CN112831368A - Preparation method of cyperus esculentus oil - Google Patents
Preparation method of cyperus esculentus oil Download PDFInfo
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- CN112831368A CN112831368A CN202110017658.3A CN202110017658A CN112831368A CN 112831368 A CN112831368 A CN 112831368A CN 202110017658 A CN202110017658 A CN 202110017658A CN 112831368 A CN112831368 A CN 112831368A
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Classifications
-
- 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
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
-
- 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
- C11B1/104—Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation method of cyperus esculentus oil, which belongs to the technical field of oil processing and preparation and comprises the following steps: carrying out microwave drying and crushing on the cyperus esculentus, and carrying out supercritical carbon dioxide extraction on the obtained cyperus esculentus powder to obtain cyperus esculentus oil; according to the invention, the cyperus esculentus oil is extracted by adopting a supercritical carbon dioxide fluid extraction method, so that on the premise of ensuring the extraction rate, the nutrient substances in the cyperus esculentus oil can be better protected, and the oil quality is improved; the cyperus esculentus is dried by a microwave drying method, so that the cyperus esculentus can be uniformly and rapidly heated, the cell wall of the cyperus esculentus can be embrittled and broken while the cyperus esculentus is dried, the mass transfer diffusion and dissolution capacity of substances in cells can be improved, the oil extraction can be further promoted, and the extraction rate of the cyperus esculentus oil can be improved.
Description
Technical Field
The invention belongs to the technical field of oil processing and preparation, and particularly relates to a preparation method of cyperus esculentus oil.
Background
Cyperus esculentus L belongs to angiosperms, monocotyledonous plants, Cyperaceae (Cyperaceae) Cyperus (Cyperus) perennial herbaceous plants of Cyperus order, Cyperus, also named as Tiger nut, iron water chestnut, Cyperus, etc. The compendium of Xinhua materia Medica is recorded: the cyperus esculentus is warm, sweet and pungent in nature, contains functional components such as vitamin E and sterol, and has the effects of strengthening spleen and stomach, soothing liver and promoting qi circulation and the like. The fat content of the cyperus esculentus is about 25 percent, the unsaturated fatty acid accounts for more than 80 percent of the total fatty acid, and the oleic acid content is taken as the main content. The Cyperus esculentus oil also contains nutrients such as vitamin E and phytosterol. In recent years, studies on cyperus esculentus mainly focus on cyperus esculentus oil, extraction methods of the cyperus esculentus mainly include a squeezing method, a solvent extraction method, an aqueous enzymatic method and the like, and the extraction rate of the cyperus esculentus oil is 70-85%. The existing extraction method has the common defects of low extraction rate, poor quality of extracted oil, difficult comprehensive utilization of byproducts, easy generation of waste gas and pollution of waste residue to the environment, and incapability of well ensuring nutrient substances in the cyperus esculentus oil.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation method of cyperus esculentus oil, which adopts a microwave drying and supercritical carbon dioxide extraction technology to remarkably improve the extraction rate and the grease quality of the cyperus esculentus oil.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of cyperus esculentus oil comprises the following steps:
and carrying out microwave drying and crushing on the cyperus esculentus, and carrying out supercritical carbon dioxide extraction on the obtained cyperus esculentus powder to obtain the cyperus esculentus oil.
Further, before the cyperus esculentus is subjected to microwave drying, the method also comprises the operation of cleaning and removing impurities from the cyperus esculentus.
Further, the microwave drying is carried out until the water content of the cyperus esculentus is less than or equal to 5 wt%, and the cyperus esculentus is crushed to 40-80 meshes.
Further, the powder was pulverized to 60 mesh.
Furthermore, the microwave drying is in a sectional type, the intermittent operation is carried out for 3-5 min after every 3-5 min of microwave, and the microwave power is 300-500W.
Further, the pressure of the supercritical carbon dioxide extraction is 20-30 MPa, the temperature is 40-50 ℃, and the time is 120-200 min.
Further, the pressure of the supercritical carbon dioxide extraction is 25MPa, the temperature is 45 ℃, and the time is 180 min.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention adopts a supercritical carbon dioxide fluid extraction method (SFE-CO)2) The cyperus esculentus oil is extracted, so that the nutrient substances in the cyperus esculentus oil can be better protected and the oil quality is improved on the premise of ensuring the extraction rate.
(2) The method adopts a microwave drying method to dry the cyperus esculentus, so that the cyperus esculentus can be uniformly and rapidly heated, has non-thermal effect, quick mass transfer, time saving and no pollution, can embrittle and break the cell wall of the cyperus esculentus while drying, improves the mass transfer diffusion and dissolution capacity of substances in cells, further promotes oil extraction, and improves the extraction rate of the cyperus esculentus oil.
(3) The method is convenient to operate, high in safety, free of organic solvent residues, free of influence on byproducts, capable of improving the comprehensive utilization rate of the cyperus esculentus, and significant in realizing green industrial production of the cyperus esculentus oil and comprehensive utilization of the byproducts.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a graph of the extraction pressure as a function of the extraction yield of Cyperus esculentus oil in example 3;
FIG. 2 is a graph of the extraction temperature as a function of the extraction yield of Cyperus esculentus oil in example 3;
FIG. 3 is a graph of the extraction time versus the extraction yield of Cyperus esculentus oil in example 3;
FIG. 4 is a graph of the particle size of the material in example 3 as a function of the extraction yield of Cyperus esculentus oil.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention. It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The description and examples are intended to be illustrative only.
Example 1
The preparation method of the cyperus esculentus powder comprises the following steps:
(1) cleaning and impurity removing of cyperus esculentus: putting the cyperus esculentus in a clean container, enabling clear water to sink the surface of the cyperus esculentus, removing weeds, root hairs and shriveled cyperus esculentus on the upper layer, rinsing the cyperus esculentus with clear water for more than three times to remove soil until the rinsed water is not turbid, manually picking out hard impurities such as stones and the like, finally manually rubbing and washing the cyperus esculentus for three times to enable the cleanliness to be more than 99%, and draining water;
(2) carrying out microwave drying treatment on the cyperus esculentus drained in the step (1), and carrying out sectional type microwave drying, wherein the microwave power is 300W, stopping for 3min after the microwave is carried out for 3min, so that the cell wall is broken, most of water is removed, and stopping the drying treatment when the water content reaches 5 wt%;
(3) and (3) crushing the cyperus esculentus dried in the step (2) by using a high-speed crusher, and sieving the crushed cyperus esculentus by using a 60-mesh sieve to obtain cyperus esculentus powder.
Example 2
Preparing cyperus esculentus powder:
(1) cleaning and impurity removing of cyperus esculentus: putting the cyperus esculentus in a clean container, enabling clear water to sink the surface of the cyperus esculentus, removing weeds, root hairs and shriveled cyperus esculentus on the upper layer, rinsing the cyperus esculentus with clear water for more than three times to remove soil until the rinsed water is not turbid, manually picking out hard impurities such as stones and the like, finally manually rubbing and washing the cyperus esculentus for three times to enable the cleanliness to be more than 99%, and draining water;
(2) carrying out microwave drying treatment on the cyperus esculentus drained in the step (1), and carrying out sectional type microwave drying with the microwave power of 500W, stopping for 5min after the microwave is 5min to break cell walls and remove most of water, and stopping the drying treatment when the water content is 5 wt%;
(3) and (3) crushing the cyperus esculentus dried in the step (2) by using a high-speed crusher, and sieving the crushed cyperus esculentus by using a 60-mesh sieve to obtain cyperus esculentus powder.
Example 3
The single-factor experiment researches the influence factors of the extraction rate of the cyperus esculentus oil, and the calculation method of the extraction rate of the cyperus esculentus oil comprises the following steps:
wherein W is the oil extraction rate,%, M is the fat content before oil extraction,%, and M is the fat content after oil extraction,%.
1. Investigation of extraction pressure
Weighing 400g of cyperus esculentus powder prepared in example 1, putting into a 2L extraction kettle, checking the airtightness of the device, and opening CO2And (3) opening and closing the gas cylinder, starting the main power supply, the refrigerating device and the heating device, setting the temperature to be 45 ℃, opening the air release valve to balance the pressure of the whole passage of the device, and closing the air release valve. Starting a high-pressure pump to enable the pressure of an extraction kettle to be 15MPa, 20MPa, 25MPa and 30MPa respectively, adjusting the flow, starting extraction timing, closing the high-pressure pump, a refrigerating device and a heating device after extraction is carried out for 180min, adjusting all gas valves to balance the pressure of a passage, closing all the gas valves, evacuating the gas of the extraction kettle, taking out cyperus bean pulp in the extraction kettle, collecting materials of a separation kettle, closing a main power supply to obtain cyperus bean oil, and drawing by using the extraction pressure-extraction rate of the cyperus bean oil as shown in figure 1. As can be seen from fig. 1, the extraction pressure is an important factor affecting the extraction of cyperus bean oil, and it can be seen that the extraction rate of cyperus bean oil is significantly improved with the increase of the pressure at 15-25 MPa; after 25MPa, the extraction rate of the cyperus esculentus oil is increased less, and the influence on the extraction rate is small. This is because with increasing pressure, CO2The density of the cyperus esculentus is increased, the dissolving capacity is enhanced, the mass transfer rate is increased, the substance dissolving performance is rapidly increased, and the extraction rate of the cyperus esculentus oil is increased; when the pressure is too high, the fluid density is too high, possibly for CO2The effect of the increased fluid solubility is less, so that the extraction yield does not vary much. Meanwhile, the cost is increased due to the fact that the extraction pressure is too large, the service life of equipment is influenced, and potential safety hazards are increased due to the fact that the pressure is large. And comprehensively considering the extraction pressure of 20-30 MPa to optimize the orthogonal process.
2. Investigation of extraction temperature
Weighing 400g of cyperus esculentus powder prepared in example 1, putting into a 2L extraction kettle, checking the airtightness of the device, and opening CO2And opening a gas cylinder switch, starting a main power supply, a refrigerating device and a heating device, setting the extraction temperatures to be 35 ℃, 40 ℃, 45 ℃, 50 ℃ and 55 ℃, respectively, opening a gas release valve to balance the pressure of the whole passage of the device, and closing the gas release valve. Starting a high-pressure pump to enable the pressure of an extraction kettle to be 25MPa, adjusting the flow, starting extraction timing, closing the high-pressure pump, a refrigerating device and a heating device after extraction is carried out for 180min, adjusting all gas valves to enable the pressure of a passage to be balanced, closing all the gas valves, emptying gas in the extraction kettle, taking out cyperus bean pulp in the extraction kettle, collecting and dividing the cyperus bean pulpSeparating the substances from the kettle, turning off the main power supply to obtain Cyperus esculentus oil, and plotting the extraction temperature-the extraction rate of the Cyperus esculentus oil as shown in FIG. 2. As can be seen from FIG. 2, the supercritical extraction equipment extracts the substances, the temperature has important influence on the substances, and the temperature has important influence on the supercritical CO2The dissolving capacity of the composite has double-sided influence, on one hand, the temperature rise can increase the diffusion speed of the composite, and the solubility of the composite is increased; on the other hand, if the temperature is too high, CO will be generated2The density of the fluid decreases and the dissolving capacity decreases. As can be seen from fig. 2, the extraction rate of cyperus esculentus oil increases with increasing temperature when the extraction temperature is 35 to 50 c, and the extraction rate is maximum at 50 c, followed by a downward trend. This is because the temperature is 35 ℃ to 50 ℃ for CO2The density of the fluid has little influence, the influence on the thermal motion of molecules and the vapor pressure of an extract is large, the mass transfer speed is accelerated, the solubility of the supercritical CO is increased, and the supercritical CO is further increased2The effective contact with the extraction components increases the extraction rate; supercritical CO when the extraction temperature is higher than 50 deg.C2The density of the fluid is reduced, the mass transfer rate, the diffusion coefficient and the capability of carrying substances are all reduced, and the extraction rate is reduced. This indicates that the temperature is influenced by the supercritical CO2The extraction rate is influenced by the density and the material vapor pressure, and the optimization test is carried out at 40-50 ℃ in consideration of energy consumption and protection of nutrient substances such as phytosterol, vitamin E and the like in the cyperus esculentus.
3. Investigation of extraction time
Weighing 400g of cyperus esculentus powder prepared in example 1, putting into a 2L extraction kettle, checking the airtightness of the device, and opening CO2And (3) opening and closing the gas cylinder, starting the main power supply, the refrigerating device and the heating device, setting the extraction temperature to be 45 ℃, opening a gas release valve to balance the pressure of the whole passage of the device, and closing the gas release valve. Starting a high-pressure pump to enable the pressure of an extraction kettle to be 25MPa, adjusting the flow, starting extraction timing, wherein the extraction time is respectively 60min, 90min, 120min, 150min and 180min, closing the high-pressure pump, a refrigerating device and a heating device after extraction is finished, adjusting each gas valve to enable the pressure of a passage to be balanced, closing all the gas valves, exhausting gas of the extraction kettle, taking out cyperus bean pulp in the extraction kettle, collecting separation kettle substances, and closing a main power supply to obtain cyperus bean oilAs shown in FIG. 3, it can be seen from FIG. 3 that the extraction rate increases with time in the whole single-factor extraction time, and increases greatly in 90-150 min, but increases slowly in 150-210 min, with little difference. The reason is that along with the extension of the extraction time, the mass transfer rate is firstly expanded at a constant speed to enable the extraction rate to rise faster, and then the mass transfer peak extraction rate is gradually and stably reached, at the moment, the effect of continuously increasing the extraction time on the extraction efficiency of the cyperus esculentus oil is not obvious, the cost is increased due to the extension of the extraction time, and the quality of the cyperus esculentus oil is influenced. Therefore, 120-180 min is selected for orthogonal test.
4. Investigation of material particle size
Cyperus esculentus powder was prepared according to the method of example 1, wherein in step (3), after the Cyperus esculentus was pulverized, the pulverized Cyperus esculentus was passed through 40 mesh, 60 mesh, 80 mesh and 100 mesh sieves, respectively, to obtain Cyperus esculentus powders with different mesh numbers, 400g of the above Cyperus esculentus powders were weighed, respectively, put into a 2L extraction vessel, the airtightness of the apparatus was checked, and CO was turned on2And (3) opening and closing the gas cylinder, starting the main power supply, the refrigerating device and the heating device, setting the extraction temperature to be 45 ℃, opening a gas release valve to balance the pressure of the whole passage of the device, and closing the gas release valve. Starting a high-pressure pump to enable the pressure of an extraction kettle to be 25MPa, adjusting the flow, starting extraction timing, wherein the extraction time is 180min, closing the high-pressure pump, a refrigerating device and a heating device after extraction is finished, adjusting all gas valves to enable the pressure of a passage to be balanced, closing all the gas valves, evacuating the gas of the extraction kettle, taking out cyperus bean pulp in the extraction kettle, collecting materials of the separation kettle, closing a main power supply to obtain cyperus bean oil, and drawing a graph by using the granularity of the materials and the extraction rate of the cyperus bean oil, wherein as shown in figure 4, the extraction rate of the oil can be influenced by the oversize or undersize of the materials. As can be seen from fig. 4, the extraction rate of the cyperus esculentus oil increases and then decreases as the particle size of the material increases from 40 mesh to 100 mesh, and the extraction rate of the cyperus esculentus oil is highest when the particle size of the material is 60 mesh. When the sieving mesh number is smaller, the material granularity is larger, more large-particle materials containing the cyperus esculentus peels can be generated, and CO is increased2The dissolution time of the fluid reduces the extraction efficiency; the particle size of the material gradually decreases along with the increase of the sieving mesh number of the material, and CO is increased2Fluid and nutletThe contact area and the mass transfer rate of the bean flour are increased, so that the extraction rate of the cyperus esculentus oil is increased; however, when the particle size is too small, the material is easy to block the material plate, channeling occurs, the bulk density of the raw material is increased, the mass transfer resistance is increased, and the oil extraction rate is reduced. Meanwhile, the selection of a larger screening mesh also consumes a lot of time, so that the orthogonal test optimization is performed by selecting 40-80 meshes.
Example 4
Orthogonal experiment optimization of supercritical CO2Process for extracting cyperus bean oil
On the basis of a single-factor test, the extraction pressure (A), the extraction temperature (B), the extraction time (C) and the material granularity (D) are selected as influencing factors, the extraction rate of the cyperus esculentus oil is taken as a reference index, and L is adopted9(34) Orthogonal experimental design, optimizing supercritical CO2A process for extracting cyperus bean oil. Each set of experiments was repeated 3 times and the levels of orthogonal test factors are shown in table 1.
TABLE 1
The results of the orthogonality test are shown in table 2.
TABLE 2
The results of the analysis of variance in the orthogonal test are shown in Table 3.
TABLE 3
| Source of variation | Sum of squares of type III | Degree of freedom | Mean square | F | Significance of |
| A pressure of extraction | 1515.759 | 2 | 757.880 | 963.815 | ** |
| B temperature of extraction | 6.330 | 2 | 3.165 | 4.025 | * |
| C extraction time | 389.829 | 2 | 194.915 | 247.878 | ** |
| Particle size of D material | 12.154 | 2 | 6077 | 7.728 | * |
| Error of the measurement | 7.077 | 9 | 0.786 | ||
| Total variation | 1931.150 | 17 |
Note: *. has obvious difference, P is less than 0.05; marked difference, P < 0.01
According to the results of the orthogonal test and the analysis of the range table, the factors influencing the extraction rate of the cyperus esculentus oil are ranked as follows: a (extraction pressure)>C (extraction time)>D (particle size of material)>B (extraction temperature). As is clear from the results of the anova in Table 3, the extraction pressure and the extraction time are very significant factors (P)<0.01), the extraction temperature and the material granularity are significant factors (P)<0.05), which is consistent with the results of the range analysis. The most preferred combination is A2B2C3D2And the particle size of the material is not in the orthogonal test table (table 2), namely the particle size of the material is 60 meshes, the extraction pressure is 25MPa, the extraction temperature is 45 ℃, and the extraction time is 180 min. The optimum combination was tested in 3 validation trials and the extraction of cyperus esculentus oil was 94.76%.
Comparative example 1
Preparation of cyperus esculentus oil:
(1) cleaning and impurity removing of cyperus esculentus: putting the cyperus esculentus in a clean container, enabling clear water to sink the surface of the cyperus esculentus, removing weeds, root hairs and shriveled cyperus esculentus on the upper layer, rinsing the cyperus esculentus with clear water for more than three times to remove soil until the rinsed water is not turbid, manually picking out hard impurities such as stones and the like, finally manually rubbing and washing the cyperus esculentus for three times to enable the cleanliness to be more than 99%, and draining water;
(2) carrying out infrared drying treatment on the cyperus esculentus drained in the step (1), and stopping the drying treatment when the moisture content of the cyperus esculentus reaches 5 wt%;
(3) crushing the cyperus esculentus dried in the step (2) by using a high-speed crusher, and sieving the crushed cyperus esculentus by using a 60-mesh sieve to obtain cyperus esculentus powder;
(4) weighing 400g of cyperus esculentus powder prepared in the step (3), putting into a 2L extraction kettle, checking the air tightness of the device, and opening CO2And (3) opening and closing the gas cylinder, starting the main power supply, the refrigerating device and the heating device, setting the temperature to be 45 ℃, opening the air release valve to balance the pressure of the whole passage of the device, and closing the air release valve. Starting a high-pressure pump to enable the pressure of an extraction kettle to be 25MPa, adjusting the flow, starting extraction timing, closing the high-pressure pump, a refrigerating device and a heating device after extraction is carried out for 180min, adjusting all gas valves to enable the pressure of a passage to be balanced, closing all the gas valves, emptying gas in the extraction kettle, taking out cyperus bean pulp in the extraction kettle, collecting substances in the separation kettle, closing a main power supply to obtain cyperus bean oil, and determining that the extraction rate of the cyperus bean oil is 78.75%.
Comparative example 2
The difference from comparative example 1 is that the infrared drying in step (2) was replaced by continuous microwave drying. The comparative example was found to have an extraction rate of 76.21% for cyperus esculentus oil.
Comparative example 3
The difference from comparative example 1 is that the infrared drying in step (2) was replaced with hot air drying in which the temperature of hot air was 70 ℃. The comparative example was found to have an extraction of 79.59% for cyperus esculentus oil.
And (3) measuring the oil quality:
for A in example 42B2C3D2Physicochemical indices of Cyperus esculentus oil extracted under experimental conditions and Cyperus esculentus oil extracted in comparative examples 1-3The target was detected, and the detection method and the detection result are shown in tables 4 and 5, respectively.
TABLE 4
TABLE 5
For A in example 42B2C3D2The content of vitamin E, phytosterol and phospholipids in the cyperus esculentus oil extracted under the experimental conditions and the cyperus esculentus oil extracted in comparative examples 1-3 were determined, the determination method was as follows, and the determination results are shown in table 6.
Vitamin E assay
Reference is made to GB/T26635-2011 high performance liquid chromatography for measuring contents of animal and vegetable oil tocopherol and tocotrienol. Accurately weighing 0.5g (accurate to 0.0001g) of cyperus esculentus oil and a 10ml volumetric flask, dissolving n-hexane, fixing the volume, shaking up and measuring.
High performance liquid chromatography conditions: column, HPLC NH2(4.6mm x 250mm, 5.0 μm); a detector, a fluorescence detector; mobile phase, n-hexane: isopropanol (9: 1); column temperature, 40 ℃; 0.8 ml/min; the excitation wavelength is 298nm, and the emission wavelength is 325 nm; 10 μ L.
Phytosterol assay
Extracting unsaponifiable matters of the grease: refer to the hexane extraction method in the national standard GB/T5535.2-2008.
And drawing a standard curve by taking the stigmasterol content as an abscissa and the absorbance value as an ordinate. The obtained unsaponifiable matter is dissolved by absolute ethyl alcohol, the volume is determined to be 25mL, and the unsaponifiable matter is diluted to be proper concentration for determination. And (3) putting 2mL of sample solution into a clean test tube, respectively adding 2mL of absolute ethyl alcohol and 2mL of phosphorus-sulfur-iron color developing agent, oscillating and uniformly mixing, standing for 15min, and then determining the absorbance of the reaction system at the 520nm position.
Phospholipid content
And the measurement is carried out by a molybdenum blue colorimetric method according to the first method of GB/T5537-2008 'measurement of phospholipid content in grain and oil inspection'.
TABLE 6
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (7)
1. The preparation method of the cyperus esculentus oil is characterized by comprising the following steps:
and carrying out microwave drying and crushing on the cyperus esculentus, and carrying out supercritical carbon dioxide extraction on the obtained cyperus esculentus powder to obtain the cyperus esculentus oil.
2. The method according to claim 1, wherein the method further comprises cleaning the cyperus esculentus to remove impurities before the cyperus esculentus is subjected to microwave drying.
3. The preparation method according to claim 1, wherein the microwave drying is performed until the water content of the cyperus esculentus is less than or equal to 5 wt%, and the crushing is performed to 40-80 meshes.
4. The method of claim 3, wherein the pulverizing is to 60 mesh.
5. The preparation method according to claim 1, wherein the microwave drying is segmented, the microwave drying is interrupted for 3-5 min after every 3-5 min of microwave, and the microwave power is 300-500W.
6. The preparation method according to claim 1, wherein the supercritical carbon dioxide extraction is performed at a pressure of 20 to 30MPa, a temperature of 40 to 50 ℃ and a time of 120 to 200 min.
7. The method according to claim 6, wherein the supercritical carbon dioxide extraction is carried out at a pressure of 25MPa and a temperature of 45 ℃ for 180 min.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20130070079A (en) * | 2011-12-19 | 2013-06-27 | 씨제이제일제당 (주) | Method for manufacturing soybean oil using supercritical extracting, and the soybean oil |
| CN103484238A (en) * | 2013-10-18 | 2014-01-01 | 长春大学 | Method for extracting cibora jadalna oil by supercritical carbon dioxide |
| JP2015168718A (en) * | 2014-03-05 | 2015-09-28 | 一般財団法人電力中央研究所 | Method for extracting grease |
| CN105602719A (en) * | 2016-03-14 | 2016-05-25 | 广州绿和缘生物科技有限公司 | Supercritical extraction method of tea oil |
| CN105838500A (en) * | 2016-06-08 | 2016-08-10 | 吉首大学 | Microwave-assisted supercritical carbon dioxide extraction method for okra seed oil |
-
2021
- 2021-01-07 CN CN202110017658.3A patent/CN112831368A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20130070079A (en) * | 2011-12-19 | 2013-06-27 | 씨제이제일제당 (주) | Method for manufacturing soybean oil using supercritical extracting, and the soybean oil |
| CN103484238A (en) * | 2013-10-18 | 2014-01-01 | 长春大学 | Method for extracting cibora jadalna oil by supercritical carbon dioxide |
| JP2015168718A (en) * | 2014-03-05 | 2015-09-28 | 一般財団法人電力中央研究所 | Method for extracting grease |
| CN105602719A (en) * | 2016-03-14 | 2016-05-25 | 广州绿和缘生物科技有限公司 | Supercritical extraction method of tea oil |
| CN105838500A (en) * | 2016-06-08 | 2016-08-10 | 吉首大学 | Microwave-assisted supercritical carbon dioxide extraction method for okra seed oil |
Non-Patent Citations (2)
| Title |
|---|
| 刘威等: "农产品微波干燥均匀性研究", 《干燥技术与设备》 * |
| 段蕾等: "响应面法优化超临界CO_2萃取油莎豆油及理化性质分析", 《食品工业》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113713423A (en) * | 2021-09-06 | 2021-11-30 | 长春大学 | Process for preparing black soya bean distillate oil by supercritical extraction and application |
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