CN114752438A - Ultrasonic-assisted cactus fruit seed oil extraction process - Google Patents
Ultrasonic-assisted cactus fruit seed oil extraction process Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/106—Production of fats or fatty oils from raw materials by extracting using ultra-sounds
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/33—Cactaceae (Cactus family), e.g. pricklypear or Cereus
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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- C11B1/00—Production of fats or fatty oils from raw materials
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- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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Abstract
The invention provides an ultrasonic-assisted cactus fruit seed oil extraction process, which belongs to the technical field of plant extraction, wherein cactus fruit seeds are used as raw materials, ultrasonic-assisted extraction is adopted, and ultrasonic-assisted extraction solvent, material-liquid ratio, ultrasonic time and extraction frequency are optimized through single-factor and orthogonal tests, so that the extraction rate of the fruit seed oil reaches 11.3%.
Description
Technical Field
The invention belongs to the technical field of plant extraction, and particularly relates to an ultrasonic-assisted cactus fruit seed oil extraction process.
Background
Cactus is a plant of Cactus family and Cactus genus, is native to east coast of Mexico, is mainly distributed in coastal areas of south America and southeast, West Indian Islands, Guangdong, Guangxi, Yunnan and Hainan areas of China, and is mostly wild. The mature cactus fruit has dark red epidermis and dark purple red pulp after peeling, is safe and nontoxic, and can be directly eaten or drunk after being soaked in water. Researches show that the cactus fruit extract contains abundant haematochrome, polysaccharide, flavone, pectin and other components, and has the effects of clearing away heat and toxic materials, improving immunity, resisting tumors, reducing blood pressure and blood sugar, scavenging free radicals and the like.
At present, more research reports on cactus in China are provided, the research on the related aspects of cactus fruit polysaccharide and haematochrome is mainly focused, and the research, development and utilization of cactus fruit seeds are less. Researches show that the prickly pear seed oil contains rich tocopherol and essential fatty acid, and has outstanding effects of restructuring skin tissues, repairing collagen and resisting aging. Therefore, if the seeds of the cactus fruit can be fully utilized, the health care function of the cactus fruit can be fully exerted while the local economy can be promoted.
The existing methods for extracting the prickly pear seed oil comprise a Soxhlet extraction method, a chloroform-methanol extraction method and an ultrasonic-assisted n-hexane extraction method. The soxhlet extraction method has the advantages that the oil extraction rate is highest, the obtained prickly pear seed oil has high linoleic acid content, but the time consumption is longer, and the product has serious solvent residue; the chloroform-methanol extraction method and the ultrasonic-assisted n-hexane extraction method have no obvious difference in oil extraction rate and linoleic acid content. Therefore, an extraction process of the prickly pear seed oil, which is simple in operation, short in extraction time and high in oil extraction rate, is urgently needed, and provides a certain theoretical basis and scientific basis for further development and utilization of the prickly pear seed oil.
Disclosure of Invention
In view of the above, the invention provides an ultrasonic-assisted cactus fruit seed oil extraction process.
The technical scheme adopted by the invention for solving the technical problems is as follows:
an ultrasonic-assisted cactus fruit seed oil extraction process comprises the following steps:
(1) pretreatment of raw materials: oven drying Opuntia Dillenii fruit seed, cooling, pulverizing, and sieving to obtain Opuntia Dillenii fruit seed powder;
(2) extraction: mixing cactus fruit seed powder and petroleum ether according to a material-liquid ratio of 1: (6-12) carrying out ultrasonic treatment after mixing in g/mL for 30-90 min for 1-3 times;
(3) concentration: and (3) merging the sample liquids subjected to ultrasonic treatment in the step (2), carrying out suction filtration to obtain a supernatant, and placing the supernatant into a rotary evaporator for evaporation and concentration to obtain the prickly pear seed oil.
Preferably, in the step (1), the cactus fruit seeds are placed in a forced air drying oven at 40 ℃ for drying for 24 hours, then cooled, crushed by a crusher and sieved by a 60-mesh sieve.
Preferably, in the step (2), the ratio of the cactus fruit seed powder to the petroleum ether is 1: mixing at 9g/mL, ultrasonic extracting for 30min for 3 times.
Preferably, in the step (3), the temperature of the concentrated water bath of the rotary evaporator is 40 ℃.
According to the technical scheme, the cactus fruit seed oil is taken as a raw material, the raw material is pretreated, the ultrasonic technology is adopted for extracting the cactus fruit seed oil in an auxiliary mode, the release of active substances in cells is accelerated by utilizing the cavitation of ultrasonic waves and coupling heat energy and mechanical effect, the extraction time is shortened, the extraction rate is improved, and the extraction process disclosed by the invention is proved to be high in extraction rate of the cactus fruit seed oil, which reaches 11.3% through single-factor tests and orthogonal tests. The extraction process is simple and feasible, the extraction time is short, the extraction rate is high, a certain theoretical basis and scientific basis are provided for further development and utilization of the prickly pear seed oil, and the prickly pear seed oil is worthy of application and popularization.
Drawings
FIG. 1 is a graph showing the effect of extraction solvent on the extraction rate of prickly pear seed oil.
Fig. 2 is a graph showing the effect of feed liquid ratio on cactus fruit seed oil extraction rate.
Fig. 3 is a graph of the effect of extraction time on the extraction rate of prickly pear seed oil.
Fig. 4 is a graph showing the effect of extraction times on the extraction rate of prickly pear seed oil.
Detailed Description
The technical solutions and effects of the embodiments of the present invention will be further described in detail below with reference to the accompanying drawings of the present invention.
The invention provides an ultrasonic-assisted cactus fruit seed oil extraction process, which comprises the following specific extraction processes and experiments:
an ultrasonic-assisted cactus fruit seed oil extraction process comprises the following steps:
(1) pretreatment of raw materials: oven drying Opuntia Dillenii fruit seed, cooling, pulverizing, and sieving to obtain Opuntia Dillenii fruit seed powder;
(2) extraction: mixing cactus fruit seed powder and petroleum ether according to a material-liquid ratio of 1: (6-12) carrying out ultrasonic treatment after mixing in g/mL for 30-90 min, wherein the extraction times are 1-3. The ultrasonic wave is used to generate high-speed and strong cavitation effect and stirring effect to destroy the cactus fruit seed cells, increase the solvent penetration force, enable petroleum ether to permeate into the cells, improve the dissolution speed and dissolution times of the fruit seed oil, and shorten the extraction time.
(3) Concentration: and (3) merging the sample liquids subjected to ultrasonic treatment in the step (2), carrying out suction filtration to obtain a supernatant, and placing the supernatant into a rotary evaporator for evaporation and concentration to obtain the prickly pear seed oil.
Further, in the step (1), the cactus fruit seeds are placed in a forced air drying oven at 40 ℃ for drying for 24 hours, then cooled, crushed by a crusher and sieved by a 60-mesh sieve.
Further, in the step (2), the cactus fruit seed powder and the petroleum ether are mixed according to the ratio of material to liquid of 1: mixing at 9g/mL, ultrasonic extracting for 30min for 3 times.
Further, in the step (3), the temperature of the rotary evaporator is 40 ℃.
In order to determine the extraction conditions of the cactus fruit seed oil, the following verification tests were performed:
1. single factor test
1) Determination of extraction solvent: drying Opuntia Dillenii fruit seeds in 40 deg.C forced air drying oven for 24 hr, taking out, cooling, pulverizing, sieving with 60 mesh sieve to obtain Opuntia Dillenii fruit seed powder, weighing, sealing, and storing. Accurately weighing 5.0g of cactus fruit seed powder, carrying out ultrasonic treatment on the cactus fruit seed powder and different extraction solvents (petroleum ether, ethyl acetate, n-hexane and dichloromethane) according to the material-liquid ratio of 1 (3-15) g/mL, ultrasonic extraction time of 30-150 min and extraction frequency of 1-5 times, carrying out suction filtration on sample liquid after ultrasonic treatment to obtain supernatant, carrying out rotary evaporation concentration at 40 ℃ to obtain cactus fruit seed oil, weighing and calculating the oil extraction rate of the cactus fruit seeds. The data are the average of 3 replicates. The results are shown in fig. 1, the influence of different extraction solvents on the extraction rate of the prickly pear seed oil is different, wherein the extraction rate of the prickly pear seed oil is the lowest when dichloromethane is used as the extraction solvent; when the petroleum ether is used as an extraction solvent, the extraction rate of the cactus fruit seed oil is the highest. And (4) comprehensively considering test results and price factors, and selecting petroleum ether as an extraction solvent of the prickly pear seed oil.
2) Determination of the feed-to-liquid ratio
Weighing 5.0g of cactus fruit seed powder, respectively placing the cactus fruit seed powder into conical flasks, respectively extracting with petroleum ether as an extraction solvent at a material-liquid ratio of 1:3, 1:6, 1:9, 1:12 and 1:15(g/mL) under the conditions of ultrasonic extraction time of 30min and extraction frequency of 1 time, respectively, filtering the sample liquid after ultrasonic treatment to obtain a supernatant, concentrating the supernatant with a rotary evaporator at 40 ℃ to obtain cactus fruit seed oil, weighing and calculating the oil extraction rate of the cactus fruit seed. The results are shown in fig. 2, the extraction effect of the prickly pear seed oil tends to decrease first, then increase, then decrease and then increase with the increase of the feed-liquid ratio, and the extraction rate is the highest when the feed-liquid ratio is 1:9 (g/mL). With the increase of the solvent content, solute is continuously separated out from the raw material, when the ratio of the material to the liquid reaches 1:9(g/mL), the solute is separated out to the highest level, and the solvent is continuously increased to separate out various impurities in the raw material, so that the extraction rate of the cactus fruit seed oil is reduced. In addition, when the content of the prickly pear seed oil is constant, the concentration of the prickly pear seed oil in the solution is reduced due to the increase of the volume of the solvent, so that the extraction rate is reduced. Therefore, a feed-to-liquid ratio of 1:9(g/mL) was chosen.
3) Determination of ultrasound extraction time
Weighing 5.0g of cactus fruit seed powder, respectively placing into conical flasks, respectively extracting for 30min, 60 min, 90min, 120 min and 150min by using petroleum ether as an extraction solvent under the conditions that the material-liquid ratio is 1:9(g/mL) and the extraction frequency is 1, performing suction filtration on sample liquid after ultrasonic treatment to obtain supernatant, concentrating by using a rotary evaporator at 40 ℃ to obtain cactus fruit seed oil, weighing and calculating the oil extraction rate of the cactus fruit seeds. The results are shown in fig. 3, where the extraction rate of the prickly pear seed oil reaches the highest when the ultrasonic extraction time is 30min, and the prickly pear seed oil is basically and completely extracted. The ultrasonic treatment time is too long, which may cause the damage of the seed oil structure of the cactus, and meanwhile, the seed oil of the cactus is easy to be oxidized in the air after being exposed for a long time, so that the extraction rate is reduced. And the ultrasonic treatment is carried out for a long time, so that the energy consumption is increased, the extraction period is prolonged, and the extraction cost is increased, therefore, 30min is the optimal ultrasonic extraction time.
4) Determination of the number of extractions
Weighing 5.0g of cactus fruit seed powder, respectively placing 5 parts of cactus fruit seed powder in conical flasks, respectively extracting for 1 time, 2 times, 3 times, 4 times and 5 times by using petroleum ether as an extraction solvent under the extraction conditions that the material-liquid ratio is 1:9(g/mL) and the ultrasonic extraction time is 30min, filtering sample liquid after ultrasonic treatment to obtain supernate, concentrating by using a rotary evaporator at 40 ℃ to obtain cactus fruit seed oil, weighing and calculating the oil extraction rate of the cactus fruit seed. The result is shown in fig. 4, the extraction effect of the prickly pear seed oil is increased along with the increase of the extraction times, the extraction times are 1-2 times, the extraction rate of the prickly pear seed oil is obviously increased along with the increase of the extraction times, and after the extraction times exceed 2 times, the increase range of the extraction rate of the prickly pear seed oil tends to be relatively gentle. Considering the factors of saving cost, working efficiency and the like, the extraction times are determined to be 2 times.
2. In order to determine the optimal extraction process of the prickly pear seed oil, an orthogonal test was performed:
1) orthogonal test optimization of cactus fruit seed oil extraction process
On the basis of a single-factor test, a four-factor three-level orthogonal test is carried out on an extraction solvent, a material-liquid ratio, ultrasonic extraction time and extraction times, and an optimal process is selected, wherein the factor levels are shown in table 1:
TABLE 1 orthogonal test L9(34) Factor level meter
TABLE 2 visual analysis of orthogonal test results
TABLE 3 analysis of variance of results for each factor
Note: -means no significant difference, P > 0.05.
Table 2 is an intuitive analysis of the results of the orthogonal test, and table 3 is an analysis of variance of the results of each factor. As shown in table 3, the F test results showed that none of the 4 factors had a significant effect on the extraction yield of the prickly pear seed oil. The reason for this may be that the test error is too large and the error freedom is small (only 2), so that the sensitivity of the test is low, thereby masking the significance of the factors to be examined. Since the influence of each factor on the extraction rate is not significant, multiple comparisons between the levels of each factor are not necessary. Direct visual analysis can be performed. The visual analysis method is also called a range analysis method, the main status, the secondary status and the optimal level of each factor are determined by comparing the range of the level of each factor, and the larger the range is, the larger the influence on the extraction rate of the prickly pear seed oil is. As can be seen from Table 2, the primary and secondary sequence of the influence of the factors on the extraction rate in the ultrasonic-assisted extraction method is as follows: the extraction times (D) > the ultrasonic extraction time (C) > the extraction solvent (A) > the material-liquid ratio (B), and the optimal extraction process parameters are A1B2C1D3Namely extracting solvent petroleum ether with the ratio of material to liquid of 1:9(g/ml) and carrying out ultrasonic extraction for time30min, and 3 times of extraction.
2) Carrying out a verification test according to the optimal process conditions: weighing 5.0g of cactus fruit seed powder, respectively placing 3 parts of the cactus fruit seed powder into conical flasks, extracting for 30min by using petroleum ether as an extraction solvent under the conditions that the material-liquid ratio is 1:9(g/mL) and the extraction frequency is 3 times, performing suction filtration on sample liquid after ultrasonic treatment to obtain supernatant, concentrating by using a rotary evaporator at 40 ℃ to obtain cactus fruit seed oil, weighing and calculating the oil extraction rate of the cactus fruit seed. The average extraction rate of the prickly pear seed oil is 11.3% after 3 times of parallel tests. Compared with the result of an optimal group of orthogonal tests, the extraction rate is increased by 10.8%, and is 4.34% higher than the extraction rate (6.96%) of ultrasonic-assisted n-hexane reported in other documents, so that reference is provided for the industrial production of the prickly pear seed oil in the future.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (4)
1. An ultrasonic-assisted cactus fruit seed oil extraction process is characterized in that: the method comprises the following steps:
(1) pretreatment of raw materials: oven drying Opuntia Dillenii fruit seed, cooling, pulverizing, and sieving to obtain Opuntia Dillenii fruit seed powder;
(2) extraction: mixing cactus fruit seed powder and petroleum ether according to a material-liquid ratio of 1: (6-12) carrying out ultrasonic treatment after mixing in g/mL for 30-90 min, wherein the extraction times are 1-3;
(3) concentration: and (3) merging the sample liquids subjected to ultrasonic treatment in the step (2), carrying out suction filtration to obtain a supernatant, and placing the supernatant into a rotary evaporator for evaporation and concentration to obtain the prickly pear seed oil.
2. The ultrasound-assisted opuntia ficus-indica seed oil extraction process of claim 1, wherein: in the step (1), the cactus fruit seeds are placed in a 40 ℃ forced air drying oven to be dried for 24 hours and then cooled, and are crushed by a crusher and sieved by a 60-mesh sieve.
3. The ultrasound-assisted opuntia ficus-indica seed oil extraction process of claim 1, wherein: in the step (2), the ratio of the cactus fruit seed powder to the petroleum ether is 1: mixing at 9g/mL, ultrasonic extracting for 30min for 3 times.
4. The ultrasound-assisted opuntia ficus-indica seed oil extraction process of claim 1, wherein: in the step (3), the temperature of the concentrated water bath of the rotary evaporator is 40 ℃.
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| CN1810945A (en) * | 2006-02-23 | 2006-08-02 | 陕西科技大学 | Kiwi seed oil extracting process |
| CN101411363A (en) * | 2008-11-21 | 2009-04-22 | 辽宁今日农业有限公司 | Raspberry seed oil product and extraction method |
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