CN101205501A - Ultrasonic-assisted method for extracting flax-seed oil - Google Patents
Ultrasonic-assisted method for extracting flax-seed oil Download PDFInfo
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Abstract
The invention discloses a method for extracting linseed oil, in particular a method for extracting linseed oil assisted by ultrasonic. The invention takes linseeds as the raw material, the solvent is used to extract the linseed oil under the ultrasonic that the frequency is between 20 and 100 kHz and the strength is between 1 and 40W/cm<2>. With the method of the invention, the extraction rate of the linseed oil is between 70.74 and 99.36 percent, the extraction time is between 30 and 180 minutes, the dosage of the solvent is 4 to 20L per 1kg linseeds, the extraction temperature is between 20 and 60 DEG C. Compared with a pressing method, a solvent method and a supercritical carbon dioxide extraction method, the process provided by the invention has the characteristics of simple equipment, convenient operation, low cost, quick speed and high yield.
Description
Technical field
The invention belongs to effective ingredients in plant extraction process technology field, relate to a kind of method of ultrasonic-assisted extraction oleum lini.
Background technology
Flax (flax family (Linaceae) linum) is annual or per nnial herb, and one of the world ten big oil crops all have extensive plantation in NORTHWEST CHINA, North China and the Northeast.Linseed oil (flaxseed orlinseed) claim flaxseed again, is the seed of flax, and the oil that obtains from linseed oil is called as oleum lini.Unsaturated fatty acid content reaches more than 80% in the oleum lini, and linolenic acid content is 40%-60%, for the 5-100 of other vegetables oil doubly.Linolenic acid is a kind of omega-3 unsaturated fatty acid, and this kind unsaturated fatty acids the mankind itself can not synthesize, must from food or nutritious prod, obtain, thereby this class unsaturated fatty acids be otherwise known as " human indispensable fatty acid (EFA) ".After linolenic acid was absorbed by the body, the effect through enzyme in small intestine can be converted into docosahexenoic acid (DHA) and two kinds of unsaturated fatty acidss of timnodonic acid (EPA).DHA and EPA have important effect to keeping HUMAN HEALTH and improving function of human body.Discover that often edible oleum lini can effectively prevent and treat illnesss such as mammary cancer, colorectal carcinoma, prostatitis and arteriosclerosis, and can significantly reduce serum blood fat, inhibition tumor growth.Therefore, oleum lini is effectively extracted have huge economic and social benefit.
Current, the method for extracting oleum lini both at home and abroad mainly contains milling process, organic solvent method and small-scale supercritical carbon dioxide extraction method etc.The milling process productive rate is low, power consumption is big and the oily impurity of expressed is more.Organic solvent method is exactly that the linseed oil after pulverizing is mixed with suitable organic solvent, lixiviate certain hour after-filtration, and under vacuum condition, realize (the B.Dave Oomah et al. that concentrates of Recovery of Organic Solvent and oleum lini, Comparison of flaxseed meal lipids extracted with different solvent, LWT-Food Science and Technology, 1996,29 (7), 654-658).
Organic solvent method extracts to be needed very long extraction time usually and consumes a large amount of extraction solvents, and the use of simultaneously a large amount of organic solvents brings adverse influence can for human body and environment.The supercritical carbon dioxide extraction cost is higher, equipment is complicated and not easy to operate.The aqueous enzymatic method of mentioning among other relevant oleum lini extracting method such as the patent CN1935962A exists extraction yield lower equally, the problem that extraction time is long.
Carry out the history that effective ingredients in plant extracts two more than ten years with ultrasonic wave as supplementary means, it is used for the assisted extraction oleum lini but still find no the people so far.
Summary of the invention
The purpose of this invention is to provide a kind of method of extracting oleum lini, method provided by the present invention is to be raw material with the linseed oil, is that 20-100kHz and ultrasound intensity are 1-40W/cm in ultrasonic frequency
2The supersound process condition under adopt organic solvent method to extract, obtain oleum lini.
Above-mentioned supersound process condition can be preferably: ultrasonic frequency is 20-40kHz, and ultrasound intensity is 5-15W/cm
2
The organic solvent of existing extraction oleum lini all can adopt, as sherwood oil, normal hexane, Virahol and soybean extracting solvent no.6 etc.
The proportioning of above-mentioned linseed oil and above-mentioned organic solvent can be the 1kg linseed oil: the 4-20L organic solvent; The proportioning of above-mentioned linseed oil and above-mentioned organic solvent can be preferably the 1kg linseed oil: the 6-10L organic solvent.
The extraction temperature of above-mentioned supersound process can be 20-60 ℃, and extraction time can be 30-180 minute; The extraction temperature of above-mentioned supersound process can be preferably 25-45 ℃, and extraction time can be preferably 30-90 minute.
Above-mentioned linseed oil can roll and/or expanded and/or pulverization process before extracting.
Also can comprise purification step in the above-mentioned oleum lini extracting method.
The present invention is on the basis of existing organic solvent extraction method, creatively introduce ultrasonication technology, with the linseed oil is raw material, separate the back through mechanical treatment, the extraction of ultrasonic wave secondary solvent, solid-liquid separation, liquid liquid and obtain oleum lini, do not change unsaturated fatty acid content in the oleum lini basically.
Utilize method provided by the invention to carry out oleum lini and extract, have the following advantages:
A) compare with traditional organic solvent extraction method, under identical extraction yield, shortened extraction time effectively, shortened to present 30-180 minute by original 24-72 hour; Solvent-oil ratio reduces, and only is the 1/8-1/10 of traditional solvent; Do not need extra heating in the leaching process, saved the energy, reduced cost.
B) extraction yield height has reduced fat residue in the residue, has saved oil resource.
C) can under lower temperature, extract, can avoid the deterioration by oxidation of oleum lini effectively, improve the quality of oleum lini, prolong the period of storage of oleum lini.
D) technology is simple, and is easy to operate, is suitable for suitability for industrialized production, is convenient in the technical transformation of existing solvent method.
Adopt method of the present invention, the extraction yield of oleum lini is 70.74%-99.86%, extraction time to be that 30-180 minute, solvent-oil ratio are 4-20L solvent/1kg linseed oil, to extract temperature be 20-60 ℃.
Adopt the optimum condition of method of the present invention, the extraction yield of oleum lini is 86.63%-97.42%, extraction time to be that 30-90 minute, solvent-oil ratio are 6-10L solvent/1kg linseed oil, to extract temperature be 25-45 ℃.
Method provided by the present invention is compared with traditional milling process, solvent method and supercritical carbon dioxide extraction method, has the advantages that equipment is simple, easy to operate, cost is low, operation is fast, yield is high.
Following embodiment is convenient to understand better the present invention, but does not limit the present invention.
Description of drawings
Fig. 1 is the electron-microscope scanning image of linseed oil residue
Embodiment
The method of extraction oleum lini provided by the present invention can may further comprise the steps successively:
1) be that raw material carries out mechanical treatment to it with the linseed oil;
2) getting linseed oil behind the mechanical treatment, is 20-100kHz in frequency, and intensity is 1-40W/cm
2Ultrasonic wave under use the solvent extraction oleum lini;
3) separating solid residue and filtrate;
4) vaporize draw liquid obtains oleum lini.
The calculation formula of the productive rate of oleum lini and extraction yield is as follows in following examples:
W
iThe quality of-the oleum lini that extraction obtains from the 10g linseed oil;
W
0The quality of the used linseed oil of-single test (10g);
W
tThe quality of contained oleum lini in the-10g linseed oil (4.877 ± 0.06g), measure according to the Soxhlet extraction process among the GB/T5512-85.
Method therefor is ordinary method if no special instructions among the following embodiment.
The extraction of embodiment 1, oleum lini and analysis
Get 60g linseed oil (Zhangjiakou, Hebei province beneficial friend's fatty foods company limited), be divided into 6 parts at random, every part of 10g, wherein 3 parts are adopted ultrasonic wave secondary solvent method of the present invention to extract oleum lini respectively; Other 3 parts are adopted existing organic solvent extraction method to extract oleum lini respectively.Concrete extracting method and result are as follows:
1, ultrasonic wave secondary solvent method is extracted oleum lini
1) linseed oil is pulverized: get the 10g linseed oil and put into pulverizer and be crushed to particle diameter 0.25-1.20mm.
2) linseed oil after will pulverizing mixes with the 40ml normal hexane, at ultrasonic frequency 20kHz, and ultrasound intensity 1W/cm
2, extract under the condition of 20 ℃ of temperature, the ultrasonic assisted extraction of mixed solution 30 minutes.
3) filter the collection extracting solution.
4) extracting solution is placed rotatory evaporator in 50 ℃, be evaporated to pulpous state under 60 rev/mins, put into vacuum drier then and further remove solvent, the oil that obtains is oleum lini.
3 repetitions are established in experiment, obtain oleum lini 3.414g, 3.497g, 3.545g respectively.
The oleum lini extraction yield of 3 revision tests is respectively 70.00%, 71.70%, 72.69%.
The oleum lini productive rate of this leaching process is 34.85 ± 0.66, extraction yield is 71.46 ± 1.36, extraction time is that 30 minutes, solvent load are 40ml, and extracting temperature is 20 ℃.
2, the conventional organic solvents extraction method is extracted oleum lini
1) linseed oil is pulverized, with step 1 1).
2) linseed oil after will pulverizing mixes with the 40ml normal hexane, extracts under the condition of 20 ℃ of temperature, mixed liquid dipping is left standstill extracted 30 minutes.
3) filter to collect extracting solution, with step 1 3).
4) with step 1 4).
3 repetitions are established in experiment, obtain oleum lini 3.107g, 3.112g, 3.099g respectively.
The oleum lini extraction yield of 3 revision tests is respectively 63.71%, 63.81%, 63.54%.
The oleum lini productive rate of this leaching process is 31.06 ± 0.07, extraction yield is 63.69 ± 0.13, extraction time is that 30 minutes, solvent load are 40ml, and extracting temperature is 20 ℃.
3, the analysis of oleum lini
1) specific gravity test of oleum lini (GB 5526-85)
Carry out specific gravity test according to State Standard of the People's Republic of China GB 5526-85, experimental result shows that the oleum lini proportion that is extracted by ultrasonic wave secondary solvent method is 0.9349, the oleum lini proportion that is extracted by the conventional organic solvents extraction method is 0.9329, all drops between the oleum lini characteristic constant 0.9260-0.9365 that " State Standard of the People's Republic of China-linseed oil " mention in (GB8235-87).
2) refractive index of oleum lini is measured (GB 5527-85)
Carrying out refractive index according to State Standard of the People's Republic of China GB 5527-85 measures, test-results shows that the oleum lini refractive index that is extracted by ultrasonic wave secondary solvent method is 1.4802, the oleum lini refractive index that is extracted by the conventional organic solvents extraction method is 1.4801, all drops between the oleum lini characteristic constant 1.4785-1.4840 that mentions among " State Standard of the People's Republic of China-linseed oil " (GB 8235-87).
3) acid value of oleum lini is measured (GB 5530-85)
Carrying out acid value according to State Standard of the People's Republic of China GB 5530-85 measures, test-results shows that the oleum lini acid value of being extracted by ultrasonic wave secondary solvent method is 1.23mgKOH/g, the oleum lini acid value of being extracted by the conventional organic solvents extraction method is 1.09mgKOH/g, all less than the accurate 4.0mgKOH/g of (eating) linolenic acid price card that mentions among " State Standard of the People's Republic of China-linseed oil " (GB 8235-87).
The extraction of embodiment 2, oleum lini and analysis
Get 60g linseed oil (Zhangjiakou, Hebei province beneficial friend's fatty foods company limited), be divided into 6 parts at random, every part of 10g, wherein 3 parts are adopted ultrasonic wave secondary solvent method of the present invention to extract oleum lini respectively; Other 3 parts are adopted existing organic solvent extraction method to extract oleum lini respectively.Concrete extracting method and result are as follows:
1, ultrasonic wave secondary solvent method is extracted oleum lini
1) linseed oil is pulverized: get the 10g linseed oil and put into pulverizer and be crushed to particle diameter 0.25-1.20mm.
2) linseed oil after will pulverizing mixes with the 60ml sherwood oil, at ultrasonic frequency 20kHz, and ultrasound intensity 5W/cm
2, extract under the condition of 25 ℃ of temperature, the ultrasonic assisted extraction of mixed solution 30 minutes.
3) filter the collection extracting solution.
4) extracting solution is placed rotatory evaporator in 45 ℃, be evaporated to pulpous state under 60 rev/mins, put into vacuum drier then and further remove solvent, the oil that obtains is oleum lini.
3 repetitions are established in experiment, obtain oleum lini 4.242g, 4.193g, 4.249g respectively.
The oleum lini extraction yield of 3 revision tests is respectively 86.98%, 85.97%, 87.12%.
The oleum lini productive rate of this leaching process is 42.28 ± 0.31, extraction yield is 86.69 ± 0.63, extraction time is that 30 minutes, solvent load are 60ml, and extracting temperature is 25 ℃.
2, the conventional organic solvents extraction method is extracted oleum lini
1) linseed oil is pulverized, with step 1 1).
2) linseed oil after will pulverizing mixes with the 60ml sherwood oil, extracts under the condition of 25 ℃ of temperature, mixed liquid dipping is left standstill extracted 30 minutes.
3) filter to collect extracting solution, with step 1 3).
4) with step 1 4).
3 repetitions are established in experiment, obtain oleum lini 3.201g, 3.269g, 3.294g respectively.
The oleum lini extraction yield of 3 revision tests is respectively 65.63%, 67.03%, 67.54%.
The oleum lini productive rate of this leaching process is 32.55 ± 0.48, extraction yield be 66.74 ± 0.99 (, extraction time is that 30 minutes, solvent load are 60ml, extracting temperature is 25 ℃.
3, the analysis of oleum lini
1) specific gravity test of oleum lini (GB 5526-85)
Carry out specific gravity test according to State Standard of the People's Republic of China GB 5526-85, experimental result shows that the oleum lini proportion that is extracted by ultrasonic wave secondary solvent method is 0.9357, the oleum lini proportion that is extracted by the conventional organic solvents extraction method is 0.9330, all drops between the oleum lini characteristic constant 0.9260-0.9365 that " State Standard of the People's Republic of China-linseed oil " mention in (GB8235-87).
2) refractive index of oleum lini is measured (GB 5527-85)
Carrying out refractive index according to State Standard of the People's Republic of China GB 5527-85 measures, test-results shows that the oleum lini refractive index that is extracted by ultrasonic wave secondary solvent method is 1.4796, the oleum lini refractive index that is extracted by the conventional organic solvents extraction method is 1.4799, all drops between the oleum lini characteristic constant 1.4785-1.4840 that mentions among " State Standard of the People's Republic of China-linseed oil " (GB 8235-87).
3) acid value of oleum lini is measured (GB 5530-85)
Carrying out acid value according to State Standard of the People's Republic of China GB 5530-85 measures, test-results shows that the oleum lini acid value of being extracted by ultrasonic wave secondary solvent method is 1.27mgKOH/g, the oleum lini acid value of being extracted by the conventional organic solvents extraction method is 1.11mgKOH/g, all less than the accurate 4.0mgKOH/g of (eating) linolenic acid price card that mentions among " State Standard of the People's Republic of China-linseed oil " (GB 8235-87).
4, the fatty acid compositional analysis of oleum lini
The oleum lini that the oleum lini and the conventional organic solvents method of ultrasonic assisted extraction method extraction are extracted carries out fatty acid compositional analysis, and concrete operations are as follows:
Gas phase equipment: Agilent 6890N, U.S. Agilent Technologies, the U.S.; GC conditions: detector: flame ionization ditector (FID); Chromatographic column: HP-Innowax (0.32*30m*0.25mm); Carrier gas: N
2, 1ml/min, constant current; Injector temperature: 250 ℃; Splitting ratio: 1: 50; Sample size: 1mL; Fid detector temperature: 280 ℃; Make-up gas: N
2, 40ml/min; Air velocity: 450ml/min; Hydrogen flow rate: 50ml/min.Adopt temperature programming: initial 40 ℃, keep 0.5min, be warming up to 195 ℃ with 25 ℃/min speed, be warming up to 205 ℃ with 3 ℃/min speed again, rise to 230 ℃ with 8 ℃/min again, keep 4min, rise to 240 ℃ with 5 ℃/min at last, keep 2min.
Detected result sees Table 1.As seen both fatty acid components and content do not have significant difference.
The fatty acid component analysis of table 1 oleum lini
| Fatty acid component | Ultrasonic assisted extraction method | Organic solvent method |
| C16∶0 C16∶1 C17∶0 | 5.529 0.053 0.059 | 5.613 0.058 0.063 |
| C17∶1 C18∶0 C18∶1 C18∶2 C18∶3 C20∶0 C20∶2 C20∶4 C22∶0 C22∶1 C22∶2 C24∶0 | 0.042 3.267 16.919 15.835 56.006 0.216 0.315 0.061 0.144 0.021 0.092 0.094 | 0.045 3.245 16.762 15.810 55.776 0.138 0.320 0.072 0.130 0.020 0.114 0.085 |
| Other | 1.347 | 1.749 |
5, the analysis of linseed oil residue
Linseed oil residue after linseed oil residue after the ultrasonic assisted extraction and the extraction of conventional organic solvents method is carried out scanning electron microscope (ratio of enlargement is 1000 times), see Fig. 1.A) be the scanning electron microscope image of residue after the de-oiling of conventional organic solvents method among Fig. 1; B) be the scanning electron microscope image of residue after the ultrasonic auxiliary law de-oiling.
As seen from the figure, the resid amount of the linseed oil residue after the ultrasonic assisted extraction significantly is lower than the resid amount of the linseed oil residue after the conventional organic solvents method is extracted.
The extraction of embodiment 3, oleum lini and analysis
Get 60g linseed oil (Zhangjiakou, Hebei province beneficial friend's fatty foods company limited), be divided into 6 parts at random, every part of 10g, wherein 3 parts are adopted ultrasonic wave secondary solvent method of the present invention to extract oleum lini respectively; Other 3 parts are adopted existing organic solvent extraction method to extract oleum lini respectively.Concrete extracting method and result are as follows:
1, ultrasonic wave secondary solvent method is extracted oleum lini
1) linseed oil is pulverized: get the 10g linseed oil and put into pulverizer and be crushed to particle diameter 0.25-1.20mm.
2) linseed oil after will pulverizing mixes with the 80ml normal hexane, at ultrasonic frequency 30kHz, and ultrasound intensity 10W/cm
2, extract under the condition of 35 ℃ of temperature, the ultrasonic assisted extraction of mixed solution 60 minutes.
3) filter the collection extracting solution.
4) extracting solution is placed rotatory evaporator in 50 ℃, be evaporated to pulpous state under 60 rev/mins, put into vacuum drier then and further remove solvent, the oil that obtains is oleum lini.
3 repetitions are established in experiment, obtain oleum lini 4.548g, 4.392g, 4.479g respectively.
The oleum lini extraction yield of 3 revision tests is respectively 93.25%, 90.06%, 91.84%.
The oleum lini productive rate of this leaching process is 44.73 ± 0.78, extraction yield is 91.72 ± 1.60, extraction time is that 60 minutes, solvent load are 80ml, and extracting temperature is 35 ℃.
2, the conventional organic solvents extraction method is extracted oleum lini
1) linseed oil is pulverized, with step 1 1).
2) linseed oil after will pulverizing mixes with the 80ml normal hexane, extracts under the condition of 35 ℃ of temperature, mixed liquid dipping is left standstill extracted 60 minutes.
3) filter to collect extracting solution, with step 1 3).
4) with step 1 4).
3 repetitions are established in experiment, obtain oleum lini 3.377g, 3.402g, 3.418g respectively.
The oleum lini extraction yield of 3 revision tests is respectively 69.24%, 69.76%, 70.08%.
The oleum lini productive rate of this leaching process is 33.99 ± 0.15, extraction yield is 69.69 ± 0.42, extraction time is that 60 minutes, solvent load are 80ml, and extracting temperature is 35 ℃.
3, the analysis of oleum lini
1) specific gravity test of oleum lini (GB 5526-85)
Carry out specific gravity test according to State Standard of the People's Republic of China GB 5526-85, experimental result shows that the oleum lini proportion that is extracted by ultrasonic wave secondary solvent method is 0.9359, the oleum lini proportion that is extracted by the conventional organic solvents extraction method is 0.9334, all drops between the oleum lini characteristic constant 0.9260-0.9365 that " State Standard of the People's Republic of China-linseed oil " mention in (GB8235-87).
2) refractive index of oleum lini is measured (GB 5527-85)
Carrying out refractive index according to State Standard of the People's Republic of China GB 5527-85 measures, test-results shows that the oleum lini refractive index that is extracted by ultrasonic wave secondary solvent method is 1.4794, the oleum lini refractive index that is extracted by the conventional organic solvents extraction method is 1.4800, all drops between the oleum lini characteristic constant 1.4785-1.4840 that mentions among " State Standard of the People's Republic of China-linseed oil " (GB 8235-87).
3) acid value of oleum lini is measured (GB 5530-85)
Carrying out acid value according to State Standard of the People's Republic of China GB 5530-85 measures, test-results shows that the oleum lini acid value of being extracted by ultrasonic wave secondary solvent method is 1.35mgKOH/g, the oleum lini acid value of being extracted by the conventional organic solvents extraction method is 1.19mgKOH/g, all less than (eating) oleum lini acid value 4.0mgKOH/g that mentions among " State Standard of the People's Republic of China-linseed oil " (GB 8235-87).
The extraction of embodiment 4, oleum lini and analysis
Get 60g linseed oil (Zhangjiakou, Hebei province beneficial friend's fatty foods company limited), be divided into 6 parts at random, every part of 10g, wherein 3 parts are adopted ultrasonic wave secondary solvent method of the present invention to extract oleum lini respectively; Other 3 parts are adopted existing organic solvent extraction method to extract oleum lini respectively.Concrete extracting method and result are as follows:
1, ultrasonic wave secondary solvent method is extracted oleum lini
1) linseed oil is pulverized: get the 10g linseed oil and put into pulverizer and be crushed to particle diameter 0.25-1.20mm.
2) linseed oil after will pulverizing mixes with the 100ml sherwood oil, at ultrasonic frequency 40kHz, and ultrasound intensity 15W/cm
2, extract under the condition of 45 ℃ of temperature, the ultrasonic assisted extraction of mixed solution 90 minutes.
3) filter the collection extracting solution.
4) extracting solution is placed rotatory evaporator in 45 ℃, be evaporated to pulpous state under 60 rev/mins, put into vacuum drier then and further remove solvent, the oil that obtains is oleum lini.
3 repetitions are established in experiment, obtain oleum lini 4.684g, 4.759g, 4.648g respectively.
The oleum lini extraction yield of 3 revision tests is respectively 96.04%, 97.58%, 95.30%.
The oleum lini productive rate of this leaching process is 46.97 ± 0.57, extraction yield is 96.31 ± 1.16, extraction time is that 90 minutes, solvent load are 100ml, and extracting temperature is 45 ℃.
2, the conventional organic solvents extraction method is extracted oleum lini
1) linseed oil is pulverized, with step 1 1).
2) linseed oil after will pulverizing mixes with the 100ml sherwood oil, extracts under the condition of 45 ℃ of temperature, mixed liquid dipping is left standstill extracted 90 minutes.
3) filter to collect extracting solution, with step 1 3).
4) with step 1 4).
3 repetitions are established in experiment, obtain oleum lini 3.471g, 3.396g, 3.493g respectively.
The oleum lini extraction yield of 3 revision tests is respectively 71.17%, 69.63%, 71.62%.
The oleum lini productive rate of this leaching process is 34.53 ± 0.38, extraction yield is 70.81 ± 1.04, extraction time is that 90 minutes, solvent load are 100ml, and extracting temperature is 45 ℃.
3, the analysis of oleum lini
1) specific gravity test of oleum lini (GB 5526-85)
Carry out specific gravity test according to State Standard of the People's Republic of China GB 5526-85, experimental result shows that the oleum lini proportion that is extracted by ultrasonic wave secondary solvent method is 0.9363, the oleum lini proportion that is extracted by the conventional organic solvents extraction method is 0.9335, all drops between the oleum lini characteristic constant 0.9260-0.9365 that " State Standard of the People's Republic of China-linseed oil " mention in (GB8235-87).
2) refractive index of oleum lini is measured (GB 5527-85)
Carrying out refractive index according to State Standard of the People's Republic of China GB 5527-85 measures, test-results shows that the oleum lini refractive index that is extracted by ultrasonic wave secondary solvent method is 1.4795, the oleum lini refractive index that is extracted by the conventional organic solvents extraction method is 1.4802, all drops between the oleum lini characteristic constant 1.4785-1.4840 that mentions among " State Standard of the People's Republic of China-linseed oil " (GB 8235-87).
3) acid value of oleum lini is measured (GB 5530-85)
Carrying out acid value according to State Standard of the People's Republic of China GB 5530-85 measures, test-results shows that the oleum lini acid value of being extracted by ultrasonic wave secondary solvent method is 1.48mgKOH/g, the oleum lini acid value of being extracted by the conventional organic solvents extraction method is 1.21mgKOH/g, all less than (eating) oleum lini acid value 4.0mgKOH/g that mentions among " State Standard of the People's Republic of China-linseed oil " (GB 8235-87).
The extraction of embodiment 5, oleum lini and analysis
Get 60g linseed oil (Zhangjiakou, Hebei province beneficial friend's fatty foods company limited), be divided into 6 parts at random, every part of 10g, wherein 3 parts are adopted ultrasonic wave secondary solvent method of the present invention to extract oleum lini respectively; Other 3 parts are adopted existing organic solvent extraction method to extract oleum lini respectively.Concrete extracting method and result are as follows:
1, ultrasonic wave secondary solvent method is extracted oleum lini
1) linseed oil is pulverized: get the 10g linseed oil and put into pulverizer and be crushed to particle diameter 0.25-1.20mm.
2) linseed oil after will pulverizing mixes with the 200ml normal hexane, at ultrasonic frequency 100kHz, and ultrasound intensity 40W/cm
2, extract under the condition of 60 ℃ of temperature, the ultrasonic assisted extraction of mixed solution 180 minutes.
3) filter the collection extracting solution.
4) extracting solution is placed rotatory evaporator in 50 ℃, be evaporated to pulpous state under 60 rev/mins, put into vacuum drier then and further remove solvent, the oil that obtains is oleum lini.
3 repetitions are established in experiment, obtain oleum lini 4.823g, 4.817g, 4.870g respectively.
The extraction yield of 3 revision tests is respectively 98.89%, 98.77%, 99.86%.
The oleum lini productive rate of this leaching process is 48.37 ± 0.29, extraction yield is 99.17 ± 0.60, extraction time is that 180 minutes, solvent load are 200ml, and extracting temperature is 60 ℃.
2, the conventional organic solvents extraction method is extracted oleum lini
1) linseed oil is pulverized, with step 1 1).
2) linseed oil after will pulverizing mixes with the 200ml normal hexane, extracts under the condition of 60 ℃ of temperature, mixed liquid dipping is left standstill extracted 180 minutes.
3) filter to collect extracting solution, with step 1 3).
4) with step 1 4).
3 repetitions are established in experiment, obtain oleum lini 3.569g, 3.603g, 3.496g respectively.
The oleum lini extraction yield of 3 revision tests is respectively 73.18%, 73.88%, 71.68%.
The oleum lini productive rate of this leaching process is 35.56 ± 0.40, extraction yield is 72.91 ± 1.12, extraction time is that 180 minutes, solvent load are 200ml, and extracting temperature is 60 ℃.
3, the analysis of oleum lini
1) specific gravity test of oleum lini (GB 5526-85)
Carry out specific gravity test according to State Standard of the People's Republic of China GB 5526-85, experimental result shows that the oleum lini proportion that is extracted by ultrasonic wave secondary solvent method is 0.9362, the oleum lini proportion that is extracted by the conventional organic solvents extraction method is 0.9338, all drops between the oleum lini characteristic constant 0.9260-0.9365 that " State Standard of the People's Republic of China-linseed oil " mention in (GB8235-87).
2) refractive index of oleum lini is measured (GB 5527-85)
Carrying out refractive index according to State Standard of the People's Republic of China GB 5527-85 measures, test-results shows that the oleum lini refractive index that is extracted by ultrasonic wave secondary solvent method is 1.4794, the oleum lini refractive index that is extracted by the conventional organic solvents extraction method is 1.4800, all drops between the oleum lini characteristic constant 1.4785-1.4840 that mentions among " State Standard of the People's Republic of China-linseed oil " (GB 8235-87).
3) acid value of oleum lini is measured (GB 5530-85)
Carrying out acid value according to State Standard of the People's Republic of China GB 5530-85 measures, test-results shows that the oleum lini acid value of being extracted by ultrasonic wave secondary solvent method is 2.11mgKOH/g, the oleum lini acid value of being extracted by the conventional organic solvents extraction method is 1.20mgKOH/g, all less than (eating) oleum lini acid value 4.0mgKOH/g that mentions among " State Standard of the People's Republic of China-linseed oil " (GB 8235-87).
Claims (9)
1. a method of extracting oleum lini is to be raw material with the linseed oil, adopts organic solvent method to extract, and obtains oleum lini, and it is characterized in that: the described ultrasonic frequency that is extracted in is that 20-100kHz and ultrasound intensity are 1-40W/cm
2The supersound process condition under carry out.
2. method according to claim 1 is characterized in that: described ultrasonic frequency is preferably 20-40kHz, and described ultrasound intensity is preferably 5-15W/cm
2
3. method according to claim 1 and 2 is characterized in that: described organic solvent is sherwood oil or normal hexane or Virahol or soybean extracting solvent no.6.
4. method according to claim 3 is characterized in that: the proportioning of described linseed oil and described organic solvent is the 1kg linseed oil, the 4-20L organic solvent.
5. method according to claim 4 is characterized in that: the proportion optimization of described linseed oil and described organic solvent is the 1kg linseed oil, the 6-10L organic solvent.
6. according to arbitrary described method in the claim 1 to 5, it is characterized in that: the extraction temperature of described supersound process is 20-60 ℃, and extraction time is 30-180 minute.
7. according to arbitrary described method in the claim 1 to 5, it is characterized in that: the extraction temperature of described supersound process is preferably 25-45 ℃, and extraction time is preferably 30-90 minute.
8. method according to claim 1 is characterized in that: described linseed oil rolls and/or expanded and/or pulverization process before extracting.
9. according to arbitrary described method in the claim 1 to 8, it is characterized in that: also comprise purification step in the described method.
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| CN102876447A (en) * | 2012-10-17 | 2013-01-16 | 青岛农业大学 | Goose fat liver oil extracting method |
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