CN101248820A - Microwave auxiliary extraction method of silybum marianum seed oil - Google Patents
Microwave auxiliary extraction method of silybum marianum seed oil Download PDFInfo
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Abstract
The invention discloses a microwave-assisted method for extracting silybum mariamum seed oil, which includes the following steps: silybum mariamum seeds are mixed with organic extraction solvent and then are radiated with microwave, after removing residues by filtering and washing, filtrate and cleaning solution are combined, and organic solvent is removed, etc., wherein, the organic extraction solvent and the silybum mariamum seeds are mixed according to the weight ratio of 5:1-7:1; and the microwave power is 420-700 watt during microwave radiation. The used time of the method is only 1/150 of the soxhlet method while the extraction efficiency can be above 93% of the soxhlet method. The method with simple device is easy to control and can be completed by a domestic microwave oven. The method provides important basic data to the industrialization of extracting the silybum mariamum seed oil with the microwave to assist, and further lays the important foundation for the development of the silybum mariamum seed oil.
Description
Technical field
The present invention relates to the processing method of a vegetable oil, relate in particular to a kind of microwave auxiliary extraction method of silybum marianum seed oil, belong to food processing field.
Background technology
Milk thistle (Silybum marianum (Linn.) Gaertn) has another name called water and flies pheasant, and newborn thistle is a composite family Silybum herbaceous plant.Include multiple rich nutrient contents, dewatering flies outside the silibin, also contains the silybum marianum seed oil of 20-30% in the milk thistle fruit seed.Discover: contain (adding up 71%-80%) such as very high oleic acid, linoleic acid, leukotrienes in the silybum marianum seed oil, has health-care effect (He Weiming such as preventing and treating atherosclerotic, hypertension, coronary heart disease significantly, permitted tree peony. the nutritional labeling of milk thistle oil and the research of effect for reducing fat [J]. Journal of Nutrition, 1996,18 (2): 163-167).At present, industrial silybum marianum seed oil still uses traditional mechanical expression method to produce.Milling process, recovery rate is low, labour intensity is big, production efficiency is low, cost is high, and the needs (Song Baosheng of factory is given birth in more and more incompatible modernization, Bai Yunai, Li Jifen, Duan Yunying. milk thistle oil and reparation technology thereof [J]. Chinese oil, 1999,2 (24): 53-54).The research of existing supercritical extraction technique at present, (Xu Defeng, Zhang Weiming, history sturdy pines, Gu Gongping, Sun Dafeng. supercritical CO
2Extraction milk thistle oil technical study [J]. food machinery, 2007,23 (1): 93-96), but, also just be confined to the scope of the extraction and the laboratory research of micro substance owing to there are many-sided reasons such as cost height, equipment complexity, solvent range of choice be narrow in this method.
Microwave auxiliary extraction (Microwave-Assisted Extraction) is a kind of a kind of novel extractive technique that microwave and traditional solvent extraction method are combined and form, and range of application more and more widely.In recent years, microwave-assisted extraction technique more and more receives the concern of lot of domestic and foreign researcher, as adopt microwave technology to extract cardamom essential oil (Lucchesi Marie E, Lucchesi Marie E, SmadjaJacqueline, etal.Solvent free microwave extraction of Elletariacardamomum L.:A mult ivariate study of a new techni que for theextraction of essential oil.Journal of Food Engineering, 2007,79 (3): 1079-1086; Ziming Wang, Lu Wang, Tiechun Li.Rapid analysis of theessential oils from dried Illicium verum Hook.f.and Zingiberofficinale Rosc.By improved solvent-free microwave extraction withthree types of microwave-absorption medium.Analytical ﹠amp; BioanalyticalChemistry, 2006,386 (6), 1863-1868.), rose hip oil (Szentmih á lyi Kl á ra, Vinkler P é ter, Lakatos B é la, etal.Rose hip (Rosa canina L.) oilobtained from waste hip seeds by different extraction methods.Bioresource Technology, 2002,82 (2): 195-202.), walnut oil (Shao Hai, Li Lihua, Gong Xiaojie, Tian Yuxin, Chen Yuyan, Li Xiuping, Zhang Jinsheng
*. microwave abstracting walnut oil technology. Liaoming Petrochemical Univ's journal, 2005,25 (2), 13-16.), coix seed oil (Du Shaolong, Zhou Chunshan. the research of microwave assisted extraction coix seed oil. Chinese grain and oil journal, 2006,21 (4): 79-81), shaddock ped essential oil (GONG Sheng-zhao, CHENG Jiang, YANG Zhuo-ru.Microwave-assistedextraction of essential oil from citrus grandis peel.Chemistry andindustry of forest products, 2005,25 (4): existing report such as 67-70.), but have not yet to see the relevant report that adopts microwave technology extraction silybum marianum seed oil.
Summary of the invention
The present invention is a raw material with the milk thistle seed, with microwave auxiliary extraction method silybum marianum seed oil is extracted research, investigated of the influence of factors such as different extractants, microwave power, liquid-solid ratio, extraction time to the silybum marianum seed oil extraction efficiency, on the basis of single factor experiment, use Orthogonal Experiment and Design, each technological parameter is carried out further optimization, thereby finished the present invention.
Technical problem to be solved by this invention provides a kind of microwave auxiliary extraction method of silybum marianum seed oil.
Technical problem to be solved by this invention is achieved through the following technical solutions:
A kind of microwave auxiliary extraction method of silybum marianum seed oil, comprise that the organic extraction solvent is mixed the back carries out radiation with the milk thistle seed with microwave, filter and the washing filter residue, filtrate and cleaning solution are merged, steps such as organic solvent are removed in heating, wherein, with organic extraction solvent and milk thistle seed according to 5: 1-7: 1 part by weight mixes; The microwave power that is adopted when carrying out the microwave radiation is: 420-700 watt (W);
In order to reach better extraction efficiency, preferred, described microwave power is preferably 560W, and the part by weight of described organic extraction solvent and milk thistle seed is preferably 7: 1.Particularly preferred, described microwave irradiation time is 3-5 minute, more preferably 4 minutes.
Described organic extraction solvent can be the organic solvent of using always that is used to extract, and for example, can be n-hexane, cyclohexane, ethyl acetate or benzinum etc., is preferably benzinum.
Microwave power is one of main factor that influences extraction effect, because milk thistle seed cell membrane absorbs microwave energy, tissue element produces instantaneous polarization under the microwave electromagnetic field action, phase mutual friction, collision between vibration, fracture and the particle of generation key, sharply heated up in the inside of vascular bundle tissue, and can keep this temperature to surpass the ability that cell membrane expands until its internal pressure, cause cell wall rupture, the grease between parts of fine cell wall inside and the cell is released out.The inventor finds by single factor experiment, when microwave power during less than 560W, extraction efficiency is the rising state always, extraction efficiency reaches the highest when microwave power reaches 560W, but microwave power is greater than after the 560W, because the grease of cell membrane inside is extracted out substantially, so continue to increase microwave power, recovery rate influence to grease is little, reduces to some extent on the contrary.
Transmission and the absorption of microwave energy in the extraction system all needs extractant, also is a significant effects factor so liquid-solid phase is compared to Microwave Extraction.Result of the test shows, Gu when liquid/than 7 when following, because extractant is less, cause the osmotic pressure of extraction system too high, transmission and absorbing state to microwave energy are all not enough, and extractant also can bring the concentration height of extract less, make that the motive force of material Transfer is little in the system, so extraction effect is relatively poor.When liquid/Gu when equaling 7, it is higher that extraction efficiency has reached, and if continue to increase the liquid-solid phase ratio, the evidence recovery rate increases and is not obvious on the one hand, can increase solvent treating capacity and energy absorption on the other hand, is unfavorable for the separation and the purifying of grease.
Microwave action is when material, and the electromagnetic field that microwave produced quickens to be extracted composition to interfacial diffusion and warm-up movement, shortens extracted component by the time of material diffusion inside in the extractant, and along with the prolongation of Microwave Extraction time, the grease extraction effect can be good more.The inventor finds that by test the microwave irradiation extraction time extracts silybum marianum seed oil fully substantially in 4min.So 4min can obtain best extraction efficiency with the control of microwave irradiation extraction time.
The used time of microwave extraction method of the present invention is 1/150 of soxhlet extraction, and extraction efficiency can reach more than 93% of soxhlet extraction method.Microwave auxiliary extraction method of the present invention has solved traditional lixiviate operation and has not carried out clasmatosis, and the extraction resistance that cell membrane and cell membrane bring has embodied that firing rate is fast, efficient energy-saving.And experimental rig simple, be easy to control, just can finish with household microwave oven.The technological parameter that the inventive method obtained provides more important basic data for the industrialization of microwave auxiliary extraction silybum marianum seed oil, and then has also established important basis for the deep exploitation of silybum marianum seed oil.
Description of drawings
The influence that Fig. 1 microwave power extracts silybum marianum seed oil; Condition: microwave action time 4min, liquid-solid phase was than 5: 1.
The influence that Fig. 2 liquid-solid phase comparison silybum marianum seed oil extracts; Condition: microwave power 560w, microwave action time 4min.
The influence that Fig. 3 microwave treatment time extracts silybum marianum seed oil; Condition: microwave power 560W liquid-solidly is in a ratio of 7: 1.
The specific embodiment
Further describe the present invention below in conjunction with specific embodiment, advantage of the present invention and characteristics will be more clear along with description.But these embodiment only are exemplary, scope of the present invention are not constituted any restriction.It will be understood by those skilled in the art that and down can make amendment or replace without departing from the spirit and scope of the present invention, but these modifications and replacing all fall within the scope of protection of the present invention the details of technical solution of the present invention and form.
One, test material and equipment
1, milk thistle seed: the Jiayin County, Heilongjiang Province provides, and is standby through removal of impurities.
2, acetone, n-hexane, cyclohexane, benzinum (60-90 ℃) are and analyze pure (the huge chemical reagent of Tianjin Dongli District factory).
3, WD700 type LG micro-wave oven (Tianjin LG ELECTRONICS Electrical Appliances Co., Ltd), DK-98-II type electric-heated thermostatic water bath (Tianjin Tai Site Instr Ltd.), apparatus,Soxhlet's (Zhen Cheng Yongxing, Shandong instrument plant), DHG-9053A type air dry oven (the Shanghai permanent laboratory apparatus of benefit Co., Ltd), TD-50 vacuum freeze drier (PVG freeze drying equipment Co., Ltd).
Embodiment 1 monofactorial pilot study
1, microwave power is to the influence of silybum marianum seed oil extraction
In microwave assisted extraction process, microwave power is to influence one of topmost factor of extraction effect, and it is the variation of the extraction effect of 280W, 420W, 560W, 700W that microwave power has been investigated in this test, result such as Fig. 1.
Microwave abstracting is to utilize a kind of wavelength extremely short, the radiant energy material handling that frequency is very high, the Ji Songrong cell membrane absorbs microwave energy, tissue element produces instantaneous polarization under the microwave electromagnetic field action, and do the reversal campaign with 2.45 hundred million times/second speed, produce the vibration of key, phase mutual friction between fracture and the particle, collision, sharply heated up in the inside of vascular bundle tissue, and can keep this temperature to surpass the ability that cell membrane expands until its internal pressure, cause cell wall rupture, be arranged in intracellular material and flow out, can transmit at a lower temperature from cell, in the spe medium around being transferred to.During extraction, if microwave power is low excessively, then microwave oscillation can be less, is not enough to produce the broken wall effect, causes extraction yield lower.Microwave power is high more, and the extraction effect of grease is good more.This test rises to 560W when microwave power, and microwave energy makes milk thistle seed cell wall rupture, and the grease between parts of fine cell wall inside and the cell is released out, and this moment, recovery rate was the highest.But microwave power,, reduces so continuation increase microwave power is little to the recovery rate influence of grease because the grease of cell membrane inside is extracted out substantially on the contrary to some extent greater than after the 560W, should be that power is bigger, causes due to the extractant gasification minimizing.
2, the influence of liquid-solid phase comparison silybum marianum seed oil extraction
It also is a significant effects factor that liquid-solid phase is compared to Microwave Extraction, and this mainly is because transmission and the absorption of microwave energy in the extraction system all needs extractant.This experimental study the situation of change of liquid-solid ratio silybum marianum seed oil recovery rate between 4-8, see Fig. 2.
The result shows, Gu when liquid/than 7 when following, because extractant is less, cause the osmotic pressure of extraction system too high, transmission and absorbing state to microwave energy are all not enough, and extractant also can bring the concentration height of extract less, make that the motive force of material Transfer is little in the system, so extraction effect is relatively poor.When liquid/Gu when equaling 7, it is higher that extraction efficiency has reached, and if continue to increase the liquid-solid phase ratio, the evidence recovery rate increases and is not obvious on the one hand, can increase treating capacity and energy absorption on the other hand, is unfavorable for the separation and the purifying of grease.
3, microwave treatment time is to the influence of silybum marianum seed oil recovery rate
Microwave power 560W is selected in this test, liquid-solidly is in a ratio of 7: 1, and when having investigated microwave irradiation time and being 2-5min, the influence to the silybum marianum seed oil recovery rate the results are shown in Figure 3.
Microwave action is when material, the electromagnetic field that microwave produced quickens to be extracted composition to interfacial diffusion and warm-up movement, shortens extracted component by the time of material diffusion inside in the extractant, thereby extraction rate is improved greatly, can obtain bigger extraction quantity in the short period of time.The microwave abstracting silybum marianum seed oil is in 2min in this test, and extraction efficiency just sharply rises to more than 85%, and along with the prolongation of Microwave Extraction time, the grease extraction effect is good more.When 4min, substantially that oil extraction is complete, so when the Microwave Extraction time greater than 4min after, the variation of recovery rate tends towards stability.
One, test method
1 sample treatment with the vacuum drying of milk thistle seed after, pulverize the back with the multifunctional food agitator and cross 40 orders, stand-by.
2 cable-styled extraction methods accurately take by weighing above-mentioned milk thistle kind powder of seeds 10g, with benzinum backflow degreasing 10h, calculate the silybum marianum seed oil recovery rate in apparatus,Soxhlet's.
3 microwave abstracting methods accurately take by weighing above-mentioned kind of powder of seeds of 10g, put in the conical flask, and add certain amount of organic solvent.Conical flask is put into micro-wave oven, radiation certain hour (taking the batch (-type) radiation) in case bumping.Filter and wash filter residue then, filtrate and cleaning solution are moved in the conical flask, organic solvent is removed in the water-bath heating, and drying takes by weighing the silybum marianum seed oil quality again.Fat content is pressed the GB/T5512-1985 method and is measured.
The calculating of 4 extraction efficiencies
In the formula: η-extraction efficiency
α-microwave abstracting gained milk thistle oil quality
β-Soxhlet is extracted gained milk thistle oil quality
5 Orthogonal Experiment and Design schemes
Determined the scope of preferable microwave power, liquid-solid ratio and microwave irradiation time by single factor pilot study of embodiment 1.And on this basis, present embodiment carries out L to the principal element (microwave power, liquid-solid ratio, microwave irradiation time) that influences the silybum marianum seed oil extraction efficiency
9(3
4) Orthogonal Experiment and Design, its factor level sees Table 1
Table 1 factor level table
| Factor level | Power (W) A | Time (min) B | Liquid-solid ratio C |
| 1 | 420 | 3 | 5∶1 |
| 2 | 560 | 4 | 6∶1 |
| 3 | 700 | 5 | 7∶1 |
6 statistical analysis software SAS 8.0
Two, test results and analysis
The influence that 1 solvent extracts silybum marianum seed oil
The chemical composition of analysis silybum marianum seed oil as can be known, silybum marianum seed oil all is soluble in organic solvents such as hexane, benzinum, therefore microwave power 560W is selected in this test, processing time 4min, liquid-solid phase was than 7: 1, the following several organic solvents of research compare the extraction situation of silybum marianum seed oil, the results are shown in Table 2.
Table 2 different solvents is to the contrast of silybum marianum seed oil extraction efficiency
| Solvent | Extraction efficiency, % | Product appearance |
| N-hexane | 81.16 | Light yellow, transparent |
| Cyclohexane | 79.16 | Light yellow, little turbid |
| Benzinum | 79.13 | Light yellow, transparent |
| Ethyl acetate | 81.34 | Yellow, muddy |
As can be seen from Table 2, selected solvent is more approaching to the extraction efficiency of silybum marianum seed oil, but considers the product appearance quality, and cyclohexane and ethyl acetate gained silybum marianum seed oil occur muddy, can not select for use.Extraction effect is not only relevant with the absorption of microwave radiant energy, but also relevant with diffusion and the dissolubility of grease of solvent in particle.The solvent dielectric constant is big more, and is good more to the absorption of microwave radiant energy.From dielectric constant, benzinum is less, but benzinum is all bigger to the dissolubility of grease and the diffusion rate in particle.
| F | P-value | F crit |
| 0.08284 | 0.921192 | 4.256495 |
Influence not remarkable as can be known by variance analysis.So it is solvent that benzinum is selected in this test, research microwave auxiliary extraction silybum marianum seed oil carries out the contrast of identical extractant with soxhlet extraction benzinum oil extracting rate just.
2 L
9(3
4) Orthogonal Experiment and Design scheme and result
Table 3 orthogonal test scheme and result
| Tested number | Power (W) | Liquid-solid ratio | Time (min) | Extraction efficiency (%) |
| 1 | 1 | 1 | 1 | 53.36 |
| 2 | 1 | 2 | 2 | 68.56 |
| 3 | 1 | 3 | 3 | 72.08 |
| 4 | 2 | 1 | 3 | 80.93 |
| 5 | 2 | 2 | 1 | 82.18 |
| 6 | 2 | 3 | 2 | 93.11 |
| 7 | 3 | 1 | 2 | 77.27 |
| 8 | 3 | 2 | 3 | 81.18 |
| 9 | 3 | 3 | 1 | 85.19 |
| K 1 | 194 | 211.56 | 220.73 | |
| K 2 | 256.22 | 231.92 | 238.94 | |
| K 3 | 243.64 | 250.38 | 234.19 | |
| k1 | 64.67 | 70.52 | 73.58 | |
| k2 | 85.41 | 7731 | 79.65 | |
| k3 | 81.21 | 83.46 | 78.06 | |
| R i | 20.74 | 12.94 | 6.07 |
Because differential (R
i) big more, influence remarkable more.Analyze as can be known from table 3, each factor is A＞B＞C in proper order to the primary and secondary that influences of silybum marianum seed oil extraction efficiency, and optimal level is A
2B
3C
2, i.e. microwave power 560W liquid-solidly is in a ratio of 7: 1, and the extraction time is 4min.
Table 4 analysis of variance table
| Factor | The free degree | Quadratic sum | Average | The F value | Pr＞ |
| A | |||||
| 2 | 721.5238222 | 360.7619111 | 87.28 | 0.0113 | |
| |
2 | 251.3659556 | 125.6829778 | 30.41 | 0.0318 |
| |
2 | 59.4820222 | 29.7410111 | 7.20 | 0.1220 |
From variance analysis as can be known, microwave power, liquid-solid phase comparison extraction efficiency influence significantly, and the microwave irradiation time influence is not remarkable.
On the basis of single factor experiment, present embodiment has drawn the optimum process condition of microwave abstracting silybum marianum seed oil by Orthogonal Experiment and Design, that is: microwave power 560W, best liquid-solid ratio are that 7: 1, extraction time are 4min, the extraction efficiency of milk thistle is up to more than 93% of soxhlet extraction, and the time has shortened 95%.The primary and secondary of influence factor power (A), time (B), liquid-solid ratio (C) is A＞B＞C in proper order, and The results of analysis of variance A, B are that significant, C is inapparent.
Claims (7)
1, a kind of microwave auxiliary extraction method of silybum marianum seed oil, comprise the organic extraction solvent is mixed back microwave radiation with the milk thistle seed, filter and the washing filter residue, filtrate and cleaning solution are merged, step such as organic solvent is removed in heating, it is characterized in that: with organic extraction solvent and milk thistle seed according to 5: 1-7: 1 part by weight mixes; When carrying out the microwave radiation, the microwave power that is adopted is 420-700 watt.
2, according to the method for claim 1, it is characterized in that: described microwave power is 560W.
3, according to the method for claim 1, it is characterized in that: the organic extraction solvent is mixed with the part by weight according to 7: 1 of milk thistle seed.
4, according to any one described method of claim 1-3, it is characterized in that: described microwave irradiation time is 3-5 minute.
5, in accordance with the method for claim 4, it is characterized in that: described microwave irradiation time is 4 minutes.
6, according to the method for claim 1, it is characterized in that: described organic extraction solvent is selected from n-hexane, cyclohexane, ethyl acetate or benzinum.
7, according to the method for claim 6, it is characterized in that: described organic extraction solvent is a benzinum.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102260589A (en) * | 2011-06-24 | 2011-11-30 | 江苏江大源生态生物科技有限公司 | Method for preparing silybum marianum oil |
| CN102268328A (en) * | 2011-07-08 | 2011-12-07 | 中国热带农业科学院农产品加工研究所 | Method for extracting tea tree oil by microwave radiation |
| CN101988025B (en) * | 2009-08-03 | 2012-07-04 | 郑小非 | Method for extracting tea seed oil from tea seeds by microwave processing |
| CN104651037A (en) * | 2014-01-17 | 2015-05-27 | 吴长军 | Method for extracting oil and protein in silybum marianum kernels by subcritical fluid |
| CN106198143A (en) * | 2016-07-14 | 2016-12-07 | 云南省林业科学院 | A kind of rapid digestion method of vegetable oil material protein determination |
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2008
- 2008-03-26 CN CNA200810084143XA patent/CN101248820A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101988025B (en) * | 2009-08-03 | 2012-07-04 | 郑小非 | Method for extracting tea seed oil from tea seeds by microwave processing |
| CN102260589A (en) * | 2011-06-24 | 2011-11-30 | 江苏江大源生态生物科技有限公司 | Method for preparing silybum marianum oil |
| CN102268328A (en) * | 2011-07-08 | 2011-12-07 | 中国热带农业科学院农产品加工研究所 | Method for extracting tea tree oil by microwave radiation |
| CN104651037A (en) * | 2014-01-17 | 2015-05-27 | 吴长军 | Method for extracting oil and protein in silybum marianum kernels by subcritical fluid |
| CN106198143A (en) * | 2016-07-14 | 2016-12-07 | 云南省林业科学院 | A kind of rapid digestion method of vegetable oil material protein determination |
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