CN1854275A - Supercritical CO extraction of Angelica dehurical oil resin - Google Patents
Supercritical CO extraction of Angelica dehurical oil resin Download PDFInfo
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- CN1854275A CN1854275A CN 200510013353 CN200510013353A CN1854275A CN 1854275 A CN1854275 A CN 1854275A CN 200510013353 CN200510013353 CN 200510013353 CN 200510013353 A CN200510013353 A CN 200510013353A CN 1854275 A CN1854275 A CN 1854275A
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Abstract
The invention belongs to the field of extraction technology; he radix angelicae dahuricae oil resin extracted out belongs to food conditioner. The purpose of the patent is to ameliorate the deficiency of the current technology, to decrease the remainder of the organic solvent, and to improve the flavor of the extractant. The supercritical fluid CO2 extraction method of the radix angelicae dahuricae oil resin is as following, the radix angelicae dahuricae power of a certain quantity is put into the extraction kettle, then the temperature is set, when the temperature reach the setting value by heating or refrigeration, the system will be compressed by CO2 with the high pressure pump, when the pressure of the extraction kettle and the isolation kettle reach the setting value, the flux of CO2 is adjusted to a certain value at the same time, keep the extraction for a while at a unvarying temperature, pressure and flux, and then put the radix angelicae dahuricae oil resin out. The technology of this patent is simple, the time of it is just as much as one sixth of that of the solvent method, the extraction ratio is 5.04%, is 1.78% higher than the extraction ratio of solvent method which is 3.26%. The radix angelicae dahuricae oil resin extracted with the method has not solvent remainder, the color and the aroma of it is pure.
Description
Technical field
The invention belongs to the abstraction technique field, the angelica dahurica tincture resin that is extracted belong to the food seasoning field.
Background technology
The root of Dahurain angelica is the dry root of umbelliferae angelica per nnial herb.Kinds such as Radix angelicae dahuricae, Angelica anomala, Xingan's root of Dahurain angelica are arranged.The hot little hardship of distinguishing the flavor of, main component has Coumarins compound, root of Dahurain angelica element, root of Dahurain angelica ether, oxypeucedanin, coral element etc.The traditional Chinese medical science is used as medicine, and excited respiratory centre, blood vessel, motorial effect are arranged.In the cooking seasoning, going the function of having a strong smell because of its fragrant odour has except that raw meat, be used for meat product processing more, is the conventional perfumes in traditional sauce spiced and stewed food.The angelica dahurica tincture resin is a main taste composition wherein.
Oleo-resinous is meant the effective constituent of extracting in the natural perfume, is thick liquid.Except that containing essential oil, also contain nonvolatile composition, pigment, fat and other and be dissolved in material in the solvent in the oleo-resinous.Be the concentrated solution of natural flavoring agent effective constituent, its concentration reaches more than 10 times of fragrant hot raw material.Oleo-resinous can not only represent effective constituent, fragrance and the mouthfeel in the natural perfume relatively more balanced, and more complete.The modern food manufacturing mostly is tending towards using oleo-resinous to replace the natural flavoring agent powder.Water distillation and organic solvent extractionprocess are adopted in the production of present domestic spice oil resin mostly.These two kinds of methods have caused the loss of volatile component and water soluble component inevitably owing to adopt high temperature and organic solvent, and organic solvent residual influenced the local flavor of extract, and the goods organoleptic quality has been caused detrimentally affect.
Supercritical liquid extraction technique (being called for short SFE) is a new and high technology that grew up in recent years.Its principle of work is to utilize fluid (solvent) near stagnation point in a certain zone (being also referred to as supercritical region), have the behavior that balances each other unusually and transmit performance with the solute of mixture to be separated, and it the solute dissolving power is changed with pressure and temperature and in quite wide scope this characteristic of change reach the isolating technology of solute.This technology is widely used in fields such as spices, food, oil, chemical industry abroad.Supercutical fluid is a kind of fluid that has density of liquid and gas viscosity characteristics simultaneously, has characteristics such as high diffusibility, low viscosity, pollution-free, nonflammable, cold operation fragrance fragrance free of losses.Supercritical CO
2(SCCO
2) extraction all can influence rate of extraction and extraction efficiency as character such as its solvability of solvent, perviousness, diffustivity, polarity.The very near fluid of its density, but mass transfer performances is similar to coercible gas.SCCO
2Density can control by changing pressure and temperature, and density directly influences its dissolving power, so these characteristics of overcritical isolation technique just, is the new technology that replaces traditional separation method.
Summary of the invention
The objective of the invention is to improve the deficiencies in the prior art, reduce organic solvent residual, improve the local flavor of extract.The object of the present invention is achieved like this:
The supercritical CO of angelica dahurica tincture resin
2Extracting process is got a certain amount of Dahurian Angelica Root and is placed extractor, makes extractor, separator reach design temperature respectively by heating and refrigeration, adopts CO
2Fill and equilibrium system pressure, by high-pressure pump system is pressurizeed then,, regulate CO simultaneously when extractor reaches selected pressure
2Pump frequency, is emitted the angelica dahurica tincture resin at the state extraction for some time that keeps system's constant temperature, constant voltage, constant current amount.
Adopt the HA120-40-01 supercritical extraction unit, this device is made up of following equipment: carbon dioxide steel cylinder, refrigeration system, high-pressure pump, purification system, heating system, extractor, splitter group, collector, under meter, recovery system.
The root of Dahurain angelica is dried, controlling moisture content＜5%, the back was crushed to 30 mesh sieves with pulverizer, and was standby.The Dahurian Angelica Root that takes by weighing after a certain amount of aforementioned processing places extractor, and design temperature heats then and freezes, and opens CO when reaching design temperature
2Steel cylinder pressurizes to system by high-pressure pump, when extractor reaches selected pressure, regulates CO simultaneously
2Pump frequency reaches certain value, keeps the state extraction certain hour of constant temperature, constant voltage, constant current amount, emits the angelica dahurica tincture resin, and oil yield is calculated in weighing.
Influence determining of yield factor:
The factor that influences root of Dahurain angelica extraction oil yield is numerous, mainly contains the pressure of water content, grinding particle size, extraction of the root of Dahurain angelica and temperature, extraction time, CO
2Concentration, CO
2The frequency of pump, CO
2Flow velocity etc.
Determining of extraction parameter:
Treated root of Dahurain angelica sample according to the weighing of 100g/ part, under the identical situation of other control condition, is got different extracting pressure respectively, carry out supercritical extraction and determine best extracting pressure; Under the identical situation of other control condition, get different CO respectively
2Pump frequency is carried out supercritical extraction and is determined the optimum pressure pump frequency; Under the identical situation of other control condition, get different extraction temperature respectively and carry out supercritical extraction and determine best extraction temperature; Under the identical situation of other control condition, get the different extraction time respectively, carry out supercritical extraction and determine optimum extraction time.
Calculation formula is as follows: extraction oil yield (%)=extract quality/raw materials quality * 100% of angelica dahurica tincture resin
Description of drawings
Fig. 1 flow process and equipment connection diagram.Among the figure: 1, extractor, 2, separator I, 3, separator II, 4, CO
2Storage tank, 5, cleaner, 6, the extractor preheater, 7, CO
2Force (forcing) pump, 8, refrigerator, 9, separator I preheater, 10, separator II preheater, 11, extractor pressure regulator valve, 12, separator I pressure regulator valve, 13, blow-off valve, 14, separator II pressure regulator valve, 15, separator I baiting valve, 16, separator II baiting valve.
Fig. 2 is at constant CO
2Pump frequency and under the extraction time, under the condition of different temperatures, extracting pressure is to the graph of a relation of extraction oil yield influence.
Fig. 3 is CO
2Under the pump frequency controlled condition, during the identical extraction time (2h), under the different extracting pressure states, extraction temperature is to the graph of a relation of extraction results influence.
Fig. 4 is constant 45 ℃ an of extraction temperature, during the extraction time identical (2h), and under the different extracting pressure, CO
2Pump frequency is to the graph of a relation of extraction results influence.
Fig. 5 is extraction CO
2When pump frequency was constant, the extraction time was to the graph of a relation of extraction results influence.
Embodiment
Determining of example l extracting pressure:
Referring to accompanying drawing 2, in the supercritical extraction process of the root of Dahurain angelica, carry agent and CO not using
2Under the certain condition of flow, extracting pressure and extraction temperature are the topmost factors that influences extraction results.Under the certain temperature, supercritical CO
2Density increases along with the increase of pressure, thereby dissolving power is increased, and the extraction oil yield increases.Be CO
2The solubleness of middle dissolved substance becomes positive correlation with its pressure.As seen from Figure 2, extracting pressure and extraction oil yield are not linear.Along with the increase of pressure, the raising of effective constituent extraction efficiency eases up, and too high pressure can make the corresponding increase with process cost of equipment simultaneously.Analysis-by-synthesis as a result by experiment, selected best extracting pressure: 25MPa.
Determining of example 2 extraction temperature:
Referring to accompanying drawing 3, temperature raises, and molecular thermalmotion speed increases, CO
2Dissolving power increases; But simultaneous temperature raises and also makes supercritical CO
2Density reduces, and the corresponding decline of its dissolving power causes extraction efficiency to descend.The size of extraction oil yield depends primarily under this temperature, and which kind of state is dominant.(35 ℃) extraction oil yield was lower when as can be seen from Figure 3, temperature reduced; Along with temperature raises, the extraction oil yield raises, and 45 ℃ reach the highest; Temperature continue to raise, and extracts to such an extent that oilyly descend on the contrary.So choosing best extraction temperature is: 45 ℃.
Example 3 best CO
2Determining of pump frequency:
Referring to accompanying drawing 4, CO
2Pump frequency major control CO
2Flow.CO
2The increase of pump frequency can be accelerated the flow velocity of supercutical fluid by material, thereby the supercritical flow volume density is increased, thereby the solubleness of solute increases, and extraction reaches balance time to be shortened, and has improved the extraction oil yield.As seen from Figure 4, along with CO
2The increase of pump frequency, the extraction oil yield is raising in various degree, but works as CO
2When pump frequency reached 28Hz, extraction results was constant substantially.CO is described
2Pump frequency to the influence of extraction results substantially near balance.
Determining of 4 extraction times of example:
Referring to accompanying drawing 5, CO
2Pump frequency one regularly, along with the prolongation of time, the extraction oil yield is in continuous increase, but along with the prolongation of time, curve is progressively mild.As seen from Figure 5, the variation tendency of curve can illustrate among the figure, and the extraction extraction time in early stage to the extraction results influence significantly reduces relatively to this influence of later stage.As the important parameter in the suitability for industrialized production, take all factors into consideration equipment energy consumption and the relation that extracts oil yield in the actual production, optimum extraction time is chosen as 2 hours.
The test of example 5 parameter optimizations:
With angelica dahurica tincture resin extraction yield is index, on the basis of single factor experiment, with extracting pressure, temperature, CO
2Flow, extraction time four factors are variable, carry out the orthogonal test L9 (3 of four factors, three levels
4), thereby the best of breed of definite supercritical extraction angelica dahurica tincture resin.
Table 1 level of factor table
Table 2 extracting pressure, temperature, time, CO
2Flow is to the result that influences of angelica dahurica tincture extraction yield
| Test number | Pressure (Mpa) | Temperature (℃) | CO 2Flow (Kg/h) | Time (h) | Angelica dahurica tincture |
| 1 2 3 4 5 6 7 8 9 | 20 20 20 25 25 25 30 30 30 20.5 | 40 45 50 40 45 50 40 45 50 22.4 | 25 28 30 25 28 30 25 28 30 26.1 | 1.5 2 2.5 1.5 2 2.5 1.5 2 2.5 23.3 | 3.15 3.38 4.72 4.75 5.21 5.02 4.28 4.86 4.96 T＝71.9 |
| K 2 K 3 k 1 k 2 k 3 R | 24.5 26.9 6.83 8.17 8.97 2.13 | 26.2 23.3 7.47 8.73 7.77 1.27 | 24.3 21.5 8.7 8.1 7.17 0.93 | 24.1 24.5 7.77 8.03 8.17 0.13 | Y＝7.99 |
On the basis of single factor experiment, adopt the orthogonal design scheme of four factors, three levels, under 9 kinds of different processing condition, extract the angelica dahurica tincture resin, measure percentage extraction respectively.The results are shown in Table 2.
The intuitive analysis method is adopted in test, and K, the k of each factor and the size of R (extreme difference) value are carried out relevant the analysis.Can obtain following result:
The descending order of extreme difference R is pressure＞temperature＞flow＞time, and the extreme difference value is big more, reflects that this factor is big more to the influence of desired value, illustrates that the principal element that influences the extraction of angelica dahurica tincture resin in extraction process is an extracting pressure, secondly is extraction temperature, CO
2Flow is the extraction time at last.
His-and-hers watches 2 are analyzed, and result's (angelica dahurica tincture resin yield) of visible No. 6 test is best, is 5.21%, we can say the very preferable processing condition of condition that this test is corresponding: extracting pressure 25MPa, 45 ℃ of extraction temperature, CO
2Pump frequency 28Hz, extraction time 2h.
The supercritical CO 2 extraction example of example 6 angelica dahurica tincture resins
Referring to accompanying drawing 1, among the figure: 1, extractor, 2, separator I, 3, separator II, 4, CO
2Storage tank, 5, cleaner, 6, the extractor preheater, 7, CO
2Force (forcing) pump, 8, refrigerator, 9, separator I preheater, 10, separator II preheater, 11, extractor pressure regulator valve, 12, separator I pressure regulator valve, 13, blow-off valve, 14, separator II pressure regulator valve, 15, separator I baiting valve, 16, separator II baiting valve.
Extraction process:
(1) the coarse reduction 30 purpose roots of Dahurain angelica are packed into barrel is put into extractor 1, builds pressure ring and upper plug head.
(2) open refrigerator 8 refrigeration, refrigeration temperature drops to 0 ℃ ± 5 ℃.
(3) with extractor 1, separator I 2, separator II 3, each corresponding preheater 6,9,10 water tanks heating.Controlled temperature respectively: 45 ℃ of extractors, 43.5 ℃ of separator I, 40 ℃ of separator II, connect the hot water circulation that adds of each water tank, keep homo(io)thermism.
(4) valve-off 11,12,13,14, open CO
2Tank valve allows CO
2Enter extractor, treat pressure equilibrium after, bleed off the residual air of extractor, close after falling a part of pressure.
(5) pressurization.By monitoring CO
2Flow control pressure pump frequency, flow is little, accelerates pump frequency; Flow is big, and pump frequency slows down.When pressure was added to 25MPa, pump frequency was 28Hz, opened the by-pass valve control of extractor back, with the pressure of valve 11 control extractors, with it constant be 25Mpa, valve 12,14 is controlled the pressure of separation 2,3 respectively.
(6) extraction.At pressure 25Mpa, 45 ℃ of extraction temperature, 43.5 ℃ of separation temperatures, CO
2Pump frequency 28Hz, the controlled condition extraction root of Dahurain angelica 2 hours.
(7) after the extraction, close cold machine, pump and each heating cycle.The pressure of extractor is put into the separator of back, treat extractor internal pressure and back face balance after, close valve before and after the extractor, emptying.After treating that extractor does not have pressure, open extractor, take out barrel, bleed off waste material.
(8) with the pressure of separator, the angelica dahurica tincture resin of separating is taken out by baiting valve 15,16.Whole extraction process finishes.
Comparison root of Dahurain angelica solvent extration with solvent method:
Pulverizings of earlier root of Dahurain angelica being milled by solid-to-liquid ratio 1: 20, use 50% alcohol solution dipping, after 80 ℃ of water-baths refluxed 6 hours, and filtration, filtrate recovery.And filter residue is used 50% alcohol solution dipping again, and water-bath refluxed 6 hours, filters, and filtrate is mixed with filtrate last time, removes filter residue, is root of Dahurain angelica extractive substance.
SFE and solvent method compare:
Table 3 SFE and solvent extraction result are relatively
| SFE | Solvent extration | |
| The mobile extractant of technology extraction time weight yield (%) purity (%) extraction yield (%) outward appearance fragrance is residual | The pure nothing that flows of the complete 2h 5.21 96.78 5.04 fawn oily liquids of single extraction | The secondary lixiviate is filtered 12h 8.27 39.42 3.26 pitchy body of paste gas astringent taste hardships three times, has the alcohol smell poor fluidity to carry ethanol water secretly |
As shown in Table 3, SFE technology is simple; Its extraction time is 1/6 of solvent method; SFE percentage extraction 5.04% is than the percentage extraction 3.26% also high 1.78% of solvent method; The angelica dahurica tincture resin no solvent residue of SFE extraction, color and luster is good, and fragrance is pure; The weight yield of solvent extration is higher than the SFE yield, but purity (angelica dahurica tincture resin content) is low, illustrates that the invalid components (impurity) of solvent extraction is more.In sum, supercritical CO
2The technology of extraction angelica dahurica tincture resin is better than solvent method.
Claims (7)
1, the supercritical CO of angelica dahurica tincture resin
2Extracting process is got a certain amount of Dahurian Angelica Root and is placed extractor, makes extractor, separator reach design temperature respectively by heating and refrigeration, adopts CO
2Fill and equilibrium system pressure, by high-pressure pump system is pressurizeed then,, regulate CO simultaneously when extractor reaches selected pressure
2Pump frequency, is emitted the angelica dahurica tincture resin at the state extraction for some time that keeps system's constant temperature, constant voltage, constant current amount.
2, the supercritical CO of angelica dahurica tincture resin according to claim 1
2Extracting process is characterized in that described extracting pressure is 15～30Mpa.
3, the supercritical CO of angelica dahurica tincture resin according to claim 1
2Extracting process is characterized in that described extraction temperature is 40～50 ℃.
4, the supercritical CO of angelica dahurica tincture resin according to claim 1
2Extracting process is characterized in that described CO
2Pump frequency is 15 ~ 30Hz.
5, the supercritical CO of angelica dahurica tincture resin according to claim 1
2Extracting process is characterized in that the described extraction time is 1～2.5h.
6, the supercritical CO of angelica dahurica tincture resin according to claim 1
2Extracting process is characterized in that described Dahurian Angelica Root fineness is 20～40 orders.
7, the supercritical CO of angelica dahurica tincture resin according to claim 1
2Extracting process is characterized in that described Dahurian Angelica Root water content＜5%.
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| CN101863896A (en) * | 2010-06-22 | 2010-10-20 | 浙江大学 | Composite extraction method for extracting coumarin from radix angelicae dahuricae |
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| CN113430050A (en) * | 2021-06-16 | 2021-09-24 | 江苏第二师范学院 | Preparation method of antioxidant essential oil of angelica dahurica |
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| CN101863896A (en) * | 2010-06-22 | 2010-10-20 | 浙江大学 | Composite extraction method for extracting coumarin from radix angelicae dahuricae |
| CN101863896B (en) * | 2010-06-22 | 2012-07-18 | 浙江大学 | Composite extraction method for extracting coumarin from radix angelicae dahuricae |
| CN104498177A (en) * | 2014-11-24 | 2015-04-08 | 广西壮族自治区亚热带作物研究所 | Method used for extracting piper sarmentosum oleoresin, and obtained piper sarmentosum oleoresin |
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| CN110003982A (en) * | 2019-04-10 | 2019-07-12 | 范加家 | A kind of combined type borneol method of extraction of essential oil |
| WO2021057936A1 (en) * | 2019-09-26 | 2021-04-01 | 上海复璐帝流体技术有限公司 | Supercritical carbon dioxide extraction apparatus and method thereof |
| CN113430050A (en) * | 2021-06-16 | 2021-09-24 | 江苏第二师范学院 | Preparation method of antioxidant essential oil of angelica dahurica |
| CN113750566A (en) * | 2021-09-30 | 2021-12-07 | 王强 | Supercritical fluid extraction device and method and application |
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