Spina date seed oil as well as preparation method and application thereof

Abstract

The invention belongs to the technical field of spina date seed oil extraction, and provides spina date seed oil as well as a preparation method and application thereof. The preparation method comprises the following steps: crushing and sieving spina date seeds to obtain spina date seed coarse powder; pre-extracting the semen ziziphi spinosae coarse powder by using an organic solvent to obtain an extracting solution 1 and residues; granulating the residues to obtain spina date seed granules; re-extracting the spina date seed particles by using an organic solvent to obtain extract liquor 2; and mixing the extract liquid 1 and the extract liquid 2 to obtain the spina date seed oil. The preparation method combines a plurality of technical characteristics of pre-extraction, granulation, staged gradient re-extraction and the like, so that the whole technical scheme has the characteristics of mild extraction conditions and no need of high temperature and high pressure; the extraction time is short; the oil yield is high; the effective components in the spina date seeds can be extracted to the maximum extent.

Description

Technical Field

[0001] The invention relates to the technical field of extraction of wild jujube seed oil, in particular to wild jujube seed oil and a preparation method and application thereof. Background Art

[0002] In the existing technology, the extraction of jujube seed oil can generally be divided into solvent extraction, pressing, microwave-assisted extraction, ultrasound-assisted extraction, subcritical extraction, supercritical fluid extraction technology, etc.

[0003] Solvent extraction is the most common extraction method in the oil extraction process. It is easy to operate, has a high oil extraction rate, and has good residual meal quality. According to the principle of "like dissolves like", the selection of a suitable solvent can selectively migrate the substances we need from the surface or interior of the raw material to the solvent. Petroleum ether, ether, cyclohexane, n-hexane and other solvents have been used for the extraction of jujube kernel oil. However, this method still has some shortcomings, such as the long solvent extraction time, which causes the oil to be in a high temperature state for a long time, accelerates the oxidation and degradation of unsaturated fatty acids, and destroys thermosensitive biologically active substances, thereby reducing the quality of the oil. In addition, this method requires a large amount of extraction solvent, and there is a lot of organic solvent residue in the product.

[0004] The pressing method is to squeeze out the oil in the raw material with the help of high pressure, which can effectively avoid the problem of organic residue in the product. In addition, the pressing method has strong adaptability, high safety, simple process operation, can be used for the extraction of various vegetable oils, and can retain the nutrients in the raw materials such as protein, fat-soluble vitamins, trace elements, etc. to a large extent. However, compared with the chemical extraction method, the pressing method has a low oil extraction rate, high labor intensity, and low production efficiency. In addition, the protein of the cake after the oil is extracted is severely denatured, which is not conducive to the subsequent processing and utilization of the oil cake. It can generally only be used for the production of animal feed, resulting in a low comprehensive utilization rate of oil resources. Therefore, its application in the extraction of jujube kernel oil is limited.

[0005] Microwave-assisted extraction technology is an emerging extraction technology in recent years. Due to its low energy consumption, high efficiency, short time and less organic solvent residue, microwave-assisted extraction has become a green and safe extraction technology. Microwave-assisted extraction technology uses electromagnetic spectrum with a radiation range of 300MHz to 300GHz to penetrate the extraction medium and produce thermal effects by changing its frequency, thereby destroying the cell walls of plant cells and improving mass transfer efficiency. Compared with other traditional solvent extraction methods, microwave-assisted extraction generates high temperatures during extraction, so it is not suitable for the extraction of heat-sensitive biological substances such as proteins.

[0006] In recent years, supercritical fluid extraction has become a new extraction technology. Compared with traditional extraction technologies, supercritical fluid extraction technology has many advantages such as no residual organic solvents, environmental friendliness, rapidity, and high efficiency. Supercritical fluids are substances with temperatures and pressures higher than their critical temperatures and critical pressures. However, their high pressure can change the structures of effective substances such as proteins, fat-soluble vitamins, and crude polysaccharides in the extracts. Moreover, the entrainer infiltrated during the extraction process brings unnecessary trouble to the subsequent processes of purifying, removing impurities, and removing the entrainer from the extracts.

[0007] It can be seen that common extraction methods in the existing technology all have certain defects. Therefore, there is an urgent need in this field to invent an extraction method for wild jujube seed oil with a shorter extraction time, lower cost, and better environmental compatibility. Summary of the Invention

[0008] The purpose of the present invention is to provide a wild jujube seed oil, its preparation method and application. The preparation method combines multiple technical features such as pre-extraction, granulation using the characteristics of wild jujube seed raw materials, and staged gradient re-extraction, making the technical solution of the present application have advantages such as mild extraction conditions, short extraction time, high oil yield, and complete extraction of effective components compared with the existing technology.

[0009] In order to achieve the above-mentioned invention purpose, the present invention provides the following technical solutions:

[0010] The present invention provides a preparation method for wild jujube seed oil, comprising the following steps:

[0011] (1) Crushing and sieving wild jujube seeds to obtain wild jujube seed coarse powder;

[0012] (2) Using an organic solvent to pre-extract the wild jujube seed coarse powder to obtain extraction liquid 1 and residue;

[0013] (3) Granulating the residue to obtain wild jujube seed granules;

[0014] (4) Using an organic solvent to re-extract the wild jujube seed granules to obtain extraction liquid 2;

[0015] (5) Mixing extraction liquid 1 and extraction liquid 2 to obtain wild jujube seed oil.

[0016] Preferably, the sieving device in step (1) is a filter screen with a pore diameter of 10 - 14 mm.

[0017] Preferably, the organic solvent in step (2) is n-butane, the usage amount of the organic solvent is 5 - 7 times the mass of the wild jujube seed coarse powder, the pressure of the pre-extraction is 0.5 - 0.8 MPa, the temperature of the pre-extraction is 35 - 40 °C, and the time of the pre-extraction is 40 - 50 min.

[0018] Preferably, the diameter of the wild jujube seed granules in step (3) is 4-8 mm.

[0019] Preferably, the method of re-extraction in step (4) is as follows: using the organic solvent to extract the wild jujube seed granules 2-5 times, with the extraction time of each time being 30-50 min; the temperature of the re-extraction is 35-40 °C, the pressure of the re-extraction is 0.5-0.8 MPa, the organic solvent is n-butane, and the usage amount of the organic solvent is 5-7 times the mass of the wild jujube seed granules.

[0020] The present invention also provides the wild jujube seed oil prepared by the above preparation method.

[0021] The present invention also provides the application of the wild jujube seed oil in the preparation of health products or drugs.

[0022] The beneficial effects of the present invention are as follows:

[0023] Compared with the conventional preparation method, in the extraction process of the wild jujube seed oil preparation method of the present invention, there is no need to add an entrainer, thus eliminating the possible pollution caused by the entrainer and realizing the greening of the production process. Moreover, the operation time of the wild jujube seed oil preparation method of the present invention is greatly shortened, which can effectively improve the production efficiency; the cost is significantly reduced, enhancing the market competitiveness of the product; and the environmental compatibility of this preparation method is excellent, and a higher extraction rate can be achieved under lower temperature and pressure conditions, having the characteristics of energy conservation and environmental protection. In addition, this preparation method also has the outstanding advantages of low organic matter residue and easy recovery of the extractant, further reducing the cost and reducing the adverse impact on the environment.

[0024] Compared with the conventional extraction method, the extraction rate of the wild jujube seed oil prepared by the preparation method of the present invention is also higher, the purity of the extracted oil is also higher, and the quality is better. Further, the present invention can maximize the retention of the content of bioactive components such as proteins and crude polysaccharides in the extract, giving full play to the medicinal value and nutritional value of the wild jujube seeds, and opening up a new path for the production and application of the wild jujube seed oil.

[0025] By optimizing the wild jujube seed oil extraction method, the present invention adopts methods not disclosed in the prior art such as pre-extraction, granulating by utilizing the characteristics of the wild jujube seed raw materials, and staged gradient re-extraction, and combines multiple technical features, making the overall technical solution show the advantages of mild extraction conditions, no need for high temperature and high pressure, short extraction time, and high oil yield. Detailed Embodiments

[0026] The present invention provides a method for preparing wild jujube seed oil, comprising the following steps:

[0027] (1) Crushing and sieving wild jujube seeds to obtain wild jujube seed coarse powder;

[0028] (2) Pre-extract the crude powder of wild jujube seeds with an organic solvent to obtain extraction liquid 1 and residue;

[0029] (3) Granulate the residue to obtain wild jujube seed granules;

[0030] (4) Re-extract the wild jujube seed granules with an organic solvent to obtain extraction liquid 2;

[0031] (5) Mix extraction liquid 1 and extraction liquid 2 to obtain wild jujube seed oil.

[0032] In the present invention, the sieving device in step (1) is preferably a filter screen with a pore size of 10 - 14 mm, and more preferably a filter screen with a pore size of 12 mm.

[0033] In the present invention, the organic solvent in step (2) is preferably n-butane, the usage amount of the organic solvent is preferably 5 - 7 times the mass of the crude powder of wild jujube seeds, more preferably 6 times the mass of the crude powder of wild jujube seeds, the pressure of the pre-extraction is preferably 0.5 - 0.8 MPa, more preferably 0.6 - 0.7 MPa, the temperature of the pre-extraction is preferably 35 - 40 °C, more preferably 37 °C, and the time of the pre-extraction is preferably 40 - 50 min, more preferably 45 min.

[0034] In the present invention, the diameter of the wild jujube seed granules in step (3) is preferably 4 - 8 mm, and more preferably 6 mm.

[0035] In the present invention, the granulation method in step (3) is preferably extrusion rotary granulation, the rotation speed of the extrusion rotary granulation is preferably 1000 - 1500 r / min, more preferably 1100 - 1300 r / min, and even more preferably 1200 r / min.

[0036] In the present invention, the re-extraction method in step (4) is: extract the wild jujube seed granules with the organic solvent 2 - 5 times, preferably 3 - 4 times, the extraction time for each time is preferably 30 - 50 min, more preferably 40 min; the temperature of the re-extraction is preferably 35 - 40 °C, more preferably 38 °C, the pressure of the re-extraction is preferably 0.5 - 0.8 MPa, more preferably 0.6 MPa, the organic solvent is preferably n-butane, and the usage amount of the organic solvent is preferably 5 - 7 times the mass of the wild jujube seed granules, more preferably 6 times the mass of the wild jujube seed granules.

[0037] The present invention also provides the wild jujube seed oil prepared by the above preparation method.

[0038] The present invention also provides the application of the wild jujube seed oil in the preparation of health products or drugs.

[0039] The technical solutions provided by the present invention will be described in detail below in conjunction with embodiments, but they should not be construed as limiting the protection scope of the present invention.

[0040] Example 1

[0041] (1) Use a stainless steel filter screen with a mesh size of 12 mm to extrude and crush 48.30 kg of wild jujube seeds, and sieve to obtain wild jujube seed coarse powder. The sieving device is a filter screen with a pore size of 12 mm;

[0042] (2) Use 289.8 kg of n-butane solution to pre-extract the wild jujube seed coarse powder. The number of pre-extraction times is 1 time, and the pre-extraction method is the non-critical extraction method. Set the pre-extraction pressure to 0.7 MPa, the pre-extraction temperature to 35 °C, and pre-extract for 45 min to obtain 6.45 kg of extraction liquid 1 and residue;

[0043] (3) Use a pharmaceutical rotary granulator with a rotation speed of 1200 r / min to granulate the residue continuously 2 times to make wild jujube seed granules with a diameter of 6 mm, totaling 41.40 kg;

[0044] (4) Use 248.4 kg of n-butane solution to re-extract 41.40 kg of wild jujube seed granules. The number of re-extraction times is three times. The re-extraction temperature is 38 °C, the re-extraction pressure is 0.7 MPa, and the extraction times are 50 min, 40 min, and 30 min in sequence. A total of 5.70 kg of extraction liquid 2 is obtained from the three extractions;

[0045] (5) Mix extraction liquid 1 and extraction liquid 2 to obtain the final wild jujube seed oil, totaling 12.15 kg, and the yield is 25.16%.

[0046] Example 2

[0047] (1) Use a stainless steel filter screen with a mesh size of 14 mm to extrude and crush 50.00 kg of wild jujube seeds, and sieve to obtain wild jujube seed coarse powder. The sieving device is a filter screen with a pore size of 10 mm;

[0048] (2) Use 250 kg of n-butane solution to pre-extract the wild jujube seed coarse powder. The number of pre-extraction times is 1 time, and the pre-extraction method is the non-critical extraction method. Set the pre-extraction pressure to 0.5 MPa, the pre-extraction temperature to 35 °C, and pre-extract for 40 min to finally obtain 6.74 kg of extraction liquid 1 and residue;

[0049] (3) Use a pharmaceutical rotary granulator with a rotation speed of 1500 revolutions per minute to granulate the residue continuously 2 times to make wild jujube seed granules with a diameter of 8 mm, totaling 43.77 kg;

[0050] (4) Use 218.85 kg of n-butane solution to re-extract 43.77 kg of wild jujube seed granules. The number of re-extraction times is two, the re-extraction temperature is 40 °C, the re-extraction pressure is 0.5 MPa, and the extraction times are 50 min and 40 min in sequence. A total of 7.03 kg of extract 2 is obtained from the two extractions;

[0051] (5) Mix extract 1 and extract 2 to obtain the final wild jujube seed oil, with a total of 13.77 kg and a yield of 27.54%.

[0052] Example 3

[0053] (1) Use a stainless steel filter screen with a mesh size of 10 mm to extrude and crush 65.00 kg of wild jujube seeds, and sieve to obtain wild jujube seed coarse powder. The sieving device is a filter screen with a pore size of 14 mm;

[0054] (2) Use 455 kg of n-butane solution to pre-extract the wild jujube seed coarse powder. The number of pre-extraction times is 1, the pre-extraction method is the non-critical extraction method, set the pre-extraction pressure to 0.8 MPa, the pre-extraction temperature to 40 °C, and pre-extract for 50 min. Finally, 8.84 kg of extract 1 and residue are obtained;

[0055] (3) Use a pharmaceutical rotary granulator with a rotation speed of 1000 revolutions per minute to continuously granulate the residue 2 times to form wild jujube seed granules with a diameter of 6 mm, totaling 53.09 kg;

[0056] (4) Use 371.63 kg of n-butane solution to re-extract 53.09 kg of wild jujube seed granules. The number of re-extraction times is five, the re-extraction temperature is 35 °C, the re-extraction pressure is 0.8 MPa, and the extraction times are 50 min, 45 min, 40 min, 35 min, and 30 min in sequence. A total of 8.41 kg of extract 2 is obtained from the five extractions;

[0057] (5) Mix extract 1 and extract 2 to obtain the final wild jujube seed oil, with a total of 17.25 kg and a yield of 26.54%.

[0058] Experimental Example

[0059] Entrust the Nanjing Institute of Product Quality Supervision and Inspection to detect the wild jujube seed oil prepared in Example 1 of this application. The detection indicators include: total saponins, quercetin, oleic acid (C18:1), linoleic acid (C18:2), zinc, selenium, β-sitosterol, acid value (KOH), peroxide value (calculated based on fat), as shown in Table 1. Sample quantity: 150 g, sample arrival date: February 26, 2025, inspection date: February 26, 2025 to March 10, 2025.

[0060] Table 1 Detection Results

[0061]

[0062] Conclusion: The present invention innovatively adopts the n-butane non-critical fluid extraction method to extract oil from the crude powder of wild jujube seeds. By this method, the yield of wild jujube seed oil can reach 25% - 30%, and compared with the conventional extraction methods, the yield is significantly increased by 6 - 8%. Moreover, the technical solution proposed in this application is excellent in improving the quality of wild jujube seed oil, showing outstanding performance in key indicators such as clarity, taste, and nutritional value. The contents of active ingredients such as β-sitosterol and total saponins contained therein are significantly higher than those of the wild jujube seed oil extracted by the pressing method or the leaching method.

[0063] As can be seen from the above embodiments, the present invention provides a wild jujube seed oil, its preparation method and application. The preparation method includes the following steps: crushing and sieving wild jujube seeds to obtain crude wild jujube seed powder; pre-extracting the crude wild jujube seed powder with an organic solvent to obtain extraction liquid 1 and residue; granulating the residue to obtain wild jujube seed granules; re-extracting the wild jujube seed granules with an organic solvent to obtain extraction liquid 2; and mixing extraction liquid 1 and extraction liquid 2 to obtain wild jujube seed oil. This preparation method combines multiple technical features such as pre-extraction, granulation, and staged gradient re-extraction, making the overall technical solution show the characteristics of mild extraction conditions without the need for high temperature and high pressure, short extraction time, high oil yield, and being able to extract the active ingredients in wild jujube seeds to the greatest extent.

[0064] The above is only the preferred embodiment of the present invention. It should be noted that for those of ordinary skill in the art, without departing from the principle of the present invention, several improvements and refinements can still be made, and these improvements and refinements should also be regarded as the protection scope of the present invention.

Claims

1. A method for preparing jujube seed oil, characterized in that: The following steps are involved: (1) crushing and sieving the Chinese jujube seeds to obtain coarse Chinese jujube seed powder; (2) pre-extracting the Ziziphus jujuba seed powder with an organic solvent to obtain an extract 1 and a residue; (3) granulating the residue to obtain spiny jujube seed granules; (4) re-extracting the Ziziphus jujuba seed particles using an organic solvent to obtain extract 2; (5) The extract 1 and the extract 2 are mixed to obtain the jujube seed oil.

2. The preparation method according to claim 1, characterized in that: The screening device in step (1) is a filter with a pore size of 10 to 14 mm.

3. The preparation method according to claim 2, characterized in that: The organic solvent in step (2) is n-butane, the amount of the organic solvent used is 5 to 7 times the mass of the jujube seed coarse powder, the pre-extraction pressure is 0.5 to 0.8 MPa, the pre-extraction temperature is 35 to 40° C., and the pre-extraction time is 40 to 50 min.

4. The preparation method according to claim 3, characterized in that: The diameter of the jujube seed particles in step (3) is 4 to 8 mm.

5. The preparation method according to claim 4, characterized in that: The re-extraction method in step (4) is: using the organic solvent to extract the Ziziphus jujuba seed particles 2 to 5 times, and the time of each extraction is 30 to 50 minutes; the temperature of the re-extraction is 35 to 40° C., the pressure of the re-extraction is 0.5 to 0.8 MPa, the organic solvent is n-butane, and the amount of the organic solvent used is 5 to 7 times the mass of the Ziziphus jujuba seed particles.

6. The wild jujube seed oil prepared by the preparation method according to any one of claims 1 to 5.

7. Use of the wild jujube seed oil according to claim 6 in the preparation of health products or medicines.

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