CN102836297B - Method for extracting rhizoma acori graminei volatile oil by microwaves - Google Patents
Method for extracting rhizoma acori graminei volatile oil by microwaves Download PDFInfo
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- CN102836297B CN102836297B CN201110172547.6A CN201110172547A CN102836297B CN 102836297 B CN102836297 B CN 102836297B CN 201110172547 A CN201110172547 A CN 201110172547A CN 102836297 B CN102836297 B CN 102836297B
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Abstract
The invention discloses a method for extracting rhizoma acori graminei volatile oil by microwaves. The method comprises the following steps of: fetching a rhizoma acori graminei medical material; adding 8-10 weight times of distilled water, and soaking for 3-6 hours; putting in a microwave extractor; and extracting for 80-120min under the power of 600-800W to obtain the rhizoma acori graminei volatile oil. The technical scheme has the biggest characteristics that the extracting speed is high; the time is saved; the solvent consumption is low; and the effective component yield is high. Integrating the factors of all aspects, the technical scheme disclosed by the invention has the remarkable advantage of high extracting efficiency, and is very good in popularization and application prospect.
Description
Technical field
The present invention relates to Rhizoma Acori Gramineii extract method and technology field, particularly relate to a kind of method of microwave extraction Rhizoma Acori Graminei volatile oil.
Background technology
Rhizoma Acori Graminei (
acoro tatarinowischot) be the dry rhizome of acorus gramineus araceae plant, in the volatile oil extracting, containing number of chemical compositions such as volatile oil, saccharide, organic acid, aminoacid, main component is asaricin, has effect of removing dampness appetizing, the eliminating phlegm of having one's ideas straightened out, refreshment Fructus Alpiniae Oxyphyllae.Secondly be caryophyllene, sekishone, asarylaldehyde, α-greenweed alkene, cis methyl isobutyl phenol, elemicin, dimerization-asaricin, γ-asaricin, d-δ cadinene, nutmeg acid, thymol etc.Generally believe that Rhizoma Acori Graminei volatile oil has dual regulation to nervus centralis, both tranquillizing and allaying excitement (calm, convulsion), again consciousness-restoring and orifice-opening (excited, antidepressant).Asaricin is as the main effective ingredient in Rhizoma Acori Graminei volatile oil, extract, but according to many results of study, the extracting method of Rhizoma Acori Graminei volatile oil do not have best by a lot of people's research and by several different methods.Conventional extracting method has steam distillation now, has the shortcoming that extraction time is long, solvent consumption is large, extraction efficiency is low.
Microwave extracting is to utilize microwave to improve a kind of new technique of extraction yield.Microwave heating belongs to inner heating process, effective ingredient in energy enrichment medical material after microwave radiation, have the advantages that selectivity is high, the operating time is short, solvent consumption is few, effective component yield is high, be applied to the aspects such as the bioactive ingredients extraction of extraction, Chinese medicine and the native compound of environmental protection aspect organic pollution.
Summary of the invention
Technical problem to be solved by this invention is to overcome the shortcoming that existing Rhizoma Acori Gramineii extract method extraction time is long, solvent consumption is large, extraction efficiency is low, and a kind of method of microwave extraction Rhizoma Acori Graminei volatile oil is provided.
In order to solve the problems of the technologies described above, the present invention adopts following technical scheme:
The method of microwave extraction Rhizoma Acori Graminei volatile oil of the present invention: get Rhizoma Acori Graminei medical material, add 8～10 times of weight distilled water immersion 3～6 hours, be placed in Microwave Extraction Apparatus, extract 80～120min under the power of 600～800W, obtain Rhizoma Acori Graminei volatile oil.
Preferably, said extracted method is: get Rhizoma Acori Graminei medical material, add 9 times of weight distilled water immersion 4 hours, be placed in Microwave Extraction Apparatus, under the power of 700W, extract 90min, obtain Rhizoma Acori Graminei volatile oil.
Technique scheme is that inventor passes through strict experiment screening out:
1, instrument and reagent
1.1 instrument
Instrument: Agilent6890-5973N gas chromatograph-mass spectrometer (An Jielun company of the U.S.); Synthesize/abstraction instrument (the auspicious swan science and technology in Beijing) of microwave catalysis; Rotary Evaporators RE-2000 (Shanghai Yarong Biochemical Instrument Plant); Sartorius 1,/10 ten thousand electronic analytical balance (Sai Duolisi instrument company of Switzerland); CQX25-06 ultrasonic cleaner (Shanghai High Kudos Science Instrument Co., Ltd.); Volatile oil extractor (making according to state-promulgated pharmacopoeia regulation).
1.2 reagent
Rhizoma Acori Graminei dry rhizome (build civilian associate professor of pharmacy through Zunyi Medical College poplar and be accredited as Rhizoma Acori Graminei dry rhizome); Ether (Kingsoft, analytical pure Chengdu chemical reagent company limited); Anhydrous sodium sulfate (Kingsoft, Chengdu chemical reagent company limited).
2, method and step
2.1 essential oil extraction method
2.1.1 water vapour distillation
Get the dry rhizome of 100g Rhizoma Acori Graminei, smash and put into beaker, add the water of 9 times of amounts, after immersion 4h, the mixture of medical material and distilled water is proceeded in 500ml round-bottomed flask, start to extract volatile oil.With reference to annex XD determination of volatile oil Division A League Matches of French Football method of " Chinese Pharmacopoeia " version in 2010, Rhizoma Acori Graminei rhizome is carried out to volatile oil and carry out the extraction of steam distillation.Keep the oil mass that water boils to extractor no longer to increase.The volatile oil obtaining is reclaimed to ether, the washing of NaCl saturated solution and with proceeding to after anhydrous sodium sulfate drying in reagent bottle through extracted with diethyl ether, Rotary Evaporators, to be measured.
2.1.2 microwave extracting extracts
Get 50g medical material, add distilled water that medical material is soaked to 4h.After assembling microwave extracter and setting each condition (heating-up temperature, heat time heating time, heating power) of Microwave Extraction Apparatus, carry out microwave extracting.After having extracted, thing to be extracted goes in reagent bottle after being chilled to room temperature, to be measured.
2.2 microwave extracting single factor experiments
Press given condition, investigate respectively amount of water (A), extraction time (B), 3 kinds of single factor experiments of microwave power (C), draw factor level and Rhizoma Acori Graminei volatile oil yield relation.Raw material all needs pre-soaking a period of time before microwave extracting, makes distilled water fully soak into the dry rhizome of Rhizoma Acori Graminei, in order to absorb microwave radiation.
What 2.2.1 amount of water extracted Rhizoma Acori Graminei volatile oil affects raw material 50g, microwave power 700W, extraction time 60min.Select the multiple that adds water (times of weight) of 5 kinds: 7 times, 8 times, 9 times, 10 times, 11 times, determine the amount of water of optimum extraction.
2.2.2 extraction time on extraction ratio affect raw material 50g, amount of water 9 times of weight, microwave power 700W, select the microwave irradiation time of 5 kinds of gradients: 30min, 60min, 90min, 120min, 150min, determine the optimum extraction time.
What 2.2.3 microwave power extracted Rhizoma Acori Graminei volatile oil affects raw material 50g, amount of water 9 times of weight, extraction time 60min, and the microwave power of 5 kinds of gradients of selection: 300W, 400W, 500W, 600W, 700W, determine optimum extraction microwave power.
2.3 orthogonal test
As index, use L taking asaricin content in gained extract
9(3
3) orthogonal table carries out orthogonal test, according to single factor experiment above, and the impact of each factor gradient level on Rhizoma Acori Graminei volatile oil extraction ratio.Adopt orthonormal design of experiments to be optimized extraction process, utilize L
9(3
3) orthogonal table carries out orthogonal test, investigates the impact that amount of water (A), extraction time (B), microwave power (C) extract Rhizoma Acori Graminei volatile oil, each factor level is in table 1.
Table 1 factor level table (Three factors-levels)
2.4 GC-MS analyze
2.4.1 chromatographic condition: (0.25 μ m) for 30m, 0.25mm for HP-5MS chromatographic column; Temperature programming: 40 DEG C keep 5min, rise to 60 DEG C with 5 DEG C/min, then rises to 230 DEG C with 3 DEG C/min and keeps 3min; 260 DEG C of temperature of vaporization chamber; Carrier gas: high-purity He, flow velocity 1ml/min; Sample size 1 μ L; Split ratio 20:1.
2.4.2 mass spectrum condition: 230 DEG C of interface temperature; Quadrupole rod temperature 150%, ionization mode: EI, electron energy 70eV; Solvent delay 4min; Mass scanning scope m/z30-500.
3, result
3.1 steam methods extract volatile oil
Amount of water is 9 times of amount distilled water, and extraction time is 6h, and soak time is 4h.
3.2 impacts of single factor on Rhizoma Acori Graminei volatile oil extracted amount
3.2.1 the impact of amount of water on Rhizoma Acori Graminei volatile oil extracted amount
Raw material 50g, extraction time 60min, microwave power 700W, the amount of water of 5 kinds of gradients of selection: 7 times, 8 times, 9 times, 10 times, 11 times, determine best amount of water, result is as shown in Figure 1.
3.2.2 the impact of extraction time on Rhizoma Acori Graminei volatile oil extracted amount
Raw material 50g, amount of water 9 times of weight, microwave power 700W, the microwave irradiation time of 5 kinds of gradients of selection: 30min, 60min, 90min, 120min, 150min, determine the optimum extraction time, result is as shown in Figure 2.
3.2.3 the impact of microwave power on Rhizoma Acori Graminei volatile oil extracted amount
Raw material 50g, amount of water 9 times of weight, extraction time 60min, the microwave power of 5 kinds of gradients of selection: 300W, 400W, 500W, 600W, 700W, determine optimum extraction microwave power, result is as shown in Figure 3.
When research shows that microwave power is between 300W～700W, extraction ratio and power are varied to positive correlation; Extraction rate reached peak value in the time that amount of water is 9 times of weight; In the time that extraction time is 120min, extraction ratio is significantly increased.Therefore, finally determine that selecting amount of water is 8 times, 9 times, 10 times, extraction time 60min, 90min, 120min, microwave power 300W, 500W, 700W, Three factors-levels carries out orthogonal test.
3.3 Orthogonal experiment results
3.3.1 Orthogonal experiment results is in table 2, and variance analysis is in table 3.
Table 2 orthogonal design table (Three factors-levels)
| Tested number | Amount of water (A) | Extraction time (B) | Microwave power (C) | Blank (D) | The area percentage of asaricin (%) in volatile oil |
| 1 | 1 | 1 | 1 | 1 | 29.800 |
| 2 | 1 | 2 | 2 | 2 | 31.394 |
| 3 | 1 | 3 | 3 | 3 | 32.812 |
| 4 | 2 | 1 | 2 | 3 | 24.995 |
| 5 | 2 | 2 | 3 | 1 | 29.109 |
| 6 | 2 | 3 | 1 | 2 | 32.312 |
| 7 | 3 | 1 | 3 | 2 | 32.236 |
| 8 | 3 | 2 | 1 | 3 | 31.429 |
| 9 | 3 | 3 | 2 | 1 | 22.989 |
| Average 1(K1) | 31.335 | 29.010 | 31.180 | 27.299 | ? |
| Average 2(K2) | 28.805 | 30.644 | 26.459 | 31.981 | ? |
| Average 3(K3) | 28.885 | 29.371 | 31.386 | 29.745 | ? |
| Extreme difference (R) | 2.530 | 1.634 | 4.927 | 4.682 | ? |
Table 3 orthogonal test analysis of variance table
| Source of error | Sum of square of deviations | Degree of freedom | F ratio | F marginal value | P significance |
| C microwave power | 46.599 | 2.00 | 10.545 | 19.000 | P is greater than 0.05 |
| A amount of water | 12.413 ? | 2.00 | 2.809 | 19.000 | P is greater than 0.05 |
| B extraction time | 4.419 | 2.00 | 1.000 | 19.000 | P is greater than 0.05 |
| D blank | 32.895 | 2.00 | 7.444 | 19.000 | P is greater than 0.05 |
| Error | 4.42 | 2.00 | ? | ? | ? |
Orthogonal test is carried out to intuitive analysis and variance analysis, and analysis result is respectively in table 2, table 3.By intuitive analysis result, extreme difference R
c> R
a> R
b; By the results of analysis of variance, F
c> F
a> F
b, factor A has compared with significant difference.Intuitive analysis is consistent with the result of variance analysis, on the impact order of extracting result be: C > A > B, be microwave power (W) having the greatest impact to Rhizoma Acori Graminei volatile oil extraction, amount of water takes second place, extraction time (min) affect minimum.Be combined as C by the area percentage of asaricin in volatile oil under each factor level in table 3 and the optimal level of the known each factor of K value size
3a
1b
2, optimum extraction condition is that microwave power is 700W, and extraction time is 90min, and amount of water is 8 times of water.
Rapidity, responsiveness and the feature of environmental protection of using microwave-assisted are also fully reflected in test, are also mathematical.
4, discuss
4.1 single factor experiment discussion
4.1.1 amount of water on Rhizoma Acori Graminei volatile oil extracted amount affect amount of water between 7 to 9 times of weight, extraction ratio increases with solvent load.For ensureing extraction ratio, therefore select 8 times, 9 times, 10 times these three gradient levels to investigate scope as orthogonal experiment.
4.1.2 microwave power on the impact of Rhizoma Acori Graminei volatile oil extracted amount in the time that extraction time is fixing, extraction temperature raises along with the increase of microwave power, cell wall cleavage rate increases, in cell, absorb the easy stripping of polar molecule of microwave energy, but excess Temperature can cause heat labile composition gelatinizing, thereby cause the reduction of productive rate.Investigate scope for (700W, 800W, 900W) these three gradient levels as orthogonal experiment therefore select microwave power.
4.1.3 volatile oil extraction ratio increases with the prolongation of extraction time on the impact of Rhizoma Acori Graminei volatile oil extracted amount between 30min-120min extraction time, and after 120min, extraction yield declines with the increase of extraction time.
4.2 orthogonal test discussion
The analysis being shown by orthogonal experiments table, can obtain having the greatest impact that microwave power (W) extracts Rhizoma Acori Graminei volatile oil, and amount of water takes second place, extraction time (min) affect minimum.Be combined as C by the area percentage of asaricin in volatile oil under each factor level in table 3 and the optimal level of the known each factor of K value size
3a
1b
2, optimum extraction condition is that microwave power is 700W, and extraction time is 90min, and amount of water is 8 times of water.
The discussion of 4.3 steam distillations and microwave auxiliary extraction
Can find out that from table 5, table 6 using microwave-assisted extracts Rhizoma Acori Graminei volatile oil better than traditional steam distillation extraction Rhizoma Acori Graminei volatile oil, and microwave auxiliary extraction has plurality of advantages, its maximum feature is exactly that rate of extraction is fast, save time, the factor considerations such as comprehensive extraction ratio, solvent load, equipment requirements, Microwave Assisted Extraction Technique has compared with traditional extraction technology the obvious advantage that extraction efficiency is high.But because its action principle affects the scope of its application, microwave is adapted to the material of Heat stability is good conventionally, microwave auxiliary extraction is also subject to many impacts because of rope, as raw material sources, the each type of solvent and the power of microwave action, microwave action time, the treating capacity of raw material and consumption and ratio etc. of solvent of processing.With mathematical statistics analysis and research, influence factor is a kind of scientific method.
4.4 GC-MS discuss
The main component of Rhizoma Acori Graminei is volatile oil, and in volatile oil, main component is asaricin.In addition in Rhizoma Acori Graminei volatile oil, still contain aminoacid, organic acid and saccharide.Relevant Rhizoma Acori Graminei volatile oil composition systematic study report is few, in order to determine that the material extracting is Rhizoma Acori Graminei volatile oil, so extract has been carried out to GC-MS analysis.From Rhizoma Acori Graminei volatile oil, isolated Characteristic chromatographic peak, by computer checking, has been identified wherein multiple compositions altogether, learn and wherein contain asaricin, and asaricin content is maximum.
5, conclusion
Asaricin is topmost effective ingredient in Rhizoma Acori Graminei volatile oil, has effect of removing dampness appetizing, the eliminating phlegm of having one's ideas straightened out, refreshment Fructus Alpiniae Oxyphyllae.Generally believe that Rhizoma Acori Graminei volatile oil has dual regulation to nervus centralis, both tranquillizing and allaying excitement (calm, convulsion), again consciousness-restoring and orifice-opening (excited, antidepressant).Microwave extracting is the new technique that a kind of latest development of utilizing microwave to improve extraction yield is got up.Microwave heating belongs to inner heating process, effective ingredient in energy enrichment medical material after microwave radiation.Have the advantages that selectivity is high, the operating time is short, solvent consumption is few, effective component yield is high.The present invention extracts the optimum process condition of Rhizoma Acori Graminei volatile oil with the preferred microwave-assisted of orthogonal experiment method, fast by the speed of microwave auxiliary extraction extract drugs as seen, saves time, and the effective percentage of extraction is high.Find for science the medium-height grass essential oil extraction method of optimizing experiment and theoretical foundation are provided.
Compared with prior art, the experiment of the present invention by scientific and precise the is preferred optimum process condition of microwave extraction Rhizoma Acori Graminei volatile oil, the maximum feature of gained technical scheme be rate of extraction fast, save time, and its solvent consumption is few, effective component yield is high, the factor of synthesise various, technical scheme of the present invention, according to having the remarkable advantage that extraction efficiency is high, has good popularizing application prospect.
Brief description of the drawings
Fig. 1 is the impact of amount of water on Rhizoma Acori Graminei volatile oil extracted amount;
Fig. 2 is the impact of extraction time on Rhizoma Acori Graminei volatile oil extracted amount;
Fig. 3 is the impact of microwave power on Rhizoma Acori Graminei volatile oil extracted amount.
Detailed description of the invention
Embodiment 1: getting Rhizoma Acori Graminei medical material, add 9 times of weight distilled water immersion 4 hours, be placed in Microwave Extraction Apparatus, is 700W by the power setting of Microwave Extraction Apparatus, extracts 90min, obtains Rhizoma Acori Graminei volatile oil.
Embodiment 2: getting Rhizoma Acori Graminei medical material, add 8 times of weight distilled water immersion 6 hours, be placed in Microwave Extraction Apparatus, is 800W by the power setting of Microwave Extraction Apparatus, extracts 80min, obtains Rhizoma Acori Graminei volatile oil.
Embodiment 3: getting Rhizoma Acori Graminei medical material, add 10 times of weight distilled water immersion 5 hours, be placed in Microwave Extraction Apparatus, is 600W by the power setting of Microwave Extraction Apparatus, extracts 120min, obtains Rhizoma Acori Graminei volatile oil.
90min, obtains Rhizoma Acori Graminei volatile oil.
Claims (1)
1. a method for microwave extraction Rhizoma Acori Graminei volatile oil, is characterized in that: get Rhizoma Acori Graminei medical material, add 9 times of weight distilled water immersion 4 hours, be placed in Microwave Extraction Apparatus, under the power of 700W, extract 90min, obtain Rhizoma Acori Graminei volatile oil.
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Citations (2)
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| CN101085129A (en) * | 2007-07-11 | 2007-12-12 | 石任兵 | Acorus gramineus total phenylpropanoid extraction and total phenols extraction and method for preparing simultaneously |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101085129A (en) * | 2007-07-11 | 2007-12-12 | 石任兵 | Acorus gramineus total phenylpropanoid extraction and total phenols extraction and method for preparing simultaneously |
| CN102391387A (en) * | 2011-11-07 | 2012-03-28 | 沈阳科思高科技有限公司 | Microwave chemical extraction method of active polysaccharide in higher plants or edible and medicinal fungi |
Non-Patent Citations (4)
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| 微波萃取技术在中药及天然产物提取中的应用;王明芝等;《人参研究》;20090630(第02期);29-33 * |
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