CN102836569A - Artemisia sacrorum ledeb volatile oil extraction process - Google Patents
Artemisia sacrorum ledeb volatile oil extraction process Download PDFInfo
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- CN102836569A CN102836569A CN2012102991315A CN201210299131A CN102836569A CN 102836569 A CN102836569 A CN 102836569A CN 2012102991315 A CN2012102991315 A CN 2012102991315A CN 201210299131 A CN201210299131 A CN 201210299131A CN 102836569 A CN102836569 A CN 102836569A
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Abstract
The invention discloses an artemisia sacrorum ledeb volatile oil extraction process. The process comprises the following steps: (1) weighting 25g of rtemisia sacrorum ledeb with particle size of 80 micrometers and placing the rtemisia sacrorum ledeb in a 500-milliliter triangular flask, adding 250 milliliters of distilled water according to a material-liquid ratio of 1: 10 (g/mL), and soaking for 1 hour, (2) carrying out batch-type ultrasound extraction at a temperature between 21 degrees to 29 degrees for 40 minutes of ultrasound time and under 400 watts of ultrasonic power, (3) filtering and moving residue, compressing filtered liquid at the temperature of 50 degrees, adding 10 milliliters of resteamed diethyl ether and extracting for three times, mixing the extraction liquid, decompressing and recycling the diethyl ether, drying through nitrogen and weighting. The process takes extraction rate of artemisia sacrorum ledeb volatile oil extract as an evaluation index, optimizes the process of volatile oil extraction assisted by ultrasound wave by means of single factor tests and orthogonal tests, and aims to select best extraction process conditions of the artemisia sacrorum ledeb volatile oil and provides certain scientific foundations for further expanded production.
Description
Technical field
The present invention relates to a kind of volatile oil extraction process, specifically, relate to a kind of Herba Artemisiae volatile oil extraction process.
Background technology
Volatile oil is one type of important secondary metabolite in the plant, has significant biologically active, and value all has a wide range of applications in fields such as medicine, food, daily use chemicals.Therefore yet volatile oil is considerably less and easy loss at the plant intensive amount, and in order at utmost to obtain target substance, it is of crucial importance to seek suitable extraction process technology.At present, the extractive technique of relevant Herba Artemisiae volatile oil mainly is a steam distillation, but that this method exists extraction time is long; Consumes energy; Therefore shortcomings such as productive rate is low select a kind of Perfected process that extracts Herba Artemisiae volatile oil simply, fast and efficiently, have crucial meaning.
Supercritical ultrasonics technology is as a novel extractive technique, mainly utilizes hyperacoustic cavitation effect to strengthen the effect of mass transmitting of extractant, impels solvent to penetrate in the plant tissue, thereby reaches efficiently, extraction effect fast.Although ultrasonic wave extraction application aspect the volatile oil extraction in plant at present is less, should technology be proved in the superiority aspect the extraction bioactivator.
Summary of the invention
In order to solve the problems of the technologies described above; The present invention provides a kind of Herba Artemisiae volatile oil extraction process; Extracting yield with Herba Artemisiae volatile oil medicinal extract is evaluation index; Be optimized through single factor experiment and Orthogonal Experiment and Design technology, be intended to filter out the optimum extraction process condition of Herba Artemisiae volatile oil, certain scientific basis is provided for further enlarging to produce to ultrasonic-assisted extraction volatile oil.
Concrete technical scheme is:
A kind of Herba Artemisiae volatile oil extraction process may further comprise the steps:
1) take by weighing 25.00g, granularity 80 purpose Herba Artemisiae samples are in the 500mL triangular flask, and 1: 10 (g/mL) adds 250mL distilled water to press solid-liquid ratio, soaks 1h;
2) under ultrasonic power 400W, ultrasonic time 40min, carry out the batch (-type) ultrasonic Extraction at 21～29 ℃;
3) remove by filter residue, decompression is concentrated down at 50 ℃ for filtrating, and adding 10mL heavily steams extracted with diethyl ether 3 times, combining extraction liquid, and the recovered under reduced pressure ether is weighed after nitrogen dries up.
Beneficial effect of the present invention: the present invention is optimized through single factor experiment and the Orthogonal Experiment and Design ultrasonic extracting process parameter to volatile oil in the Herba Artemisiae; The result shows; The optimum process condition of ultrasonic-assisted extraction volatile oil is: solid-liquid ratio 1: 10 (g/mL), ultrasonic power 400W, ultrasonic time 40min; Granularity 80 orders, volatile oil medicinal extract maximum extracted yield is 1.5440%.Simultaneously, test further illustrates supercritical ultrasonics technology and has advantage such as save time, efficient is high, operation is simple and easy, applicable to the extraction of volatile oil.
Description of drawings
Fig. 1 is degree of grinding is extracted yield to volatile oil impact effect figure;
Fig. 2 is ultrasonic time extracts yield to volatile oil to degree of grinding impact effect figure;
Fig. 3 is ultrasonic power extracts yield to volatile oil impact effect figure;
Fig. 4 is solid-liquid ratio extracts yield to volatile oil impact effect figure.
The specific embodiment
Below in conjunction with the accompanying drawing and the specific embodiment method of the present invention is done explanation in further detail.
Test material
Raw material is handled
Herba Artemisiae picks up from the Ansai County, Shaanxi Province in late July, 2010, and crossing the aperture respectively after its aerial part dries in the shade, pulverizes is 10,18,40,65,80,100 mesh sieves, gets the material in different apertures, is stored in cool place, dry place after the sealing, and is subsequent use.
Reagent
It is pure for analyzing heavily to steam ether; Nitrogen.
Key instrument and equipment
KQ-500DE type supersonic wave cleaning machine (Kunshan Ultrasonic Instruments Co., Ltd.); RE-52AA type Rotary Evaporators (Shanghai Yarong Biochemical Instrument Plant); Standard test sieve (Shangyu, Zhejiang city gold ancient cooking vessel standard screen tool factory); LX-300 water bath with thermostatic control circulation (Beijing long stream scientific instrument company); One of ALC-1100.2 percentage electronic balance (Beijing Sai Duolisi instrument system Co., Ltd);
Nitrogen evaporator (the handsome grace science and technology limited Company in Beijing).
Test method
The extraction of volatile oil
The Herba Artemisiae sample that takes by weighing the 25.00g certain particle size in the 500mL triangular flask, by different feed liquid than adding an amount of distilled water, soak 1h after, at certain power, under the time, carry out the batch (-type) ultrasonic Extraction in 21～29 ℃.Remove by filter residue after ultrasonic, decompression is concentrated down at 50 ℃ for filtrating, and adding 10mL heavily steams extracted with diethyl ether 3 times, combining extraction liquid, and the recovered under reduced pressure ether is weighed after nitrogen dries up, and calculates volatile oil medicinal extract and extracts yield.
The optimization of ultrasonic-assisted extraction volatile oil technology
It is evaluation index that the present invention extracts yield with Herba Artemisiae volatile oil medicinal extract; Selected ultrasonic power (200,250,300,350,400,450W), ultrasonic time (0,20,40,60,80,100min), granularity (10,18,40,65,80,100 order), 4 factors of solid-liquid ratio (1: 7,1: 8,1: 10,1: 12,1: 14,1: 16 (g/mL)) are investigated the influence that Herba Artemisiae volatile oil extracts; Based on this, adopt L
9(3
4) Orthogonal Experiment and Design is optimized, experimental factor and level are seen table 1.
Table 1 orthogonal test factor level table
Result and analysis
Single factor experiment
Set solid-liquid ratio 1: 8, ultrasonic Treatment 40min, ultrasonic power 300W investigates different grain size extracts yield to volatile oil medicinal extract influence.Can know that by Fig. 1 along with reducing of sample granularity, volatile oil extracts yield and is tangible ascendant trend.In the leaching process, along with the reduction of material granule granularity, directly being exposed to the cell quantity that extracts solvent increases, and increases with the contact area of extracting solvent, helps the leaching of active ingredient.But the material granule particle diameter is more little, and the rate of filtration then can be slow more, will cause extraction efficiency to reduce, even cause than lossy; Simultaneously, the sample fragmentation is thin more, and is consuming time long more, is prone to cause that pulverizer self temperature raises, and volatile oil is scattered and disappeared.Comprehensive above the analysis selected the factor level of 40,65,80 purpose sample granularities as follow-up orthogonal test.
Embodiment 2 ultrasonic treatment times are to extracting the influence of yield
Set solid-liquid ratio 1: 8, sample granularity 40 orders, ultrasonic power 300W investigates (0～100min) influence to volatile oil medicinal extract extraction yield of different extraction times.As shown in Figure 2, in 0～60min,, the prolongation volatile oil of ultrasonic time presents tangible ascendant trend along with extracting yield; After the processing time surpassed 60min, the extraction yield was along with the prolongation of time then begins to descend.In general, ultrasonic treatment time is long more, to obtain extract output high more.This is because of the prolongation along with the time, and the amount that impurity gets into the extraction solvent in the cell increases resistance to mass tranfer also with corresponding increase, has hindered the stripping of active ingredient, so the extraction yield is reduced; In addition, extraction time is long may to make the loss of part volatile ingredient, and the structural instability composition decomposes, thereby makes that extracting yield reduces.Therefore, select ultrasonic time 40,60,80min factor level as orthogonal test.
Embodiment 3 ultrasonic powers are to extracting the influence of yield
Set solid-liquid ratio 1: 8, granularity 40 orders, sonicated 40min investigates different ultrasonic power (200～450W) influences to volatile oil medicinal extract extraction yield.As shown in Figure 3, along with the increase of power, volatile oil extracts yield and is the trend that raises and afterwards reduce earlier, peaks during 350W.Ultrasonic wave has strong fragmentation to plant cell, when low-power, along with the increase of power; Cavitation strengthens, and cavitation bubble is acutely broken, and the plant cell degree of breaking increases; The release of intracellular organic matter, diffusion and dissolving are strengthened, and help the stripping of active ingredient; In addition, hyperacoustic mechanical agitation also can be along with power improves and increases, and this has promoted the contact between solvent and the material to a certain extent.When power constantly increases; The fragmentation of ultrasonic wave pair cell continues to strengthen, but impurity also can be accompanied by increase, and this will hinder the dissolving of active ingredient; Therefore should select suitable ultrasonic power in the test, excessive or too small and cause the decline of extracting yield to avoid extracting power.Simultaneously, ultrasonic wave also has certain fuel factor, and the power increase can cause that temperature raises, and then causes volatile ingredient to scatter and disappear or degraded.Take all factors into consideration, select ultrasonic power 300,350,400W factor level as Orthogonal Experiment and Design.
Embodiment 4 solid-liquid ratios are to extracting the influence of yield
Set granularity 40 orders, extraction time 40min, ultrasonic power 300W investigates different feed liquid is extracted yield to volatile oil medicinal extract than (1: 7～1: 16) influence.Can know by Fig. 4, in trial stretch, extract yield and raise earlier along with solvent load increases and afterwards reduce, the highest during solid-liquid ratio 1: 14 (g/mL).Generally speaking, solid-liquid ratio is big more, and the inside and outside concentration difference of cell is big more, the easy more stripping of object.If solid-liquid ratio is excessive, solvent will increase the absorption of ultrasonic energy, reduce cavitation effect, cushion effect of mass transmitting, weaken the fragmentation of pair cell wall, be unfavorable for that extract discharges from cell, thereby cause recovery rate to reduce.On the contrary, when solvent was very few, vegetable material was too close, also can cushion the mass transfer of ultrasonic energy, caused extracting not exclusively, and it is on the low side to extract yield.In the process of the test, when solid-liquid ratio is lower than 1: 6 when (g/mL), solution is thickness too, is difficult to extract; When solvent load is excessive, filtration difficulty, the energy consumption when increase concentrating and can cause the waste of solvent.Therefore, with operation, improve extraction efficiency for just, the present invention is set at 1: 10 with solid-liquid ratio (g/mL).
Orthogonal experiments and analysis
Table 2 orthogonal test knot
Table 3 Orthogonal Experiment and Design analysis of variance table
Annotate: F
0.05(2,2)=19.00, * appreciable impact (p＜0.05)
Orthogonal experiments shows (table 2), and each factor to the primary and secondary that Herba Artemisiae volatile oil medicinal extract extracts the yield influence is in proper order: sample granularity＞ultrasonic time＞ultrasonic power.Further The results of analysis of variance (table 3) shows: granularity is extracted yield influence significantly (p＜0.05) to volatile oil medicinal extract, and ultrasonic power and time then do not have the conspicuousness influence.Herba Artemisiae volatile oil optimum extraction condition is ultrasonic power 400W, ultrasonic treatment time 40min, granularity 80 orders.
Confirmatory experiment
For the further reliability of checking orthogonal experiments, by above optimum process condition, i.e. solid-liquid ratio 1: 10 (g/mL), ultrasonic power 400W, ultrasonic treatment time 40min, granularity 80 orders carry out volatile oil and extract, test repetition 3 times.The result shows that it is 1.5440% that Herba Artemisiae volatile oil medicinal extract extracts yield mean value, and the result is close with optimization of orthogonal test.
The present invention utilizes the ultrasonic wave auxiliary law that the volatile compound in the Herba Artemisiae has been carried out preliminary extraction, and has investigated solid-liquid ratio, sample granularity, ultrasonic time and ultrasonic power four factors are extracted yield to Herba Artemisiae volatile oil medicinal extract influence.Except that these four factors; Temperature also is the key factor that influences Extraction by Ultrasound volatile oil; Because the too high meeting of temperature causes thermally labile composition degraded or structural change, so the present invention is controlled at 21～29 ℃ with the ultrasonic wave temperature, reduces the influence of temperature to test as far as possible.Related invention shows; Compare with steam distillation method and microwave auxiliary water steam distillation extraction method; Ultrasonic-assisted extraction has reduced the degraded of thermally sensitive composition; Be highly suitable for the extraction of volatile ingredient, can be used as a kind of method of simply extracting volatile oil fast and be used for large-scale industrial production.
In addition; The present invention adopts Orthogonal Experiment and Design that the volatile oil extraction process is optimized ignoring under the interactive prerequisite; But in actual production process, the extraction of the interaction partners volatile oil between factor has influence significantly, so need careful consideration; Reduce unnecessary loss, in the hope of obtaining top gain with least cost as far as possible.
The above; Be merely the preferable specific embodiment of the present invention; Protection scope of the present invention is not limited thereto; Any technical staff who is familiar with the present technique field is in the technical scope that the present invention discloses, and the simple change of the technical scheme that obtains or equivalence replacement all fall in protection scope of the present invention with may be obvious that.
Claims (1)
1. a Herba Artemisiae volatile oil extraction process is characterized in that, may further comprise the steps:
1) take by weighing 25.00g, granularity 80 purpose Herba Artemisiae samples are in the 500mL triangular flask, and 1: 10 (g/mL) adds 250mL distilled water to press solid-liquid ratio, soaks 1h;
2) under ultrasonic power 400W, ultrasonic time 40min, carry out the batch (-type) ultrasonic Extraction at 21～29 ℃;
3) remove by filter residue, decompression is concentrated down at 50 ℃ for filtrating, and adding 10mL heavily steams extracted with diethyl ether 3 times, combining extraction liquid, and the recovered under reduced pressure ether is weighed after nitrogen dries up.
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Citations (4)
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| CN101205232A (en) * | 2006-12-19 | 2008-06-25 | 浙江大学宁波理工学院 | Technical new method for extracting artemisinin from sweet wormwood plants by ultrasonic assistance |
| CN101530674A (en) * | 2009-03-16 | 2009-09-16 | 王艺瑾 | Process for extracting active ingredients of traditional Chinese medicine in unit and combined type and device thereof |
| CN102134185A (en) * | 2011-01-19 | 2011-07-27 | 浙江大学宁波理工学院 | Method for extracting 3. 4 resacetophenone from Picea schrenkiana |
| WO2012103777A1 (en) * | 2011-02-01 | 2012-08-09 | 北京北大维信生物科技有限公司 | Compound isolated from monascus purpureus, preparation method therefor and uses thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101205232A (en) * | 2006-12-19 | 2008-06-25 | 浙江大学宁波理工学院 | Technical new method for extracting artemisinin from sweet wormwood plants by ultrasonic assistance |
| CN101530674A (en) * | 2009-03-16 | 2009-09-16 | 王艺瑾 | Process for extracting active ingredients of traditional Chinese medicine in unit and combined type and device thereof |
| CN102134185A (en) * | 2011-01-19 | 2011-07-27 | 浙江大学宁波理工学院 | Method for extracting 3. 4 resacetophenone from Picea schrenkiana |
| WO2012103777A1 (en) * | 2011-02-01 | 2012-08-09 | 北京北大维信生物科技有限公司 | Compound isolated from monascus purpureus, preparation method therefor and uses thereof |
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| 万水昌等: "超声提取技术在中药及天然产物提取中的应用", 《西北药学杂志》 * |
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| 王玉龙等: "小茴香挥发油超声波萃取工艺优化及数学模拟", 《广东化工》 * |
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