CN109852470A - A kind of method that Seabuckthorm Seed Oil is extracted in ultrasonic-microwave collaboration - Google Patents
A kind of method that Seabuckthorm Seed Oil is extracted in ultrasonic-microwave collaboration Download PDFInfo
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Abstract
The present invention relates to a kind of ultrasonic-microwaves to cooperate with the method for extracting Seabuckthorm Seed Oil, using sea-buckthorn powder of seeds as raw material, after extractant is added, extracts Seabuckthorm Seed Oil through Ultrasonic-microwave synergistic extraction method.The present invention is high by the Seabuckthorm Seed Oil recovery rate that ultrasonic-microwave collaboration method is extracted, and shortens extracting cycle, and filled up application blank of this method on Seabuckthorm Seed Oil, while ultrasonic-microwave collaboration method and supercritical CO2The composition and content of the hippophae rhamnoides seed oil fatty acid of method extraction are essentially identical.
Description
Technical field
The invention belongs to eat oil extract field, in particular to the side of Seabuckthorm Seed Oil is extracted in a kind of ultrasonic-microwave collaboration
Method.
Background technique
Sea-buckthorn is the shrub of Elaeangnaceae Hippophne, and alias vinegar willow, black thorn, acid thorn have 7 kind of 11 subspecies, China in the world
There is 7 kind of 7 subspecies, China accounts for the 99% of world's sea-buckthorn gross area, is distributed mainly on northwest, North China, northeast and southwest etc. in China
A provinces and regions more than 10.China is to sea buckthorn resources using earliest country, and early in the second half 8th century of Christian era, the Four-Volume Medical Code is just
There is record to sea-buckthorn medical usage, contains flavone compound in sea buckthorn fruit, Polyphenols chemical substance and abundant
The nutriments such as unsaturated fatty acid, vitamin.Seabuckthorm Seed Oil has very high nutritive value and economic value, in Seabuckthorm Seed Oil
Unsaturated fatty acid is up to 74.16%-90.70%, linoleic acid and linolenic acid with high-content.In addition, also containing class Hu trailing plants
The bioactive substances such as Bu Su, tocopherol, phytosterol, phosphatide, micromolecule polypeptide, Seabuckthorm Seed Oil have promote regeneration and
The medicines and health protections functions such as epithelial tissue healing, anti-inflammatory, anti-tumor aging.
The common extracting method of Seabuckthorm Seed Oil includes lixiviation process, squeezing method, supercritical CO2Extraction and subcritical abstraction etc..Pressure
The recovery rate of squeezing method is low, and the processing of expressing process high temperature has larger impact to oil quality；Supercritical CO2Extraction with it is subcritical
Extraction is stringent to equipment requirement, at high cost；Lixiviation process extracts the recovery rate highest of Seabuckthorm Seed Oil, but extraction time is longer, can lead to
Supplementary means is crossed to shorten extraction time and obtain high-quality grease.Jiang Mingzhu passes through supercritical CO2Seabuckthorn seeds are obtained by extraction in technology
Oil, the extraction yield of the Seabuckthorm Seed Oil after process optimization are 7.57%.Feng Lidan etc. using R134a be used as extractant, selection compared with
Seabuckthorm Seed Oil, extraction yield 7.32% is obtained by extraction in supercritical operation mild condition, the subcritical technology of advantage of lower cost.
It opens ease etc. and has studied Microwave Pretreatment solvent extraction new process, in fixed microwave frequency 2450MHz, power level 560W/120g
Under conditions of extract 2min, Seabuckthorm Seed Oil recovery rate reaches 7.94%, and recovery rate improves 9.34%, and greatly shortens
The time of extraction.Zhu Yanrong etc. is research shows that using petroleum ether as extractant, extraction time 3h, recovery rate 11.09%.
Meng Shaohua etc. has studied the water substitution extraction process of Seabuckthorm Seed Oil, has obtained the preferable Seabuckthorm Seed Oil of physicochemical property, recovery rate
It is 3.5%.
The Seabuckthorm Seed Oil recovery rate that lixiviation process obtains in the prior art is low, and the present invention provides a kind of ultrasonic-microwave collaboration
The method for extracting Seabuckthorm Seed Oil to improve the recovery rate of Seabuckthorm Seed Oil, and does not have ultrasonic-microwave collaboration method to mention in the prior art
The report of Seabuckthorm Seed Oil is taken, and then fills up application blank of this method on Seabuckthorm Seed Oil.
Summary of the invention
The purpose of the present invention is the recovery rates to further increase Seabuckthorm Seed Oil, shorten extracting cycle, provide a kind of super
The method that sound wave-microwave cooperating extracts Seabuckthorm Seed Oil has probed into the technique item of ultrasonic-microwave collaboration method extraction Seabuckthorm Seed Oil
Part, to fill up application blank of this method on Seabuckthorm Seed Oil.
The present invention is achieved through the following technical solutions:
One, extraction is added using sea-buckthorn powder of seeds as raw material in a kind of method that Seabuckthorm Seed Oil is extracted in ultrasonic-microwave collaboration
After solvent, Seabuckthorm Seed Oil is extracted through Ultrasonic-microwave synergistic extraction method.
Specifically, the extraction conditions are as follows: extraction time 5-30min, liquid-to-solid ratio 4-12:1, ultrasonic power 400-
900W, microwave power 100-600W, 35-70 DEG C of extraction temperature, the extractant are petroleum ether, n-hexane, ethyl acetate
In any one.
Specifically, the extraction conditions are as follows: extraction time 20-30min, liquid-to-solid ratio 8-12:1, ultrasonic power 600-
800W, microwave power 200-500W, 50-60 DEG C of extraction temperature, the extractant are petroleum ether, n-hexane, ethyl acetate
In any one.
Specifically, the extraction conditions are as follows: extraction time 22min, liquid-to-solid ratio 9:1, ultrasonic power 628W, microwave function
57 DEG C of rate 200W, extraction temperature, the extractant are n-hexane.
Specifically, the method that Seabuckthorm Seed Oil is extracted in a kind of ultrasonic-microwave collaboration, it is characterised in that: specific step
It is rapid as follows:
Step 1: seabuckthorn seeds are cleaned, select, dried, it is placed in 45 DEG C of drying boxes that drying to constant weight；
Step 2: the seabuckthorn seeds that step 1 obtains are through crushing crusher machine, then seabuckthorn seeds are through 60 mesh sieves；
Step 3: taking the sea-buckthorn powder of seeds under a certain amount of sieve through step 2, extractant is added and is placed on ultrasonic-microwave
Seabuckthorm Seed Oil extraction is carried out in synergic solvent extraction instrument；
Step 4: the resulting extracting solution of step 3 is filtered by vacuum, filtrate is obtained；
Step 5: the filtrate that step 4 is collected first is carried out rotary evaporation recycling organic solvent, and it is placed on 80-90 DEG C of drum
It is constant to quality constant weight in wind drying box.
Good effect by adopting the above technical scheme: 1, it by Seabuckthorm Seed Oil that ultrasonic-microwave collaboration method extract extracts
Rate is high, and extractant further improves the recovery rate of Seabuckthorm Seed Oil when being n-hexane, shortens extracting cycle, and there is collaboration to make
With；2, the Seabuckthorm Seed Oil and supercritical CO for cooperateing with method to be obtained by extraction by analysis ultrasonic-microwave2The sea-buckthorn that technology is obtained by extraction
The composition and its content of fatty acid in seed oil, it is thus understood that ultrasonic-microwave cooperates with method and supercritical CO2The Seabuckthorm Seed Oil of method extraction
The composition of fatty acid and content are essentially identical.
Detailed description of the invention
Fig. 1 is influence of the different extractants to Seabuckthorm Seed Oil recovery rate；
Fig. 2 is influence of the extraction time to Seabuckthorm Seed Oil recovery rate；
Fig. 3 is influence of the liquid-to-solid ratio to Seabuckthorm Seed Oil recovery rate；
Fig. 4 is influence of the ultrasonic power to Seabuckthorm Seed Oil recovery rate；
Fig. 5 is influence of the microwave power to Seabuckthorm Seed Oil recovery rate；
Fig. 6 is influence of the extraction temperature to Seabuckthorm Seed Oil recovery rate；
Fig. 7 is the response surface design and contour map of extraction time and ultrasonic power to Seabuckthorm Seed Oil extraction rate impact；
Fig. 8 is the response surface design and contour map of extraction temperature and ultrasonic power to Seabuckthorm Seed Oil extraction rate impact；
Fig. 9 is the response surface design and contour map of ultrasonic power and liquid-to-solid ratio to Seabuckthorm Seed Oil extraction rate impact.
Specific embodiment
Below by specific embodiment and test example, the present invention will be further described, but should not be construed as to of the invention
It limits.
Raw material: late autumn red big fruit sea-buckthorn adopts the seed behind 93 farm of Heilungkiang, juice processed, carries out naturally dry.
Reagent: Wijs reagent: Shanghai Mike's woods biochemical technology Co., Ltd；
Petroleum ether, n-hexane, ethyl acetate, ether, isopropanol, hexamethylene, glacial acetic acid are that analysis is pure: Tianjin great Mao
Chemical reagent factory.
Instrument and equipment: III type vacuum pump of SHZ-D: the city Gong Yi Yu Hua instrument Co., Ltd；
HWS24 type electric-heated thermostatic water bath: the permanent Science and Technology Ltd. in Shanghai one；
RE-2000B Rotary Evaporators: Shanghai Yarong Biochemical Instrument Plant；
101-2AB type electric drying oven with forced convection: Tianjin Stettlen Instrument Ltd.；
XH-300A type Ultrasonic-microwave synergistic extraction instrument: Beijing XiangHu Science and Technology Development Co., Ltd.；
7890A gas chromatograph, Agilent company, the U.S.；
GY-PS-02 multifunctional crusher, Jiangxi cloud Food Machinery Co., Ltd.；
EX324 type electronic balance: Ohaus Instrument (Shanghai) Co., Ltd..
Recovery rate calculates
The Seabuckthorm Seed Oil that ultrasonic-microwave collaboration method is obtained by extraction, the following formula of the calculation of recovery rate:
In formula: Y is recovery rate；m1To extract Seabuckthorm Seed Oil quality, g；m2For seabuckthorn seeds powder quality, g.
The detection of Seabuckthorm Seed Oil physical and chemical index
The identification of transparency is referring to GB/T 5525-2008；The identification of color is referring to GB/T 5492-2008；Iodine number
Measurement is referring to GB/T 5532-2008；The measurement of acid value is referring to GB 5009.229-2016；The measurement of peroxide value (POV) is joined
According to GB5009.27-2016；The measurement of saponification number is referring to GB/T 5534-2008；The measurement of grease refraction index is referring to GB/T
5527-2010；The measurement of vitamin E is referring to GB/T 5009.82-2016；The measurement of moisture and volatile matter content is referring to GB
5009.236-2016；Analysis of Fatty Acids Composition: referring to GB 5009.168-2016.
Data processing method: each test is repeated 3 times, using 2013 software of Microsoft Excel calculate average value and
Standard deviation is mapped using 8.0 software of Origin, and 17.0 software of SPSS analyzes the significance of difference between average value, and P < 0.05 is poor
Different significant, there are significant difference (P < 0.05) for the different extraction time Seabuckthorm Seed Oil recovery rates of the expression such as a in Figure of description, b.
Embodiment 1
Embodiment 1 illustrates the selection of extractant
5g sea-buckthorn powder of seeds is weighed respectively in extracting in flask, and 40mL (liquid-to-solid ratio 8:1mL/g) petroleum ether, just oneself is respectively added
Alkane, ethyl acetate are placed in Ultrasonic-microwave synergistic extraction instrument.In ultrasonic power 800W, microwave power 300W, temperature is extracted
When spending 50 DEG C, 20min is extracted.Seabuckthorm Seed Oil recovery rate is calculated, as a result as shown in Figure 1, and the seabuckthorn seeds of different solvents extraction
Oil carries out physical and chemical index measurement, chooses the optimum extractant of Seabuckthorm Seed Oil.
The Seabuckthorm Seed Oil physical and chemical index of 1 different solvents of table extraction
Note: same column difference small English alphabet indicates that there are significant difference (P < 0.05).
As shown in Figure 1, recovery rate highest of the n-hexane as Seabuckthorm Seed Oil Extraction solvent Seabuckthorm Seed Oil, petroleum ether take second place,
But there was no significant difference between the two (P>0.05), the recovery rate of ethyl acetate is minimum (P<0.05).Extracted by 1 different solvents of table
The physical and chemical index of the Seabuckthorm Seed Oil taken it is found that ethyl acetate extracted as extractant Seabuckthorm Seed Oil saponification number highest (P <
0.05), but muddy stain, impurity is more, and recovery rate is low, is not appropriate for the Extraction solvent as Seabuckthorm Seed Oil.N-hexane is made
The iodine number of Seabuckthorm Seed Oil is higher (P > 0.05) when for Extraction solvent, illustrates that its unsaturated fatty acid content is higher.Petroleum ether with just
When hexane is as Extraction solvent, there was no significant difference with saponification number (P > 0.05) for the acid value of Seabuckthorm Seed Oil.In view of industrial one
As extracted with n-hexane, therefore, extractant of the n-hexane as Seabuckthorm Seed Oil is chosen in this experiment.
Embodiment 2
Embodiment 2 illustrates influence of the extraction time to Seabuckthorm Seed Oil recovery rate
5g sea-buckthorn powder of seeds is accurately weighed respectively in extracting in flask, n-hexane is added by liquid-to-solid ratio 8:1 (mL/g), super
Acoustic power 800W, microwave power 300W at 50 DEG C of Extracting temperature, extract 5,10,15,20,25,30min respectively.It calculates different
Influence of the extraction time to Seabuckthorm Seed Oil recovery rate, as a result as shown in Fig. 2, determining optimal extraction time.
As shown in Figure 2, extraction time is increased to 10min by 5min, and solid-liquid concentration difference is larger at this time, grease diffusion rate compared with
Fastly, Seabuckthorm Seed Oil recovery rate is significantly raised；With the increase of ultrasonic-microwave synergistic effect time, solid-liquid concentration difference is reduced, husky
Spine seed oil extract rate increases slow；It, may be broken due to ultrasonic wave and microwave when extraction time increases to 25min by 20min
Effect, so that Seabuckthorm Seed Oil the amount of dissolution continues growing, Seabuckthorm Seed Oil recovery rate significantly improves and reaches highest, and recovery rate reaches
12.47%；But it is to continue with the time for extending extraction, Seabuckthorm Seed Oil recovery rate declines instead, it may be possible to because excessively prolonged super
The effect of the fuel factor of sound wave and microwave, causes organic solvent to volatilize and the entrainment of grease has occurred, cause Seabuckthorm Seed Oil recovery rate
Decline.
Embodiment 3
Embodiment 3 illustrates influence of the liquid-to-solid ratio to Seabuckthorm Seed Oil recovery rate
In ultrasonic power 800W, microwave power 300W, 50 DEG C of Extracting temperature, the sea-buckthorn powder of seeds of 5g is weighed in extraction
In flask, n-hexane is added according to the liquid-to-solid ratio of 4:1,6:1,8:1,10:1,12:1 (mL/g) respectively and carries out mentioning for Seabuckthorm Seed Oil
It takes, extraction time 25min.Influence of the different liquid-to-solid ratios to Seabuckthorm Seed Oil recovery rate is calculated, as a result as shown in figure 3, determining
Seabuckthorm Seed Oil extracts optimum liquid-to-solid ratio.
From the figure 3, it may be seen that liquid-to-solid ratio increases to 8:1 (mL/g) by 4:1, Seabuckthorm Seed Oil recovery rate is obviously increased, in liquid-to-solid ratio
Recovery rate reaches maximum value 12.83% when 8:1 (mL/g)；With continuing growing for organic solvent ratio, decline is presented in recovery rate
Trend may can not be such that more greases dissolve out due to the increase of organic solvent, and lead to organic solvent recovery time
Extend, causes the waste of Seabuckthorm Seed Oil.Therefore, it chooses ultrasonic-microwave collaboration method and extracts the optimal liquid-to-solid ratio of Seabuckthorm Seed Oil
For 8:1 (mL/g).
Embodiment 4
Embodiment 4 illustrates influence of the ultrasonic power to Seabuckthorm Seed Oil recovery rate
The sea-buckthorn powder of seeds of 5g is weighed in extracting in flask, in microwave power 300W, 50 DEG C of Extracting temperature, liquid-to-solid ratio 8:1
(mL/g) n-hexane is added under conditions of under the conditions of, ultrasonic power is respectively 400W, 500W, 600W, 700W, 800W, 900W
It carries out ultrasonic-microwave collaboration method and extracts Seabuckthorm Seed Oil, extraction time 25min.Different ultrasonic powers are calculated to seabuckthorn seeds
The influence of oil extract rate, as a result as shown in figure 4, determining optimal ultrasonic wave extraction power.
As shown in Figure 4, ultrasonic power increases, and Seabuckthorm Seed Oil recovery rate is continuously increased, when ultrasonic power is 700W
It is 13.59% that recovery rate, which reaches maximum value,；Ultrasonic power continues growing, and Seabuckthorm Seed Oil recovery rate declines instead.Therefore ultrasonic wave-
It is 700W that microwave cooperating method, which extracts the optimal ultrasonic power of Seabuckthorm Seed Oil,.
Embodiment 5
Embodiment 5 illustrates influence of the microwave power to Seabuckthorm Seed Oil recovery rate
The sea-buckthorn powder of seeds of 5g is weighed in extracting in flask, in ultrasonic power 800W, 50 DEG C of Extracting temperature, liquid-to-solid ratio 8:
N-hexane is added under the conditions of 1 (mL/g), microwave power is respectively that 100W, 200W, 300W, 400W, 500W, 600W carry out ultrasound
Wave-microwave cooperating method extracts Seabuckthorm Seed Oil, extraction time 25min.Different microwave powers is calculated to Seabuckthorm Seed Oil recovery rate
Influence, as a result as shown in figure 5, determining that Seabuckthorm Seed Oil extracts optimal microwave power.
As shown in Figure 5, when microwave power is 200W and 500W, recovery rate is higher, and still, microwave power is to Seabuckthorm Seed Oil
The influence of recovery rate is not significant.In microwave power 200W, Seabuckthorm Seed Oil recovery rate is relatively high, is 12.89%.This may
It is related with the synergic solvent extraction of microwave using ultrasonic wave (power 800W) in this experiment.
Embodiment 6
Embodiment 6 illustrates influence of the extraction temperature to Seabuckthorm Seed Oil recovery rate
The sea-buckthorn powder of seeds of 5g is weighed in extracting in flask, in ultrasonic power 800W, microwave power 300W, liquid-to-solid ratio 8:
N-hexane is added under the conditions of 1 (mL/g), Extracting temperature is respectively 35 DEG C, 40 DEG C, 45 DEG C, 50 DEG C, 55 DEG C, 60 DEG C, 65 DEG C, 70 DEG C
It carries out ultrasonic-microwave collaboration method and extracts Seabuckthorm Seed Oil, extraction time 25min.Different extraction temperatures is calculated to seabuckthorn seeds
The influence of oil extract rate, as a result as shown in fig. 6, determining optimal extraction temperature.
It will be appreciated from fig. 6 that extraction temperature is promoted by 35 DEG C to 65 DEG C, Seabuckthorm Seed Oil recovery rate is continuously improved, this is because warm
The raising of degree accelerates the movement velocity of organic solvent and grease molecules, and then the diffusion velocity for accelerating grease improves sea-buckthorn
The recovery rate of seed oil；Extraction temperature continues to rise, and Seabuckthorm Seed Oil recovery rate declines instead, it may be possible to due to close to extractant just
The boiling point of hexane, high temperature promote organic solvent volatilization in part that Seabuckthorm Seed Oil recovery rate is caused to decline, it is also possible to so that certain wave
The loss of volatile material is so that the recovery rate of Seabuckthorm Seed Oil declines.Ultrasonic-microwave cooperates with method to extract the optimal extraction of Seabuckthorm Seed Oil
Taking temperature is 65 DEG C, its recovery rate is 13.58% at this time, and still, 60 DEG C and 65 DEG C of difference to its extraction rate impact are not shown
It writes, it is contemplated that influence of the high temperature to active material, choosing extraction temperature is 60 DEG C.
Test example 1
Test example 1 illustrates that response surface optimization is tested
By experiment of single factor it is found that influence of the microwave power to Seabuckthorm Seed Oil recovery rate be not significant, therefore when selection extraction
Between, 4 liquid-to-solid ratio, ultrasonic power, extraction temperature factors to its extraction process carry out response surface optimization test, with Seabuckthorm Seed Oil
Recovery rate is response, carries out experimental design, response surface using the Box-Behnken design of 8.0 software of Design-Expert
Experimental design and the results are shown in Table 2, regression model variance analysis is as shown in table 3:
The design of 2 response surface experiments of table and result
3 regression model variance analysis of table
Regression fit is carried out to response surface experiments result according to Design-Expert 8.0.6 Data Analysis Software, is obtained
Regression fit equation is
Y=13.68-0.35A-0.14B-0.19C+0.079D-0.065AB+0.57AC+0.10AD+0 .15BC-
0.083BD-0.63CD-0.46A2-0.52B2-0.33C2-0.40D2.As shown in Table 3, the model influence it is extremely significant (P <
0.0001) it is not significant (0.9256 > 0.05), to lose quasi- item, coefficient of determination R2It is 0.9682, shows that the model degree of correlation is good, corrects
Coefficient of determination R2 AdjIt is 0.9364, illustrates that the model can explain the variation of 93.64% effect value, i.e. forecast of regression model value and reality
Measured value energy quite well.
Variance analysis is carried out to regression model, the results are shown in Table 3, and first order A, B, C influences extremely significant in model, and
And the influence order to Seabuckthorm Seed Oil recovery rate is A > C > B, quadratic term A2、B2、C2、D2Influence extremely significant (P < 0.0001).
AC, CD reciprocation are extremely significant (P < 0.01), BC significant interaction (P < 0.05).Response surface and contour such as Fig. 7~Fig. 9 institute
Show.
Test example 2
The confirmatory experiment that 2 Seabuckthorm Seed Oil of test example extracts
After the analysis of Design-Expert 8.0.6 software, ultrasonic-microwave collaboration method extraction Seabuckthorm Seed Oil is determined most
Good process conditions are as follows: extraction time 22.18min, liquid-to-solid ratio 8.95:1 (mL/g), ultrasonic power 627.73W, microwave power
200W, 57.25 DEG C of extraction temperature, Seabuckthorm Seed Oil theoretical extraction rate is 14.05% with this condition, considers the side of practical operation
It just, is extraction time 22min by technical arrangement plan, liquid-to-solid ratio is 9:1 (mL/g), ultrasonic power 628W, microwave power
200W, 57 DEG C of extraction temperature.3 verification tests are carried out under this optimum process condition, calculate the average value of actual extracting rate, knot
Fruit is as shown in table 4.
The confirmatory experiment that 4 Seabuckthorm Seed Oil of table extracts
Note: different small English alphabets indicate that there are significant difference (P < 0.05).
As shown in Table 4, the average value of actual extracting rate is 13.97%, and actual value is close with theoretical value, illustrates the model pair
The description of Seabuckthorm Seed Oil extraction process is reasonable.
It is by the ultrasonic cavitation resonant interaction of certain frequency and the high energy of microwave field that ultrasonic-microwave, which cooperates with extractive technique,
Fuel factor effect combines, have many advantages, such as quickly, it is efficient, do not destroy molecular structure.When ultrasonic-microwave, which cooperates with, to be extracted,
Cell is because absorbing microwave energy inside sea-buckthorn powder of seeds, so that cell interior temperature steeply rises, internal pressure increases, and causes
The pressure increase that cell wall is born；It is acted on simultaneously using the cavitation of ultrasonic wave and Mechanical Crushing, so that cell wall is quickly broken
It splits, accelerates the dissolution of grease.As shown in Table 4, the recovery rate of Ultrasonic-microwave synergistic extraction Seabuckthorm Seed Oil is significantly higher than super
The recovery rate of sound wave extraction and microwave abstracting shows that ultrasonic wave and microwave can be synergistic.Meanwhile ultrasonic-microwave cooperates with
The recovery rate of extraction is also significantly greater than supercritical CO2Method illustrates that ultrasonic-microwave collaboration extractive technique is a kind of extraction sea-buckthorn
The effective ways of seed oil.
Test example 3
Test example 3 illustrates ultrasonic-microwave collaboration method and supercritical CO2The fatty acid compositional analysis of method extraction Seabuckthorm Seed Oil
5 hippophae rhamnoides seed oil fatty acid of table composition and relative amount
Note: "-" is to be not detected
As shown in Table 5, the extraction of ultrasonic-microwave collaboration method and supercritical CO2It is identified in the Seabuckthorm Seed Oil of method extraction
The Seabuckthorm Seed Oil of 14 kinds of fatty acid, ultrasonic-microwave collaboration method extraction individually detects methyl eicosapentaenoic acid (EPA), surpasses
Critical CO2The Seabuckthorm Seed Oil of method extraction individually detects methyl caprylate C8:0.Ultrasonic-microwave cooperates with the Seabuckthorm Seed Oil of method extraction
Unsaturated fatty acid content accounts for 88.93%, and saturated fatty acid content accounts for 11.03%；Main rouge of the content of fatty acid 1% or more
Fat acid type is 5 kinds, including palmitinic acid (7.42%), stearic acid (2.80%), cis- 9- oleic acid (15.90%), linoleic acid
(39.60%), linolenic acid (32.60%), remaining is unsaturated fatty acid, and content is highest for sub- oil in the Seabuckthorm Seed Oil of extraction
Acid, is secondly linolenic acid, and linoleic acid plus linolenic acid has different physiological roles as essential fatty acid.Supercritical CO2Method
The main fatty acid type that hippophae rhamnoides seed oil fatty acid content is obtained by extraction 1% or more cooperates with method to extract with ultrasonic-microwave
The Seabuckthorm Seed Oil type arrived is identical and each content of fatty acid is close, unsaturated fatty acid content 88.57%, saturated fat
Acid content is 11.44%.It follows that the main fatty acid type and content of Seabuckthorm Seed Oil is different, may with the type of sea-buckthorn,
The factors such as the place of production are related.It follows that ultrasonic-microwave collaboration method and supercritical CO2The hippophae rhamnoides seed oil fatty acid of method extraction
It forms essentially identical with content.
Test example 4
Test example 4 illustrates physical and chemical index
Carry out the measurement of main physical and chemical index to the Seabuckthorm Seed Oil extracted under optimum process condition, resulting Seabuckthorm Seed Oil at
Transparence, orange-yellow, iodine number 152.91g/100g, acid value are 3.75mg KOH/g, and peroxide value (POV) is 0.03g/
100g, saponification number are 152.36mg KOH/g, grease refraction index 1.4753, content of vitamin E 127.82mg/100g, water
Divide and volatile content is 0.14%.These parameters meet People's Republic of China (PRC) water conservancy industry standard SL 493-2010 sand
The index of spine seed oil.
In conclusion Seabuckthorm Seed Oil is extracted using ultrasonic-microwave collaboration method, using n-hexane as extractant, in Dan Yin
On the basis of element test and response surface optimization test, the optimal extraction process of Seabuckthorm Seed Oil is determined are as follows: extraction time 22min, liquid
Material is than being 9:1 (mL/g), and ultrasonic power 628W, microwave power 200W, Seabuckthorm Seed Oil extracts 57 DEG C of extraction temperature under this condition
Rate reaches 13.97%, and ultrasonic-microwave cooperates with method abstraction technique to be applied to Seabuckthorm Seed Oil and extracts in test, can effectively shorten week
Phase improves the recovery rate of Seabuckthorm Seed Oil.
Claims (5)
1. a kind of method that Seabuckthorm Seed Oil is extracted in ultrasonic-microwave collaboration, it is characterised in that: using sea-buckthorn powder of seeds as raw material, add
After entering extractant, Seabuckthorm Seed Oil is extracted through Ultrasonic-microwave synergistic extraction method.
2. a kind of method that Seabuckthorm Seed Oil is extracted in ultrasonic-microwave collaboration according to claim 1, it is characterised in that: institute
The extraction conditions stated are as follows: extraction time 5-30min, liquid-to-solid ratio 4-12:1, ultrasonic power 400-900W, microwave power 100-
35-70 DEG C of 600W, extraction temperature, the extractant are petroleum ether, n-hexane, any one in ethyl acetate.
3. a kind of method that Seabuckthorm Seed Oil is extracted in ultrasonic-microwave collaboration according to claim 2, it is characterised in that: institute
The extraction conditions stated are as follows: extraction time 20-30min, liquid-to-solid ratio 8-12:1, ultrasonic power 600-800W, microwave power 200-
50-60 DEG C of 500W, extraction temperature, the extractant are petroleum ether, n-hexane, any one in ethyl acetate.
4. a kind of method that Seabuckthorm Seed Oil is extracted in ultrasonic-microwave collaboration according to claim 3, it is characterised in that: institute
State extraction conditions are as follows: extraction time 22min, liquid-to-solid ratio 9:1, ultrasonic power 628W, microwave power 200W, extraction temperature 57
DEG C, the extractant is n-hexane.
5. a kind of method that Seabuckthorm Seed Oil is extracted in ultrasonic-microwave collaboration according to any one of claims 1-4, special
Sign is: specific step is as follows:
Step 1: seabuckthorn seeds are cleaned, select, dried, it is placed in 45 DEG C of drying boxes that drying to constant weight；
Step 2: the seabuckthorn seeds that step 1 obtains are through crushing crusher machine, then seabuckthorn seeds are through 60 mesh sieves；
Step 3: taking the sea-buckthorn powder of seeds under a certain amount of sieve through step 2, extractant is added and is placed on ultrasonic-microwave collaboration
Seabuckthorm Seed Oil extraction is carried out in abstraction instrument；
Step 4: the resulting extracting solution of step 3 is filtered by vacuum, filtrate is obtained；
Step 5: the filtrate that step 4 is collected first is subjected to rotary evaporation recycling organic solvent, and it is dry to be placed on 80-90 DEG C of air blast
It is constant to quality constant weight in dry case.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110713860A (en) * | 2019-10-10 | 2020-01-21 | 南京益唯森生物科技有限公司 | Method for extracting unsaturated fatty acid from nitraria tangutorum bobr seed oil |
| CN113717788A (en) * | 2021-08-25 | 2021-11-30 | 内蒙古淳点生物科技有限公司 | Sea-buckthorn seed oil and extraction process thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110713860A (en) * | 2019-10-10 | 2020-01-21 | 南京益唯森生物科技有限公司 | Method for extracting unsaturated fatty acid from nitraria tangutorum bobr seed oil |
| CN113717788A (en) * | 2021-08-25 | 2021-11-30 | 内蒙古淳点生物科技有限公司 | Sea-buckthorn seed oil and extraction process thereof |
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