CN107586605B - Comprehensive extraction method of oil, protein, aucubin and gutta-percha in eucommia seeds - Google Patents
Comprehensive extraction method of oil, protein, aucubin and gutta-percha in eucommia seeds Download PDFInfo
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Abstract
The invention discloses a comprehensive extraction method of grease, protein, aucubin and gutta-percha in eucommia seeds, which comprises the steps of taking eucommia seeds as raw materials, crushing the eucommia seeds, extruding, puffing and granulating by adopting a double-screw extrusion device, rolling by adopting a roller press after granulation, and then squeezing to obtain eucommia seed oil and cake pulp, washing the cake pulp with alcohol to obtain washing liquid and residue, eluting the washing liquid after being adsorbed by macroporous resin, concentrating in vacuum, and drying to obtain aucubin; extracting the residues with petroleum ether at the temperature of 60-90 ℃ to obtain an extracting solution and residues, and freezing and washing the extracting solution with acetone to obtain gutta-percha; extracting the residue with NaOH solution, and performing acid precipitation, vacuum concentration and drying treatment to obtain eucommia seed protein. Through the steps, the comprehensive extraction of 4 components of the grease, the protein, the aucubin and the gutta-percha in the eucommia seeds is realized, the resources are saved, and the added value of the product is improved.
Description
Technical Field
The invention belongs to the fields of food and chemical industry, and particularly relates to a comprehensive extraction method of grease, protein, aucubin and gutta-percha in eucommia seeds.
Background
Eucommia ulmoides is a single-genus plant of the family Eucommiaceae, is a unique and precious economic tree species in China, and is rich in chemical components including eucommia ulmoides seed oil, aucubin, gutta Percha, protein and the like. The effective components of the extract are extracted, and the extract has important significance for development and utilization of the extract.
The dissolution characteristics of various components in eucommia are different, and the current extraction method mostly extracts the components alone.
At present, methods such as a squeezing method, a solvent extraction method, a supercritical extraction method, a subcritical extraction method and the like exist for the eucommia seed oil, and the eucommia seed oil is contained in cells of seeds, so that the cells are damaged, oil is released, and the eucommia seed oil plays an important role in later-stage oil extraction. The oil residue after extraction of eucommia seeds also contains rich components such as gutta-percha, aucubin, protein and the like, and further extraction of the eucommia seed oil residue plays an important role in improving economic benefits. At present, there are some patents and documents for comprehensive extraction of chemical components in eucommia ulmoides. The chrysanthemum morifolium ramat carries out a comprehensive extraction process on oil and gutta-percha in eucommia seeds (the book of the Guiyang academy-Nature, 2011.1); the preparation method comprises the following steps of taking eucommia seed meal as a raw material, extracting aucubin by using an alcohol washing process, and preparing concentrated protein (Chinese oil 2017, 4); the chemical research institute of Chinese academy of sciences invented a method for efficiently, circularly and continuously extracting gutta-percha, eucommia seed oil, eucommia extract and eucommia resin from eucommia seeds (application number: CN 201110147426.6); the northwest agriculture and forestry science and technology university develops a method for extracting and separating eucommia seed oil and gutta-percha from eucommia key fruits (application number: CN 201410503740.7), but in the current report, a comprehensive extraction method is adopted to comprehensively extract 4 components of eucommia seed oil, aucubin, gutta-percha and protein, and the current report is not available.
Disclosure of Invention
Aiming at the defects of low yield and insufficient utilization of raw materials in the extraction of the components such as eucommia seed oil, eucommia ulmoides gum and the like at present, the invention provides a comprehensive extraction method of grease, protein, aucubin and eucommia ulmoides gum in eucommia ulmoides seeds, which realizes the comprehensive utilization of the raw materials, improves the economic benefit, reduces the emission and reduces the resource waste.
In order to solve the technical problems, the invention adopts the following technical scheme:
a comprehensive extraction method of oil, protein, aucubin and gutta-percha in eucommia seeds comprises the following steps:
(1) taking eucommia seeds as raw materials, crushing the eucommia seeds into 10-60 meshes, and then extruding, puffing and granulating by adopting a double-screw extrusion device;
(2) after granulation, rolling the blank by using a roller press until the thickness is less than 0.2-1.2 mm, then squeezing to obtain eucommia seed oil A and cake B;
(3) washing the cake B obtained after squeezing by using ethanol as an alcohol washing solvent to obtain a washing liquid C and a residue D;
(4) eluting the washing solution C after adopting macroporous resin for adsorption to obtain an eluent E, and concentrating and drying the eluent in vacuum to obtain aucubin F; extracting the residue D with petroleum ether at the temperature of 60-90 ℃ for 30-90 min to obtain an extracting solution G and a residue H;
(5) freezing the extracting solution G, separating out a precipitate I, and washing the precipitate I with acetone to obtain gutta-percha J;
(6) adjusting the pH of the residue H to 8-10 by adopting a NaOH solution, extracting for 20-60 min at 30-50 ℃, centrifuging to obtain a supernatant, adjusting the supernatant by using a hydrochloric acid solution until the protein is completely precipitated, and carrying out vacuum freeze drying on the obtained precipitate to obtain the eucommia seed protein N.
The extrusion temperature in the granulation in the step (1) is 180-250 ℃, and the water content of the extruded granules is 5-7%.
The squeezing temperature in the step (2) is 60-90 ℃, and the squeezing pressure is 3.0-4.0 MPa.
The mass fraction of the ethanol in the step (3) is 80-100%
And (3) eluting the washing liquid C in the step (4) by using acetone with the volume being 3 times that of the column after being adsorbed by macroporous resin T8, wherein the temperature of vacuum concentration is 40-60 ℃.
The freezing temperature of the extracting solution G in the step (5) is-4 to-10 ℃, and the freezing time is 12 to 24 hours.
In the step (6), the concentration of the NaOH solution is 0.1 mol/L, and the concentration of the hydrochloric acid solution is 0.1 mol/L.
The technological parameters of vacuum freeze drying in the step (6) are as follows: the vacuum degree is 50-60 Pa, the temperature is-28 to-18 ℃, and the time is 24-36 h.
The invention has the beneficial effects that: (1) the invention adopts a double-screw extrusion device to carry out pretreatment methods such as extrusion puffing granulation, blank rolling by a roller press and the like, effectively destroys the cells of seeds, is beneficial to the release of grease and the extraction of ingredients such as gutta-percha and the like, and has high extraction yield; (2) the invention adopts a comprehensive extraction method to comprehensively extract 4 components of the eucommia seed oil, the aucubin, the gutta percha and the protein, which is beneficial to the comprehensive utilization of raw materials, the improvement of economic benefits, the reduction of emission and the reduction of resource waste.
Drawings
FIG. 1 is a process flow diagram of the present invention.
FIG. 2 is a graph showing the effect of petroleum ether extraction time on gutta-percha yield in example 3 of the present invention.
FIG. 3 is a graph showing the effect of pH on protein yield in example 4 of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples. It is to be understood that the following examples are illustrative only and are not intended to limit the scope of the invention, which is to be given numerous insubstantial modifications and adaptations by those skilled in the art based on the teachings set forth above.
Example 1
A comprehensive extraction method of oil, protein, aucubin and gutta-percha in eucommia seeds comprises the following steps:
(1) the eucommia seeds are taken as raw materials, after being crushed to 20 meshes, the eucommia seeds are extruded and puffed to be granulated by a double-screw extrusion device, the extrusion temperature is 220 ℃ during granulation, and the water content of the granules after extrusion is 5%;
(2) after granulation, rolling the blank by using a roller press until the thickness is less than 0.5mm, and then squeezing the blank at the temperature of 60 ℃ and under the pressure of 4.0MPa to obtain eucommia seed oil A and cake B;
(3) washing the pressed cake B by using 100% ethanol as an alcohol washing solvent to obtain a washing liquid C and a residue D;
(4) adsorbing the washing solution C with macroporous resin T8, eluting with 3 times column volume of acetone to obtain eluate E, vacuum concentrating the eluate at 60 deg.C, and drying to obtain aucubin F; extracting the residue D with 60-90 deg.C petroleum ether for 60min to obtain extractive solution G and residue H,
(5) freezing the extracting solution G at-4 ℃ for 24h, separating out a precipitate I, and washing the precipitate I with acetone to obtain gutta-percha J;
(6) adjusting the pH of the residue H to 9.5 by using 0.1 mol/L NaOH solution, extracting for 60min at 30 ℃, centrifuging (5000r/min) for 15min to obtain supernatant, namely eucommia seed meal protein extracting solution, adjusting the supernatant by using 0.1 mol/L diluted hydrochloric acid until the protein is completely precipitated, and carrying out vacuum freeze drying on the obtained precipitate for 36H under the conditions of vacuum degree of 50Pa and temperature of-18 ℃ to obtain eucommia seed protein N.
The results of comparing the kernel pressing effect of single puffing, single rolling with that of the present invention (puffing + rolling) are shown in table 1.
TABLE 1 Effect of different pretreatment methods on the pressing effect of fats and oils
| Index (I) | Puffing independently | Single roll press | Puffing and rolling |
| Residual oil ratio (%) | 8.2 | 12.3 | 2.1 |
As can be seen from Table 1, the present invention adopts a method combining puffing and rolling, and the residual oil rate after kernel pressing is the lowest.
Example 2
A comprehensive extraction method of oil, protein, aucubin and gutta-percha in eucommia seeds comprises the following steps:
(1) the eucommia seeds are taken as raw materials, after the eucommia seeds are crushed to 60 meshes, a double-screw extrusion device is adopted for extrusion, puffing and granulation, the extrusion temperature is 200 ℃ during granulation, and the water content of the granules after extrusion is 7%;
(2) rolling the mixture to a thickness of less than 0.5mm by using a roller press after granulation, and then squeezing the mixture at 70 ℃ and 3.8MPa to obtain eucommia seed oil A and cake B;
(3) washing the pressed cake B by using 50-100% ethanol as an alcohol washing solvent to obtain a washing liquid C and a residue D;
(4) adsorbing the washing solution C with macroporous resin T8, eluting with 3 times column volume of acetone to obtain eluate E, vacuum concentrating the eluate at 40 deg.C, and drying to obtain aucubin F; extracting the residue D with petroleum ether at the temperature of 60-90 ℃ for 60min to obtain an extracting solution G and a residue H;
(5) freezing the extracting solution G at-10 ℃ for 12h, separating out a precipitate I, and washing the precipitate I with acetone to obtain gutta-percha J;
(6) adjusting the pH of the residue H to 9.5 by using 0.1 mol/L NaOH solution, extracting at 30 ℃ for 30min, centrifuging (5000r/min) for 15min to obtain supernatant, namely eucommia seed meal protein extracting solution, adjusting the supernatant by using 0.2 mol/L dilute hydrochloric acid until the protein is completely precipitated, and carrying out vacuum freeze drying on the obtained precipitate for 24H under the conditions of vacuum degree of 60Pa and temperature of-28 ℃ to obtain eucommia seed protein N.
The effect of different ethanol concentrations on aucubin yield in this example is shown in Table 2.
TABLE 2 influence of different ethanol concentrations on aucubin yield
| Ethanol concentration (%) | 80 | 85 | 95 | 100 |
| Aucubin yield (%) | Not detected out | 10.3 | 20.3 | 95.6 |
As can be seen from Table 2, the absolute ethanol extraction effect was good.
Example 3
A comprehensive extraction method of grease, protein, aucubin and gutta-percha in eucommia seeds comprises the following steps:
(1) the eucommia seeds are taken as raw materials, after being crushed to 20 meshes, the eucommia seeds are extruded and puffed to be granulated by a double-screw extrusion device, the extrusion temperature is 50 ℃ during granulation, and the water content of the granules after extrusion is 6%;
(2) after granulation, rolling the blank by using a roller press until the thickness is less than 1.0mm, and then squeezing the blank at the temperature of 80 ℃ and under the pressure of 3.5MPa to obtain eucommia seed oil A and cake B;
(3) washing the pressed cake B by using 100% ethanol as an alcohol washing solvent to obtain a washing liquid C and a residue D;
(4) adsorbing the washing solution C with macroporous resin T8, eluting with 3 times column volume of acetone to obtain eluate E, vacuum concentrating the eluate at 60 deg.C, and drying to obtain aucubin F; extracting the residue D with petroleum ether at 60-90 deg.C for 10-90 min (the influence of petroleum ether extraction time on gutta Percha is shown in figure 2) to obtain extractive solution G and residue H,
(5) freezing the extracting solution G at-10 ℃ for 20h, separating out a precipitate I, and washing the precipitate I with acetone to obtain gutta-percha J;
(6) adjusting the pH of the residue H to 9.5 by using 0.1NaOH solution, extracting for 30min, centrifuging (5000r/min) for 15min to obtain supernatant, namely eucommia seed meal protein extracting solution, adjusting the supernatant by using 0.1 mol/L diluted hydrochloric acid until the protein is completely precipitated, and carrying out vacuum freeze drying on the obtained precipitate for 30H under the conditions of vacuum degree of 55Pa and temperature of-20 ℃ to obtain eucommia seed protein N.
Example 4
A comprehensive extraction method of oil, protein, aucubin and gutta-percha in eucommia seeds comprises the following steps:
(1) the eucommia seeds are taken as raw materials, after being crushed to 20 meshes, the eucommia seeds are extruded and puffed to be granulated by a double-screw extrusion device, the extrusion temperature is 50 ℃ during granulation, and the water content of the granules after extrusion is 6%;
(2) after granulation, rolling the blank by using a roller press until the thickness is less than 1.0mm, and then squeezing the blank at the temperature of 90 ℃ and under the pressure of 3.0MPa to obtain eucommia seed oil A and cake B;
(3) washing the pressed cake B by using 100% ethanol as an alcohol washing solvent to obtain a washing liquid C and a residue D;
(4) adsorbing the washing solution C with macroporous resin T8, eluting with 3 times column volume of acetone to obtain eluate E, vacuum concentrating the eluate at 60 deg.C, and drying to obtain aucubin F; extracting the residue D with petroleum ether at the temperature of 60-90 ℃ for 90min to obtain an extracting solution G and a residue H;
(5) freezing the extracting solution G at-10 ℃ for 20h, separating out a precipitate I, and washing the precipitate I with acetone to obtain gutta-percha J;
(6) adjusting the pH of the residue H to 8-10 by using 0.1NaOH solution (the influence of the pH on the protein yield is shown in figure 3), extracting at 40 ℃ for 30min, centrifuging (5000r/min) for 15min to obtain supernatant, namely eucommia seed meal protein extract, adjusting the supernatant by using 0.1 mol/L diluted hydrochloric acid until the protein is completely precipitated, and carrying out vacuum freeze drying on the obtained precipitate at the vacuum degree of 60Pa and the temperature of-24 ℃ for 32H to obtain eucommia seed protein N.
The foregoing shows and describes the general principles and features of the present invention, together with the advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (5)
1. A comprehensive extraction method of grease, protein, aucubin and gutta-percha in eucommia seeds is characterized by comprising the following steps:
(1) taking eucommia seeds as raw materials, crushing the eucommia seeds into 10-60 meshes, and then extruding, puffing and granulating by adopting a double-screw extrusion device;
(2) after granulation, rolling the blank by using a roller press until the thickness is less than 0.2-1.2 mm, then squeezing to obtain eucommia seed oil A and cake B;
(3) washing the cake B obtained after squeezing by using ethanol as an alcohol washing solvent to obtain a washing liquid C and a residue D;
(4) eluting the washing solution C after adopting macroporous resin for adsorption to obtain an eluent E, and concentrating and drying the eluent in vacuum to obtain aucubin F; extracting the residue D with petroleum ether at the temperature of 60-90 ℃ for 30-90 min to obtain an extracting solution G and a residue H;
(5) freezing the extracting solution G, separating out a precipitate I, and washing the precipitate I with acetone to obtain gutta-percha J;
(6) adjusting the pH of the residue H to 8-10 by adopting a NaOH solution, extracting for 20-60 min at 30-50 ℃, centrifuging to obtain a supernatant, adjusting the supernatant by using a hydrochloric acid solution until the protein is completely precipitated, and carrying out vacuum freeze drying on the obtained precipitate to obtain eucommia seed protein N;
the extrusion temperature in the granulation in the step (1) is 180-250 ℃, and the water content of the extruded granules is 5-7%;
the squeezing temperature in the step (2) is 60-90 ℃, and the squeezing pressure is 3.0-4.0 MPa;
the mass fraction of the ethanol in the step (3) is 100%.
2. The method for comprehensively extracting oil, protein, aucubin and gutta-percha from eucommia seeds as claimed in claim 1, wherein: and (3) eluting the washing liquid C in the step (4) by using acetone with the volume being 3 times that of the column after being adsorbed by macroporous resin T8, wherein the temperature of vacuum concentration is 40-60 ℃.
3. The method for comprehensively extracting oil, protein, aucubin and gutta-percha from eucommia seeds as claimed in claim 1, wherein: the freezing temperature of the extracting solution G in the step (5) is-4 to-10 ℃, and the freezing time is 12 to 24 hours.
4. The method for comprehensively extracting oil, protein, aucubin and gutta-percha from eucommia seeds as claimed in claim 1, wherein the concentration of NaOH solution in said step (6) is 0.1 mol/L, and the concentration of hydrochloric acid solution is 0.1 mol/L.
5. The method for comprehensively extracting oil, protein, aucubin and gutta-percha from eucommia seeds as claimed in claim 1, wherein: the technological parameters of vacuum freeze drying in the step (6) are as follows: the vacuum degree is 50-60 Pa, the temperature is-28 to-18 ℃, and the time is 24-36 h.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1400299A (en) * | 2001-08-06 | 2003-03-05 | 张康健 | Method for continuously extracting eucommia oil and aucuboside from eucommia seed |
| CN102796610A (en) * | 2012-08-18 | 2012-11-28 | 湘西老爹生物有限公司 | Production technology for extracting eucommia oil and eucommia protein from eucommia kernels |
| CN103254445A (en) * | 2012-02-17 | 2013-08-21 | 北京林业大学 | Eucommia ulmoides rubber refining method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1400299A (en) * | 2001-08-06 | 2003-03-05 | 张康健 | Method for continuously extracting eucommia oil and aucuboside from eucommia seed |
| CN103254445A (en) * | 2012-02-17 | 2013-08-21 | 北京林业大学 | Eucommia ulmoides rubber refining method |
| CN102796610A (en) * | 2012-08-18 | 2012-11-28 | 湘西老爹生物有限公司 | Production technology for extracting eucommia oil and eucommia protein from eucommia kernels |
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