CN104232311A - Extraction method of ginger essential oil - Google Patents
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- CN104232311A CN104232311A CN201410442134.9A CN201410442134A CN104232311A CN 104232311 A CN104232311 A CN 104232311A CN 201410442134 A CN201410442134 A CN 201410442134A CN 104232311 A CN104232311 A CN 104232311A
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Abstract
The invention discloses an extraction method of ginger essential oil. The method comprises the following steps: preparing ginger powder: slicing fresh ginger, soaking the sliced ginger in a 0.5-0.9wt% starch solution for 10-15min, drying and grinding the sliced ginger, and filtering obtained powder through a sieve of 60-80 meshes; preparing enzymatic hydrolysate: adding a de-ionized liquid 1-ethyl-3-methyl imidazole acetate ([Emim]OAc) to a disodium hydrogen phosphate-citrate buffer solution to obtain an ionic liquid system; adding the ginger powder to the ionic liquid system, controlling a material-to-liquid ratio at (1: 10)g/ml-(1: 20)g/mL, adding cellulase which is 2000-4000U/g in enzyme activity ratio and enzymatically hydrolyzing for 3-5h at 40-50 DEG C; and 3) essential oil extraction: and implementing enzyme deactivation to the system in a water bath after the reaction, ultrasonically extracting for 5-10min, conducting microwave treatment, filtering through gauze, centrifuging, standing and taking the de-ionized liquid on lower layer, spin-steaming, collecting oily matters having intense fragrance and drying the oily matters through anhydrous sodium sulfate to obtain the ginger essential oil.
Description
Technical field
The present invention relates to ginger essential oil extractive technique, be specifically related to a kind of extracting method of ginger essential oil.
Background technology
Ginger belongs to a kind of conventional crop that Zingiber is China, is also a kind of plant of medicine-food two-purpose.Ginger essential oil refers to the volatility oil content obtained from ginger rhizome, it is a kind of brown oil clear liquid, main component is sesquialter mushroom alkene class carbohydrate, is oxidized sesquialter mushroom ene compound, single mushroom alkene class carbohydrate and is oxidized single mushroom vinyl compound, has strong aromatic odour.Research shows that ginger essential oil has anticoagulation and preventing thrombosis, and adjusting blood lipid and the atherosclerotic effect of control, also have anti-oxidant, antibacterial effect, in the perfuming that simultaneously can also be used for food raw material and skin cosmetic.How the efficient ginger essential oil that extracts from ginger becomes study hotspot both domestic and external always.At present, the extracting method of ginger essential oil has a lot, and wherein steam distillation method extracts modal a kind of method of ginger essential oil, and additive method is as solvent method, milling process, supercritical CO
2extraction process etc.Steam distillation method is simple to operate, but shortcoming to be distillation time long, generally need about 7h, energy consumption is large; Solvent method needs to use a large amount of organic solvents as ether, sherwood oil etc., and the ginger essential oil of extraction can be made like this to remain a large amount of organic reagents; Supercritical CO
2extraction process is with CO
2for fluid, in the supercritical state ginger oil is extracted, harsher to the conditional request of reaction, cost is high.Enzymolysis assisted extraction essential oil is a kind of novel extracting method, and relevant report is less, compared with additive method, has extraction time short, effective constituent and destroys the advantages such as few.
Ionic liquid at room temperature is usually referred to as ionic liquid, it is made up of organic cation and inorganic or organic anion, there is volatility little, steam forces down, liquid state range is wide, dissolving power is low, the specific physical properties that extracting power is good, in organic synthesis, catalysis, be used widely in the fields such as extraction, as biocatalysis medium, the activity that ionic liquid physical efficiency improves enzyme accelerates enzymolysis speed, as extraction agent compared with traditional organic solvent, not only environmentally friendly, and can selectivity be improved, there is Heat stability is good, nonflammable, do not explode, non-volatile, be convenient to the feature reused.Therefore, we extract ginger essential oil with enzymolysis process, using ionic liquid both as the catalytic media of enzyme digestion reaction, again as the extraction solvent of ginger essential oil, adopt the essential oil in ultrasonic-microwave auxiliary extraction ginger, the impact that under research ion liquid system, ginger essential oil extracts, to providing a kind of new approach for the extraction of ginger essential oil.
Summary of the invention
The object of the present invention is to provide a kind of extracting method of ginger essential oil.The method effectively can extract ginger essential oil from ginger.
Object of the present invention is achieved through the following technical solutions.
An extracting method for ginger essential oil, comprises the steps:
(1) preparation of ginger powder: get ginger, washes the impurity on ginger surface with water, ginger is cut into the thin slice of 2 ~ 4mm, put into starch solution to soak, dry, dried ginger splices is put into high speed Universalpulverizer and pulverize 1 ~ 3min, cross 60 ~ 80 mesh sieves, obtain ginger powder;
(2) preparation of enzymolysis solution: in Sodium phosphate dibasic-citric acid solution, add ionic liquid 1-ethyl-3-methylimidazole acetate ([Emim] OAc), be mixed with the ionic liquid buffer system that volume fraction is 10% ~ 30%, ginger powder is added to ionic liquid buffer system, solid-liquid ratio 1:10 ~ 1:20g/mL, adding enzyme again lives than the cellulase of 2000 ~ 4000U/g, enzymolysis;
(3) extraction of ginger essential oil: go out the water-bath that system after reaction is placed in 80 ~ 90 DEG C ferment treatment 5 ~ 10min, be cooled to normal temperature, first ultrasonic extraction, rear microwave treatment, then filters with 4 layers of gauze, centrifugal, stratification takes off a layer ionic liquid, steams, collect the oily matter of strong fragrance at temperature 45 ~ 55 DEG C, vacuum tightness-0.06 ~-0.1Mpa backspin, with anhydrous sodium sulfate drying, obtain ginger essential oil.
In aforesaid method, described in step (1), starch solution mass percent concentration is 0.5% ~ 0.9%; Described soak time is 10 ~ 15min; The temperature of described drying is 60 ~ 80 DEG C, and the time is 6 ~ 8h.
In aforesaid method, described in step (2), the pH value of Sodium phosphate dibasic-citric acid solution is 6.5 ~ 8.5.
In aforesaid method, described in step (2), hydrolysis temperature is 40 ~ 50 DEG C, and the time is 3 ~ 5h.
In aforesaid method, described in step (3), the ultrasonic power of ultrasonic extraction is 220 ~ 250w, and the time is 5 ~ 10min; The power of described microwave treatment is 350 ~ 400w, and the time is 3 ~ 5min.
In aforesaid method, rotating speed centrifugal described in step (3) is 4500 ~ 5000r/min, and centrifugation time is 5 ~ 15min.
In aforesaid method, during the preparation of ginger powder, the starch solution that the ginger slice be cut into puts into 0.5% ~ 0.9% is soaked, prevents from occurring browning phenomenon in drying process and losing more effective constituent.
In aforesaid method, during ginger slice enzymolysis, add ionic liquid [Emim] OAc in buffer system, ionic liquid [Emim] OAc both can be used as the catalyzer of enzyme digestion reaction, also can as the extraction agent extracting ginger essential oil.
In aforesaid method, the ginger powder first prepared, through cellulase degradation process, on this basis using ionic liquid [Emim] OAc as extraction agent under the synergy of ultrasonic-microwave, extract ginger essential oil.
Principle of the present invention is as follows:
Ion liquid system principle: ionic liquid refers to the salt compounds be in a liquid state under room temperature or nearly room temperature be made up of organic cation and inorganic or organic anion.Have a wide range of applications in biological enzymolysis katalysis, its cardinal principle is, Mierocrystalline cellulose can directly be dissolved in ionic liquid at room temperature, and research finds that ionic liquid [Emim] OAc can Mierocrystalline cellulose effectively in degradation of cell wall, thus the carrying out of quickening enzyme digestion reaction; Ion liquid system can improve the selectivity of enzyme digestion reaction as the medium reacted, and can reduce the carrying out of enzymic catalytic reaction side reaction, maintains and even improves its regioselectivity and enantio-selectivity; And ionic liquid [Emim] OAc system, compared with traditional water solution system, can improve the thermostability of cellulase, not easy in inactivation.Ionic liquid [Emim] OAc as extraction agent, can have good selectivity to ginger essential oil, can avoid the introducing of other organic extractants like this, pollute ginger essential oil.
The principle of microwave extracting of the present invention is: microwave radiation process is that frequency electromagnetic waves penetrates the spe medium arrival microtubule fasolculus of internal batch and the process of glandular cell's system.Owing to absorbing micro-wave energy, the temperature of cell interior will rise rapidly, thus the ability making the pressure of cell interior exceed cell wall expansion to can bear, result cell rupture, effective constituent in it freely flows out, and is dissolved at a lower temperature in spe medium.By further filtering and being separated, required extract can be obtained.
Ultrasonic extraction principle of the present invention: ultrasonic wave is a kind of physical wave, in its communication process, the energy that ultrasonic wave has discharges gradually and acts on the physics particle in its propagation medium, thus makes these particles that corresponding physical change and chemical transformation occur.The ultrasonic topmost reason of strengthening effect to extraction is the micro-bubble that namely cavitation effect is present in liquid, be activated under the effect of ultrasonic field, show as the formation of complex, vibration, growth, a series of dynamic processes such as contraction and even collapse, and the physics and chemistry effect caused. bubble collapses suddenly within a few microsecond, the hot localised points up to 5 000 more than K can be formed, pressure can reach tens of and even up to a hundred MPas, along with the release of high pressure, form powerful shockwave (homogeneous phase) or high-speed jet (heterogeneous) in a liquid, its speed can reach the microjet that 100 m/ s. produce with ultrasonic cavitation, the mechanical effects such as shockwave exacerbate the less turbulence of system, accelerate mutually alternate mass transfer velocity. simultaneously, impingement flow produces a kind of physical shear power to animal and plant cells tissue, make it distortion, break, and discharge inclusion, thus the stripping of effective constituent in promotion cell.
Compared with prior art, advantage of the present invention is: present method have employed a kind of new system ionic liquid system and extracts ginger essential oil, reaction conditions is gentle, consuming time short, easy and simple to handle, extraction yield is high, whole process avoids the use of organic reagent, thus prevents organic reagent to the pollution of ginger essential oil, and the ionic liquid adopted is through process, can recycle, provide cost savings.At preparation Jiang Fenshi, have employed the guard method of ginger slice being put into starch solution and soaking, avoid a large amount of losses of ginger oil in drying process.
Embodiment
In order to understand the present invention better, below in conjunction with embodiment, the invention will be further described, but the scope of protection of present invention is not limited to the scope that embodiment represents.
embodiment 1:
The preparation of the first step ginger powder: select meat plump, fresh ginger 500g, the impurity on ginger surface is washed with flowing water, ginger is cut into the thin slice of 2mm, put into mass concentration be 0.7% starch solution soak 10min, dry 8h in the baking oven of 80 DEG C, dried ginger splices is put into high speed Universalpulverizer pulverize 2min, cross 60 mesh sieves, normal temperature sealing is preserved stand-by;
The preparation of second step enzymolysis solution: be in 7.0 Sodium phosphate dibasics-citric acid solution in pH value, add ionic liquid [Emim] OAc(Shanghai bio tech ltd), be mixed with the ionic liquid buffer system that volume fraction is 10%, get 10g ginger powder and add ionic liquid buffer system, solid-liquid ratio is made to be 1:15g/mL, adding enzyme lives than the cellulase (Guangzhou Qi Yun Bioisystech Co., Ltd) for 3000U/g, enzymolysis 3h under temperature is 40 DEG C of conditions;
The extraction of the 3rd step ginger essential oil: the water reacted enzymolysis solution being put into 80 DEG C goes out ferment treatment 10min, be cooled to normal temperature, under ultrasonic power 220w, ultrasonic extraction 10min, microwave power is 350w, microwave treatment 3min, then filter with 4 layers of gauze, at the centrifugal 10min of 4500r/min, stratification takes off a layer ionic liquid, at 45 DEG C, vacuum tightness is that-0.08Mpa backspin steams, and collects the oily matter of strong fragrance, with anhydrous sodium sulfate drying, obtain ginger essential oil, recording extraction yield is 1.8%.
embodiment 2:
The preparation of the first step ginger powder: select meat plump, fresh ginger 500g, the impurity on ginger surface is washed with flowing water, ginger is cut into the thin slice of 4mm, put into mass concentration be 0.5% starch solution soak 13min, dry 6h in the baking oven of 70 DEG C, dried ginger splices is put into high speed Universalpulverizer pulverize 3min, 70 mesh sieves, normal temperature sealing is preserved stand-by;
The preparation of second step enzymolysis solution: be in 6.5 Sodium phosphate dibasics-citric acid solution in pH value, add ionic liquid [Emim] OAc(Shanghai bio tech ltd), be mixed with the ionic liquid buffer system that volume fraction is 30%, get 10g ginger powder and add ionic liquid buffer system, solid-liquid ratio is made to be 1:10g/mL, adding enzyme lives than the cellulase (Guangzhou Qi Yun Bioisystech Co., Ltd) for 2000U/g, enzymolysis 4h under temperature is 45 DEG C of conditions;
The extraction of the 3rd step ginger essential oil: the water reacted enzymolysis solution being put into 85 DEG C goes out ferment treatment 5min, be cooled to normal temperature, under ultrasonic power 250w, ultrasonic extraction 8min, microwave power is 400w, microwave treatment 4min, then filter with 4 layers of gauze, at the centrifugal 5min of 5000r/min, stratification takes off a layer ionic liquid, at 55 DEG C, vacuum tightness is that-0.06Mpa backspin steams, and collects the oily matter of strong fragrance, with anhydrous sodium sulfate drying, obtain ginger essential oil, recording extraction yield is 1.6%.
embodiment 3:
The preparation of the first step ginger powder: select meat plump, fresh ginger 500g, the impurity on ginger surface is washed with flowing water, ginger is cut into the thin slice of 3mm, put into mass concentration be 0.9% starch solution soak 15min, dry 7h in the baking oven of 60 DEG C, dried ginger splices is put into high speed Universalpulverizer pulverize 1min, cross 60 mesh sieves, normal temperature sealing is preserved stand-by;
The preparation of second step enzymolysis solution: be in 8.5 Sodium phosphate dibasics-citric acid solution in pH value, add ionic liquid [Emim] OAc(Shanghai bio tech ltd), be mixed with the ionic liquid buffer system that volume fraction is 20%, get 10g ginger powder and add ionic liquid buffer system, solid-liquid ratio is made to be 1:20g/mL, adding enzyme lives than the cellulase (Guangzhou Qi Yun Bioisystech Co., Ltd) for 4000U/g, enzymolysis 5h under temperature is 50 DEG C of conditions;
The extraction of the 3rd step ginger essential oil: the water reacted enzymolysis solution being put into 90 DEG C goes out ferment treatment 8min, be cooled to normal temperature, under ultrasonic power 240w, ultrasonic extraction 5min, microwave power is 370w, microwave treatment 5min, filter with 4 layers of gauze, at the centrifugal 15min of 4800r/min, stratification takes off a layer ionic liquid again, at 50 DEG C, vacuum tightness is that-0.1Mpa backspin steams, and collects the oily matter of strong fragrance, with anhydrous sodium sulfate drying, obtain ginger essential oil, recording extraction yield is 1.5%.
embodiment 4:
The preparation of the first step ginger powder: select meat plump, fresh ginger 500g, the impurity on ginger surface is washed with flowing water, ginger is cut into the thin slice of 3mm, dry 8h in the baking oven of 60 DEG C, dried ginger splices is put into high speed Universalpulverizer and pulverize 2min, cross 70 mesh sieves, normal temperature sealing is preserved stand-by;
The preparation of second step enzymolysis solution: be in 8.5 Sodium phosphate dibasics-citric acid solution in pH value, add ionic liquid [Emim] OAc(Shanghai bio tech ltd), be mixed with the ionic liquid buffer system that volume fraction is 20%, get 10g ginger powder and add ionic liquid buffer system, solid-liquid ratio is made to be 1:15g/mL, adding enzyme lives than the cellulase (Guangzhou Qi Yun Bioisystech Co., Ltd) for 4000U/g, enzymolysis 5h under temperature is 50 DEG C of conditions;
The extraction of the 3rd step ginger essential oil: the water reacted enzymolysis solution being put into 90 DEG C goes out ferment treatment 8min, be cooled to normal temperature, under ultrasonic power 235w, ultrasonic extraction 5min, microwave power is 375w, microwave treatment 5min, filter with 4 layers of gauze, at the centrifugal 12min of 4800r/min, stratification takes off a layer ionic liquid again, at 50 DEG C, vacuum tightness is that-0.1Mpa backspin steams, and collects the oily matter of strong fragrance, with anhydrous sodium sulfate drying, obtain ginger essential oil, recording extraction yield is 0.8%.
The ginger powder prepared in embodiment 4 is more shallow than the ginger powder color arrived of first three embodiment; quality is lighter; final ginger essential oil extraction yield is also low than first three; visible ginger slice is put in starch solution soak have significant protective effect, prevent the loss that ginger essential oil is a large amount of when drying.
The above embodiment of the present invention is only for example of the present invention is clearly described, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments.All any amendments done within the spirit and principles in the present invention, equivalent to replace and improvement etc., within the protection domain that all should be included in the claims in the present invention.
Claims (6)
1. an extracting method for ginger essential oil, is characterized in that, comprises the steps:
(1) preparation of ginger powder: get ginger, washes the impurity on ginger surface with water, ginger is cut into the thin slice that 2 ~ 4mm is thick, put into starch solution to soak, dry, dried ginger splices is put into high speed Universalpulverizer and pulverize 1 ~ 3min, cross 60 ~ 80 mesh sieves, obtain ginger powder;
(2) preparation of enzymolysis solution: in Sodium phosphate dibasic-citric acid solution, add ionic liquid 1-ethyl-3-methylimidazole acetate ([Emim] OAc), be mixed with the ionic liquid buffer system that volume fraction is 10% ~ 30%, ginger powder is added to ionic liquid buffer system, solid-liquid ratio 1:10 ~ 1:20g/mL, adding enzyme again lives than the cellulase of 2000 ~ 4000U/g, enzymolysis;
(3) extraction of ginger essential oil: go out the water-bath that system after reaction is placed in 80 ~ 90 DEG C ferment treatment 5 ~ 10min, be cooled to normal temperature, first ultrasonic extraction, rear microwave treatment, then filters with 4 layers of gauze, centrifugal, stratification takes off a layer ionic liquid, steams, collect the oily matter of strong fragrance at temperature 45 ~ 55 DEG C, vacuum tightness-0.06 ~-0.1Mpa backspin, with anhydrous sodium sulfate drying, obtain ginger essential oil.
2. the extracting method of ginger essential oil according to claim 1, it is characterized in that, described in step (1), starch solution mass percent concentration is 0.5% ~ 0.9%; Described soak time is 10 ~ 15min; The temperature of described drying is 60 ~ 80 DEG C, and the time is 6 ~ 8h.
3. the extracting method of ginger essential oil according to claim 1, it is characterized in that, described in step (2), the pH value of Sodium phosphate dibasic-citric acid solution is 6.5 ~ 8.5.
4. the extracting method of ginger essential oil according to claim 1, it is characterized in that, described in step (2), hydrolysis temperature is 40 ~ 50 DEG C, and the time is 3 ~ 5h.
5. the extracting method of ginger essential oil according to claim 1, it is characterized in that, described in step (3), the ultrasonic power of ultrasonic extraction is 220 ~ 250w, and the time is 5 ~ 10min; The power of described microwave treatment is 350 ~ 400w, and the time is 3 ~ 5min.
6. the extracting method of ginger essential oil according to claim 1, it is characterized in that, rotating speed centrifugal described in step (3) is 4500 ~ 5000r/min, and centrifugation time is 5 ~ 15min.
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| CN109504538A (en) * | 2018-12-04 | 2019-03-22 | 贵州鼎立生物科技香料有限公司 | A kind of extracting method of ginger essential oil |
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| CN114958483A (en) * | 2022-04-08 | 2022-08-30 | 四川农业大学 | Quality-improving and efficiency-increasing method for Photinia sericea essential oil and compound essential oil containing Photinia sericea essential oil |
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| CN105647231A (en) * | 2016-03-25 | 2016-06-08 | 贵州大学 | Process for extracting curcumine in enzymic method-microwave method combination way |
| CN107488515B (en) * | 2017-09-30 | 2020-03-31 | 江苏农林职业技术学院 | Extracting solution and method for extracting tea tree flower essential oil by using same |
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| CN109055012A (en) * | 2018-08-08 | 2018-12-21 | 阜阳师范学院 | A kind of extracting method and its application of chinese rose essential oil |
| CN109504538A (en) * | 2018-12-04 | 2019-03-22 | 贵州鼎立生物科技香料有限公司 | A kind of extracting method of ginger essential oil |
| CN109363994A (en) * | 2018-12-07 | 2019-02-22 | 安阳工学院 | A kind of rosemary tears facial mask and preparation method thereof |
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| CN111995509A (en) * | 2020-07-31 | 2020-11-27 | 株洲千金药业股份有限公司 | Preparation method of gingerol |
| CN111995509B (en) * | 2020-07-31 | 2023-04-14 | 株洲千金药业股份有限公司 | Preparation method of gingerol |
| CN113209666A (en) * | 2021-06-17 | 2021-08-06 | 浙江大学 | Preparation method and application of ionic liquid solution containing nano bubbles |
| CN114958483A (en) * | 2022-04-08 | 2022-08-30 | 四川农业大学 | Quality-improving and efficiency-increasing method for Photinia sericea essential oil and compound essential oil containing Photinia sericea essential oil |
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