CN103333741A - Preparation method for subcritical fennel essential oil water extraction - Google Patents
Preparation method for subcritical fennel essential oil water extraction Download PDFInfo
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- CN103333741A CN103333741A CN2013103011249A CN201310301124A CN103333741A CN 103333741 A CN103333741 A CN 103333741A CN 2013103011249 A CN2013103011249 A CN 2013103011249A CN 201310301124 A CN201310301124 A CN 201310301124A CN 103333741 A CN103333741 A CN 103333741A
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- extraction
- essential oil
- fennel
- deionized water
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- 239000000341 volatile oil Substances 0.000 title claims abstract description 42
- 235000004204 Foeniculum vulgare Nutrition 0.000 title claims abstract description 30
- 238000003809 water extraction Methods 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 240000006927 Foeniculum vulgare Species 0.000 title 1
- 238000000605 extraction Methods 0.000 claims abstract description 45
- 241000212314 Foeniculum Species 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 11
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 238000007789 sealing Methods 0.000 claims abstract description 4
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- 238000007601 warm air drying Methods 0.000 claims description 3
- 238000002203 pretreatment Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 3
- 235000011164 potassium chloride Nutrition 0.000 abstract description 2
- 239000001103 potassium chloride Substances 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract description 2
- 239000012141 concentrate Substances 0.000 abstract 1
- 230000032798 delamination Effects 0.000 abstract 1
- 239000012467 final product Substances 0.000 abstract 1
- 238000007602 hot air drying Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 239000000284 extract Substances 0.000 description 14
- 238000000034 method Methods 0.000 description 13
- 238000004821 distillation Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 238000001256 steam distillation Methods 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000003205 fragrance Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 244000205574 Acorus calamus Species 0.000 description 1
- 235000011996 Calamus deerratus Nutrition 0.000 description 1
- 206010010774 Constipation Diseases 0.000 description 1
- 239000004278 EU approved seasoning Substances 0.000 description 1
- 240000008415 Lactuca sativa Species 0.000 description 1
- 240000004760 Pimpinella anisum Species 0.000 description 1
- 235000012550 Pimpinella anisum Nutrition 0.000 description 1
- 208000004880 Polyuria Diseases 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000003579 anti-obesity Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 210000004556 brain Anatomy 0.000 description 1
- 235000008429 bread Nutrition 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000004332 deodorization Methods 0.000 description 1
- 230000035619 diuresis Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 235000011194 food seasoning agent Nutrition 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
- 230000005501 phase interface Effects 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 235000012045 salad Nutrition 0.000 description 1
- 235000014102 seafood Nutrition 0.000 description 1
- 230000007226 seed germination Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000009331 sowing Methods 0.000 description 1
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 description 1
- 238000000194 supercritical-fluid extraction Methods 0.000 description 1
- 239000013076 target substance Substances 0.000 description 1
- 229940034610 toothpaste Drugs 0.000 description 1
- 239000000606 toothpaste Substances 0.000 description 1
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Abstract
The invention provides a preparation method for subcritical fennel essential oil water extraction, which comprises the following steps: hot-air drying fennel seeds for 24 h, smashing the fennel seeds, enabling the smashed fennel seeds to pass through a 40-mesh sieve, sealing and storing the final product at ordinary temperature for standby; to be specific, putting pre-processed powder into an extraction tank; conveying deionized water to a pre-heater to preheat through a pressure pump, and enabling the heated deionized water to enter the extraction tank when the deionized water is heated to 100-180 DEG C, wherein the mass ratio of the deionized water and the powder is 10 : 1, and the pressure is 10 Mpa; adding a certain amount of potassium chloride to fully stir and adding absolute alcohol after extraction for a while, wherein the proportion of the extracting solution and the absolute alcohol is 1 : 1; uniformly mixing and still standing the extracting solution and the absolute alcohol for 40 min for delamination; obtaining the fennel essential oil after the alcohol evaporates and concentrates. According to the invention, the problems of element breakage, low recovery ratio and the like caused by extraction solvent residue and overlong extraction time in the traditional essential oil extraction technology can be solved, the cost is low, the production technology is simple, the yield is high and the preparation method is suitable for commercial production.
Description
Technical field
The present invention relates to a kind of method of extraction of essential oil, relate in particular to a kind of preparation method of Subcritical Water Extraction fennel essential oil.
Background technology
Europe fennel (Pimpinella anisum L.), Proterozoic is mostly at Continent of Europe and U.S.West Coast.Umbelliferae Foeniculum per nnial herb, brightly yellowish look, spring and autumn sowing, vegetative period 100 d, cold-resistant drought-enduring impoverishment tolerant.The special fragrant of tool, the cauline leaf edible, leaf can be mended brain, improves memory, and can be used as the batching of seafood and salad, increases mouthfeel.Seed can be used for seasonings such as bread, coffee, alec.Can make breath freshening after seed is chewed, help digest and dissolve constipation.Leaf, stem, seed germination
After can mix cold dish.Essential oil can be used for making toothpaste, the detoxifcation diuresis of extract tool and the antiobesity action of root, and Turkey is widely used in this kind of plant in the liquor production.But liquid deep layer cleaning skin is got in seed and blade refining, uses a small amount of essential oil massage muscle, can slow down fatigue.There is research report fennel essential oil to have anti-oxidant and bacteriostasis.
The extracts essential oil method mainly contains steam distillation, organic solvent extraction, dry distillation and supercritical carbon dioxide extraction method etc.The essential oil of dry distillation has the smell of burning, and color is dark, and fragrance is destroyed, the burnt deodorization of need dispelling; The essential oil separating technology complexity of organic solvent lixiviate has dissolvent residual, has limited use range; The essential oil cost height of CO2 supercritical extraction; So at present the most effective, method is still with steam distillation and extracts plants essential oil the most widely.But conventional steam distillation is directly used in extracts essential oil also exists some problems to need to solve: when distillation temperature was low, the essential oil yield was lower, and distillation time is long, the Long contact time of fragrance matter and water and the too much hydrolysis of quilt; When distillation temperature was high, owing to be heated for a long time, the essential oil color of extraction was darker, even some activeconstituents heated denaturalization wherein again.
Respect and think the group and wait and delivered the optimum process condition that research steam distillation in " fennel essential oil extraction process is optimized and composition analysis " document prepares essential oil of fennel seeds, power is 110W, liquid ratio is 7:1, and distillation time is 4.0 h, and the extraction yield that makes essential oil of fennel seeds is 3.98%.
Application number: 96118216.4 extract technology and the method for essential oil from the fennel calamus plant, this invention is the fennel calamus to be gathered herb carry out air-dry processing, extracts essential oil by distillating method then, the air-dry 70-80% of plant, distillation time 2-4 hour, then oily water separation is become essential oil.The yield that this method obtains is not high.
Summary of the invention
Exist many more formidable problems for solving traditional essential oil extracting process, composition residual as extraction solvent, that the extraction overlong time causes destroys, the rate of recovery is low etc., seriously influenced the essential oil quality, it is low to the invention provides a kind of cost, production technique is simple, the yield height, the preparation method of the Subcritical Water Extraction fennel essential oil that is fit to commercially produce.
The present invention adopts the Subcritical Water Extraction technology that essential oil of fennel seeds is extracted research.Subcritical water refers under certain pressure, and water is heated to 100 ℃ with the high temperature of upper critical temperature below 374 ℃, and water still keeps liquid state.The specific inductivity of water is 78. 85 under the normal temperature and pressure, belongs to polar solvent.Under subcritical state, keeping suitable pressure is in a liquid state water, along with the rising of temperature has weakened hydrogen bond action between the water molecules, the polarity of water is reduced greatly, gradually become nonpolar by strong polarity, utilize this characteristic can from raw material, optionally extract the target substance of opposed polarity.In addition, intensification can also reduce the Film strength of solid-liquid phase interface, accelerates solvent and spreads to solid interior by the space, reduces surface tension and viscosity, increases the solubleness of organic active substance in water, improves percentage extraction.
A kind of preparation method of Subcritical Water Extraction fennel essential oil:
1) with the fennel seed more than warm air drying 24 h, pulverized 40 mesh sieves, sealing normal temperature is preserved standby.
2) pre-treatment is good powder is put into extractor, by pressure pump deionized water is transported to preheating in the preheater, deionized water is heated to 100-180 ℃ and enters into extractor, and the quality of deionized water and powder is 10:1, and extractor pressure is 10MPa, behind the extraction 15-60min, add a certain amount of Repone K and fully stir, add dehydrated alcohol, extracting solution and dehydrated alcohol ratio 1:1, mix and leave standstill the 40min layering, collect the dehydrated alcohol evaporation concentration and get the fennel essential oil.Extraction temperature is preferably 130 ℃, extraction time and is preferably 35min.
Add the abundant stirring and dissolving of a certain amount of Repone K among the present invention, to play demulsification (weight such as potassium chloride dosage and fennel seed powder).
Through experimental study, along with the prolongation of extraction time, extraction yield is not more and more higher, and along with the increase of extraction time, extraction yield reduces on the contrary.This may with component between exist " dissolving is helped each other " effect relevant, extraction time is long, owing to the decomposition of some component wherein promotes to lose the advantage of guiding and supporting mutually.So it is optimum extraction time that the present invention selects 35min for use.
Extraction temperature is the important parameter that subcritical water extracts essential oil.Consider the condition restriction of subcritical state water temperature, select all more than 100 ℃ so extract the parameter of temperature; Find that in experimentation when extracting temperature above 180 ℃, extract has tangible burnt burning, and extraction yield can descend significantly.So the present invention selects for use 130 ℃ to be best extraction temperature.
The present invention adopt Subcritical Water Extraction with its save time, economize can, efficient, high-quality characteristics are better than other traditional extraction techniques, suitable at abstraction technique aspect extracting power, extraction yield, selectivity, the product quality with the supercritical CO 2 extraction process, but the supercritical CO 2 extraction process must can extract under the ultra-high voltage state more than 25 MPa, and the pressure of subcritical water is significantly less than the ultra-high voltage state, make and the easier realization on equipment of Subcritical Water Extraction technology also more be adapted to the industrial applications that essential oil of fennel seeds is produced.
Embodiment 1
The extraction time is to the influence of essential oil yield
According to the method described above, get degree of grinding 40 order fennel powder 100g, put into extractor, extracting pressure 10MPa, 150 ℃ of extraction temperature respectively 15,25,35,45, extract under the condition of 60min, are calculated extract yield.
The table 1 extraction time is to the influence of essential oil yield
| The extraction time (min) | Extraction yield (%) |
| 15 | 4.12 |
| 25 | 4.98 |
| 35 | 5.98 |
| 45 | 4.56 |
| 60 | 4.07 |
Embodiment 2 extraction temperature are to the influence of essential oil yield
According to the method described above, get degree of grinding 40 order fennel powder 100g, put into extractor, extracting pressure 10MPa, extraction temperature is extracted under the condition of extraction temperature 35min respectively 100,110,130,150,180 ℃ of conditions, calculates extract yield.
Table 2 extraction temperature is to the influence of essential oil yield
| Extraction temperature ℃ | Extraction yield % |
| 100 | 3.04 |
| 110 | 4.05 |
| 130 | 5.72 |
| 150 | 4.74 |
| 180 | 4.01 |
Embodiment 3
The fennel seed through warm air drying 24 h, was pulverized 40 mesh sieves, and sealing normal temperature is preserved standby.The 100g powder is put into extractor, by pressure pump deionized water is transported to preheating in the preheater, deionized water is heated to 130 ℃ and enters into extractor, and the quality of deionized water and powder is 10:1, and extractor pressure is 10Mpa, behind the extraction 35min, add a certain amount of Repone K and fully stir, add dehydrated alcohol, extracting solution and dehydrated alcohol ratio 1:1, mix and leave standstill the 40min layering, collect the dehydrated alcohol evaporation concentration and get the fennel essential oil.Extraction yield is that 5.87%, GC method mensuration essential oil content is 95.2%.
Claims (3)
1. the preparation method of a Subcritical Water Extraction fennel essential oil is characterized in that step is as follows:
1) with the fennel seed more than warm air drying 24 h, pulverized 40 mesh sieves, sealing normal temperature is preserved standby;
2) pre-treatment is good powder is put into extractor, by pressure pump deionized water is transported to preheating in the preheater, deionized water is heated to 100-180 ℃ and enters into extractor, and the quality of deionized water and powder is 10:1, and extractor pressure is 10Mpa, behind the extraction 15-60min, add a certain amount of Repone K and fully stir, add dehydrated alcohol, extracting solution and dehydrated alcohol ratio 1:1, mix and leave standstill the 40min layering, collect the dehydrated alcohol evaporation concentration and get the fennel essential oil.
2. according to the preparation method of the described Subcritical Water Extraction fennel of claim 1 essential oil, it is characterized in that extraction temperature is 130 ℃.
3. according to the preparation method of the described Subcritical Water Extraction fennel of claim 1 essential oil, it is characterized in that the extraction time is 35min.
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| CN2013103011249A CN103333741A (en) | 2013-07-18 | 2013-07-18 | Preparation method for subcritical fennel essential oil water extraction |
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| CN2013103011249A CN103333741A (en) | 2013-07-18 | 2013-07-18 | Preparation method for subcritical fennel essential oil water extraction |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103849468A (en) * | 2014-03-12 | 2014-06-11 | 青海清华博众生物技术有限公司 | Garlic essential oil extraction method |
| CN105907474A (en) * | 2016-06-12 | 2016-08-31 | 刘小华 | A kind of essential oil extraction process and equipment |
| CN108179065A (en) * | 2017-12-27 | 2018-06-19 | 安徽香杰香精科技有限公司 | A kind of extracting method of jasmine essential oil |
| CN108949351A (en) * | 2017-05-25 | 2018-12-07 | 无限极（中国）有限公司 | Fennel seeds extraction process of active component |
| CN114437870A (en) * | 2021-12-22 | 2022-05-06 | 广东石丰农业科技有限公司 | Extraction preparation process of essential oil of Abelmoschus manihot |
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| CN101274156A (en) * | 2007-12-18 | 2008-10-01 | 华南理工大学 | Ultrasound-enhanced subcritical water extraction method and device for active ingredients of natural products |
| CN102165973A (en) * | 2011-04-11 | 2011-08-31 | 山东三星玉米产业科技有限公司 | Flavor corn oil and preparation method thereof |
| CN102204663A (en) * | 2011-05-06 | 2011-10-05 | 新疆大学 | Tomato sauce added with fennel essential oil |
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2013
- 2013-07-18 CN CN2013103011249A patent/CN103333741A/en active Pending
Patent Citations (4)
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| CN102165973A (en) * | 2011-04-11 | 2011-08-31 | 山东三星玉米产业科技有限公司 | Flavor corn oil and preparation method thereof |
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Non-Patent Citations (2)
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103849468A (en) * | 2014-03-12 | 2014-06-11 | 青海清华博众生物技术有限公司 | Garlic essential oil extraction method |
| CN105907474A (en) * | 2016-06-12 | 2016-08-31 | 刘小华 | A kind of essential oil extraction process and equipment |
| CN108949351A (en) * | 2017-05-25 | 2018-12-07 | 无限极（中国）有限公司 | Fennel seeds extraction process of active component |
| CN108179065A (en) * | 2017-12-27 | 2018-06-19 | 安徽香杰香精科技有限公司 | A kind of extracting method of jasmine essential oil |
| CN114437870A (en) * | 2021-12-22 | 2022-05-06 | 广东石丰农业科技有限公司 | Extraction preparation process of essential oil of Abelmoschus manihot |
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Application publication date: 20131002 |