oil of Rhizoma Zingiberis Recens crude product of comparative example
Rhizoma Zingiberis Recens powder 6.0kg obtained in Example one, loading extraction kettle (includes the extraction equipped with the western tower ring filler of rustless steel
Post) in, supercritical CO2Entered in extraction kettle by extraction kettle bottom, extract through first time extraction and second, collect and merge and contain
The CO of extract2, separate through first time parsing and second parsing separated, separating liquid I and separating liquid II is collected, is merged, obtain
Oil of Rhizoma Zingiberis Recens crude product；The pressure for extracting for the first time is 14MPa, temperature is 52 DEG C, CO2Flow velocity is 400L/h, the time is 45min；The
The pressure of reextraction is 18MPa, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C, CO, temperature is 55 DEG C2Flow velocity is 400L/h, the time is 30min；Parse for the first time detached
Pressure is 8MPa, temperature is 50 DEG C；Parse for the second time detached pressure for 6MPa, temperature be 48 DEG C.
Comparative example one is with the difference of embodiment two：The pressure of second extraction is changed into 18MPa from 24MPa.
In terms of Rhizoma Zingiberis Recens powder, the mass yield of oil of Rhizoma Zingiberis Recens crude product is 4.38%.
The preparation of two oil of Rhizoma Zingiberis Recens crude product of comparative example
Rhizoma Zingiberis Recens powder 12.0kg obtained in Example one, loading extraction kettle (includes the extraction equipped with the western tower ring filler of rustless steel
Take post) in, supercritical CO2Entered in extraction kettle by extraction kettle bottom, extract through first time extraction and second, collect and merge
CO containing extract2, separate through first time parsing and second parsing separated, separating liquid I and separating liquid II is collected, is merged, obtain
To oil of Rhizoma Zingiberis Recens crude product；The pressure for extracting for the first time is 14MPa, temperature is 52 DEG C, CO2Flow velocity is 400L/h, the time is 45min；
The pressure of second extraction is 30MPa, temperature is 55 DEG C, CO2Flow velocity is 400L/h, the time is 30min；Parsing is separated for the first time
Pressure be 8MPa, temperature be 50 DEG C；Parse for the second time detached pressure for 6MPa, temperature be 48 DEG C.
Comparative example two is with the difference of embodiment two：The pressure of second extraction is changed into 30MPa from 24MPa.
In terms of Rhizoma Zingiberis Recens powder, the mass yield of oil of Rhizoma Zingiberis Recens crude product is 5.17%.Increase the pressure of second extraction, do not enter one
Step improves the yield of oil of Rhizoma Zingiberis Recens crude product, different from advance desired.
The preparation of example IV ginger essential oil
Oil of Rhizoma Zingiberis Recens crude product 0.5kg obtained in Example two, water-bath 15min under the conditions of 50 DEG C, stirring, 400rpm, when
Between be 6min.After standing, oil-water separation is carried out, vacuum filtration is carried out to oil phase, vacuum is -0.08Mpa, collects and obtains Rhizoma Zingiberis Recenss
Quintessence oil 0.459kg.Water-bath be in order to accelerate profit layering speed, but temperature can not be too high.
Ginger essential oil stable homogeneous, limpid transparent, not stratified after centrifugation.Component analyses, α-zingiberene are carried out to ginger essential oil
Content be 9.1% for the content of 28.5%, β-sesquiphellandrene, the content of farnesene is that 6.7%, 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 Rhizoma Zingiberis Recens crude product 0.5kg obtained in Example three, water-bath 15min under the conditions of 50 DEG C, stirring, 400rpm, when
Between be 6min.After standing, oil-water separation is carried out, vacuum filtration is carried out to oil phase, vacuum is -0.08Mpa, collects and obtains Rhizoma Zingiberis Recenss
Quintessence oil 0.453kg.
Ginger essential oil stable homogeneous, limpid transparent, not stratified after centrifugation.Component analyses, α-zingiberene are carried out to ginger essential oil
Content for 26.3%, β-sesquiphellandrene content 8.8%, the content of farnesene is that 7.2%, 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 Rhizoma Zingiberis Recens crude product 0.5kg obtained in comparative example one is taken, water-bath 15min under the conditions of 50 DEG C, stirring, 400rpm, when
Between be 6min.After standing, oil-water separation is carried out, vacuum filtration is carried out to oil phase, vacuum is -0.08Mpa, collects and obtains Rhizoma Zingiberis Recenss
Quintessence oil 0.461kg.
Component analyses are 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 1.8% for the content of 3.5%, 6- zingiberol, the content 3.8% of water.
The preparation of four ginger essential oil of comparative example
Oil of Rhizoma Zingiberis Recens crude product 0.5kg obtained in comparative example two is taken, water-bath 15min under the conditions of 50 DEG C, stirring, 400rpm, when
Between be 6min.After standing, oil-water separation is carried out, as a result：Vacuum filtration is carried out to oil phase, vacuum is -0.08Mpa, to collect
To ginger essential oil 0.448kg.
Component analyses are 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 6.9% for the content of 6.0%, 6- zingiberol, the content 4.1% of water.
The evaluation of test example ginger essential oil
Respectively to example IV, embodiment five, comparative example three and ginger essential oil obtained in comparative example four, and commercially available Rhizoma Zingiberis Recenss
Quintessence oil carries out the detection of acid number 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, as a result as shown in table 1.
The evaluation of the different ginger essential oils of table 1
As known from Table 1, obtained in preparation method of the present invention, ginger essential oil quality is good, and acid number and peroxide value are low, total ceramide
Content height, fragrance local flavor is good.The combination property of wherein example IV is optimal, and by specialty evaluation, personage is liked.
To example IV and ginger essential oil obtained in embodiment five carries out study on the stability, as a result：Shelf-life is up to 18
Month.
In sum, the preparation method that the present invention is provided, high income with oil of Rhizoma Zingiberis Recens crude product and ginger essential oil, when preparing
Between short the advantages of, obtained ginger essential oil quality is good, and acid number and peroxide value are low, and fragrance local flavor is good, long shelf-life.
Claims (10)
1. a kind of preparation method of ginger essential oil, it is characterised in that：Comprise the steps：
The preparation of S1 Rhizoma Zingiberis Recens powder：Rhizoma Zingiberis Recenss cleaning, drying to water content are 5～14%, to crush, obtain Rhizoma Zingiberis Recens powder；
The preparation of S2 oil of Rhizoma Zingiberis Recens crude product：The Rhizoma Zingiberis Recens powder that step S1 is obtained loads in extraction kettle, supercritical CO2By extraction kettle bottom
Enter in extraction kettle, extract through first time extraction and second, collect and merge the CO containing extract2, through first time parsing point
From separating with second parsing, separating liquid I and separating liquid II is collected, is merged, obtain oil of Rhizoma Zingiberis Recens crude product；
The preparation of S3 ginger essential oil：The oil of Rhizoma Zingiberis Recens crude product that step S2 is obtained is stirred under water bath condition, carries out oil-water separation, right
Oil phase carries out vacuum filtration, and vacuum is -0.07Mpa～-0.1Mpa, collects and obtains ginger essential oil.
2. the preparation method of ginger essential oil according to claim 1, it is characterised in that：The condition of the first time extraction
For：Pressure is 10～16MPa, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO, temperature is 40～60 DEG C, CO,2Flow velocity is 200～500L/h, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30～60min, the time is 30.
3. the preparation method of ginger essential oil according to claim 1, it is characterised in that：The condition of second extraction
For：Pressure is 20～28MPa, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO, temperature is 50～60 DEG C, CO,2Flow velocity is 300～500L/h, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20～60min, the time is 20.
4. the preparation method of ginger essential oil according to claim 1, it is characterised in that：The first time parses detached bar
Part is：40～55 DEG C of 5～10MPa of pressure, temperature.
5. the preparation method of ginger essential oil according to claim 1, it is characterised in that：Described parse detached bar for the second time
Part is：40～55 DEG C of 5～7MPa of pressure, temperature.
6. the preparation method of ginger essential oil according to claim 1, it is characterised in that：In step S1, dry to containing
The water yield is 6～12%, is crushed to 30～60 mesh.
7. the preparation method of ginger essential oil according to claim 1, it is characterised in that：In step S3, the temperature of water-bath
Spend for 45～60 DEG C, the time is 10～20min；The rotating speed of stirring is 200～500rpm, and the time is 5～10min.
8. 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.
9. the preparation method of ginger essential oil according to claim 8, it is characterised in that：Described filler is the western tower ring of rustless steel
Filler.
10. a kind of ginger essential oil, it is characterised in that：Preparation method by the ginger essential oil any one of claim 1 to 9
It is obtained.
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