A method for preparing hemp seed extract

Abstract

This invention relates to the field of traditional Chinese medicine extraction technology, and discloses a method for preparing hemp seed extract: Hemp seed slices are ground into the coarsest powder, and 6-12 times their weight of water are added to an extraction tank. Simultaneously, 2%-10% of the weight of β-cyclodextrin from the coarsest hemp seed powder is added to a β-cyclodextrin solution prepared by dissolving β-cyclodextrin in 5-20 times its weight of water. The mixture is dynamically stirred and simmered at a gentle boil for 0.5-3 hours. The mixture is then filtered to obtain a first extract and a residue. The residue and 5-12 times their weight of water from the coarsest hemp seed powder are added to the extraction tank, and the mixture is dynamically stirred and simmered at a gentle boil for 0.5-3 hours. The mixture is then filtered to obtain a second extract. The two extracts are combined and centrifuged to obtain a centrifuged liquid. The centrifuged liquid is concentrated under low-temperature reduced pressure to a relative density of 1.05-1.15, which is measured at 60°C. The concentrate is then spray-dried or belt-dried to obtain the hemp seed extract. This invention can effectively extract both water-soluble and fat-soluble components from hemp seeds, avoiding the complex process of first pressing the oil and then encapsulating it. The process is effective, simple, and easy to implement, making it suitable for large-scale production.

Description

Technical Field

[0001] This invention relates to the field of traditional Chinese medicine extraction technology, and in particular to a method for preparing hemp seed extract. Background Technology

[0002] Hemp seeds are the dried, mature seeds of the hemp plant (Cannabis sativa), a member of the Moraceae family. Also known as hemp kernels, hemp seeds, fire hemp, white hemp seeds, and winter hemp seeds, they are widely distributed in Northeast, North, and South China. Modern research shows that hemp seeds are rich in nutrients, including protein, oils, and dietary fiber, and have beneficial effects such as lowering blood lipids, anti-inflammation, anti-oxidation, and improving memory. Hemp seed oil is an oil extract from hemp seeds, comprising over 50% of the seed. It contains a large amount of unsaturated fatty acids, which also contribute to lowering blood lipids, anti-oxidation, and improving memory.

[0003] Currently, most methods for preparing hemp seed water extract involve extracting hemp seed slices with water or pressing the oil first and then extracting the water. Direct water extraction of hemp seeds results in insufficient extraction and utilization of the hemp seed oil, leading to a low yield and small amount of extract. While pressing the oil first and then extracting the water allows for the collection of hemp seed oil, it requires additional oil pressing equipment (increasing costs) and processes (time-consuming). Furthermore, the extracted oil needs further processing before being mixed with the extract; otherwise, the extract has poor stability and is prone to oil seepage. Additionally, direct spray drying of the hemp seed water extract results in the spray-dried powder easily sticking to the walls, leading to significant powder loss and a low powder yield, thus resulting in a low overall yield of extract.

[0004] Therefore, there is an urgent need to develop an effective, simple, and easy-to-implement method for preparing hemp seed extract that is suitable for large-scale production. Summary of the Invention

[0005] To address the aforementioned problems, the present invention aims to provide a method for preparing hemp seed extract. This method effectively extracts both water-soluble and fat-soluble components from hemp seeds. This preserves the water-soluble components while avoiding the complex process of first pressing the oil and then encapsulating it. The process is effective, simple, and suitable for large-scale production.

[0006] To achieve the above objectives, the present invention adopts the following technical solution:

[0007] A method for preparing hemp seed extract includes the following steps:

[0008] (1) Grind hemp seed slices into the coarsest powder;

[0009] (2) Put the coarsest powder of hemp seeds into an extraction tank with 6 to 12 times its weight of water. At the same time, put the β-cyclodextrin solution prepared by dissolving 2% to 10% of the weight of the coarsest powder of hemp seeds in 5 to 20 times its weight of water into the extraction tank. Dynamically stir and extract the product at a stirring speed of 20 to 50 rpm. Maintain a gentle boil for 0.5 to 3 hours. Filter while hot to obtain the first extract and the residue.

[0010] (3) Add 5 to 12 times the weight of the dregs and the coarsest powder of hemp seeds to the extraction tank, stir dynamically and extract, with a stirring speed of 20 to 50 rpm, and keep it boiling for 0.5 to 3 hours. Filter while hot to obtain the second extract.

[0011] (4) Combine the first and second extracts and centrifuge to obtain centrifuged liquid;

[0012] (5) The centrifuged liquid is concentrated under low temperature and reduced pressure in a vacuum concentrator at a temperature of 65-85℃ and a vacuum degree of -0.04 to -0.08 MPa to a relative density of 1.05-1.15. The relative density is measured at 60℃. The liquid is then spray-dried or belt-dried to obtain hemp seed extract.

[0013] Preferably, the centrifugation in step (4) is specifically performed by centrifuging at a drum speed of 12,000 rpm to 16,000 rpm in a tubular centrifuge.

[0014] Preferably, the spray drying conditions in step (5) are: controlling the inlet air temperature to be 140-190°C and the outlet air temperature to be 75-95°C.

[0015] Preferably, the conditions for belt drying in step (5) are: drying temperature controlled at 90-120℃, cooling temperature at 20-40℃, absolute vacuum degree ≤2000Pa, cloth-making motor speed at 160-240rpm / min, cloth-making angle at 10-20°, and a feeding speed of 1-5L / h and a track running speed of 60-400mm / min.

[0016] Another objective of this invention is to disclose a hemp seed derivative preparation, wherein the active ingredient of the hemp seed derivative preparation is the hemp seed extract obtained by the above preparation method.

[0017] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0018] (1) In this invention, hemp seed slices are crushed into the coarsest powder and then extracted with water, which destroys the seed coat structure of hemp seeds and can effectively increase the dissolution of hemp seed oil.

[0019] (2) This invention involves two decoctions with water. In the first decoction, 2-10% by weight of β-cyclodextrin (the coarsest weight of hemp seed powder) is added to the extract. This allows the hemp seed oil to be encapsulated or embedded within the cavities of the β-cyclodextrin, forming an ultrafine particle dispersion for effective extraction. This process pulverizes the volatile and deformable drug, thereby improving its stability and bioavailability, and also mitigating the wall-sticking phenomenon during spray drying. Simultaneously extracting water-soluble and fat-soluble substances makes it suitable for large-scale production, significantly improving hemp seed oil extraction, increasing the total fatty oil content of the extract, and increasing the yield.

[0020] Existing technologies using β-cyclodextrin inclusion technology typically involve first collecting the fatty oil through other methods, and then using β-cyclodextrin inclusion to retain the fat-soluble substances in the extract. Other methods usually involve oil extraction or organic solvent extraction. Oil extraction requires additional equipment and increases costs, while organic solvent extraction is unsuitable for large-scale production. The preparation method of this invention can effectively extract both water-soluble and fat-soluble components from hemp seeds. This preserves the water-soluble components while avoiding the complex process of first extracting oil and then inclusion. The process is effective, simple, and suitable for large-scale production.

[0021] (3) The present invention uses dynamic stirring extraction, which can improve the inclusion efficiency of β-cyclodextrin in hemp seed oil. Attached Figure Description

[0022] Figure 1 This is a process flow diagram of the present invention;

[0023] Figure 2 These are thin-layer chromatograms of the hemp seed extract and hemp seed reference medicinal material solution prepared in Examples 1-2 and Comparative Examples 1-4 of this invention. Detailed Implementation

[0024] The present invention will be further described below with reference to specific embodiments.

[0025] It should be noted that, unless otherwise specified, the raw materials used in the technical solutions provided by this invention are all prepared by conventional means or purchased through commercial channels.

[0026] Example 1:

[0027] A method for preparing hemp seed extract, such as Figure 1 As shown, it includes the following steps:

[0028] (1) The hemp seed slices are made into the coarsest powder (the pharmacopoeia stipulates that the coarsest powder refers to powder that can pass through the No. 1 sieve, but contains no more than 20% powder that can pass through the No. 3 sieve).

[0029] (2) Put the coarsest powder of hemp seeds and 8 times its weight of water into an extraction tank. At the same time, add 2% of the weight of β-cyclodextrin of the coarsest powder of hemp seeds into 10 times its weight of purified water to prepare a β-cyclodextrin solution and put it into the extraction tank. Dynamically stir and extract the product. The stirring speed is 20-50 rpm. Maintain a gentle boil for 2 hours (it should be noted that gentle boil is a routine operation in the extraction of traditional Chinese medicine. Those skilled in the art can maintain a gentle boil). Filter while hot to obtain the first extract and the residue.

[0030] (3) Add water equal to 6 times the weight of the dregs and the coarsest powder of hemp seeds into the extraction tank, stir dynamically and extract, with a stirring speed of 20-50 rpm, maintain a gentle boil and decoct for 1.5 hours, filter while hot to obtain the second extract;

[0031] (4) Combine the first extract and the second extract, centrifuge at a drum speed of 12,000 rpm to obtain centrifuged liquid;

[0032] (5) The centrifuged liquid was concentrated under low-temperature reduced pressure in a vacuum concentrator at a temperature of 65–85°C and a vacuum degree of -0.04–-0.08 MPa until a relative density of 1.05–1.15 (measured at 60°C) was obtained, yielding a concentrated solution. The concentrated solution was then spray-dried to obtain hemp seed extract. The spray-drying conditions were: inlet air temperature controlled at 140–190°C and outlet air temperature controlled at 75–95°C.

[0033] Example 2:

[0034] A method for preparing hemp seed extract includes the following steps:

[0035] (1) Grind hemp seed slices into the coarsest powder;

[0036] (2) Put the coarsest powder of hemp seeds and 8 times its weight of water into an extraction tank. At the same time, put the β-cyclodextrin solution prepared by dissolving 10% of the weight of the coarsest powder of hemp seeds in 20 times its weight of purified water into the extraction tank. Dynamically stir and extract the product. The stirring speed is 20-50 rpm. Maintain a gentle boil for 2 hours. Filter while hot to obtain the first extract and the residue.

[0037] (3) Add water equal to 6 times the weight of the dregs and the coarsest powder of hemp seeds into the extraction tank, stir dynamically and extract, with a stirring speed of 20-50 rpm, maintain a gentle boil and decoct for 1.5 hours, filter while hot to obtain the second extract;

[0038] (4) Combine the first extract and the second extract, centrifuge at a drum speed of 12,000 rpm to obtain centrifuged liquid;

[0039] (5) The centrifuged liquid was concentrated under low-temperature reduced pressure in a vacuum concentrator at a temperature of 65–85℃ and a vacuum degree of -0.04–-0.08 MPa to a relative density of 1.05–1.15 (measured at 60℃) to obtain a concentrate. The concentrate was then subjected to vacuum belt drying to obtain hemp seed extract. The belt drying conditions were as follows: drying temperature controlled at 90–120℃, cooling temperature at 20–40℃, absolute vacuum degree ≤2000Pa, cloth motor speed at 160–240 rpm / min, cloth angle at 10–20°, feed rate at 1–5 L / h, and belt running speed at 60–400 mm / min.

[0040] Example 3:

[0041] A hemp seed derivative preparation, wherein the active ingredient of the hemp seed derivative preparation is the hemp seed extract prepared in Example 1 or Example 2.

[0042] Comparative Example 1:

[0043] A method for preparing hemp seed extract includes the following steps:

[0044] (1) Put the hemp seed slices and 8 times their weight of water into an extraction tank, keep it at a gentle boil for 2 hours, filter while hot, and obtain the first extract and the residue.

[0045] (2) Put the dregs and hemp seed slices into an extraction tank with 6 times the weight of water, keep it boiling gently for 1.5 hours, filter while hot to obtain the second extract;

[0046] (3) Combine the first extract and the second extract, centrifuge at a drum speed of 12,000 rpm to obtain centrifuged liquid;

[0047] (4) The centrifuged liquid was concentrated under low-temperature reduced pressure in a vacuum concentrator at a temperature of 65–85°C and a vacuum degree of -0.04–-0.08 MPa until the relative density reached 1.05–1.15 (measured at 60°C), yielding a concentrated solution. The concentrated solution was then spray-dried to obtain hemp seed extract. The spray-drying conditions were: inlet air temperature controlled at 140–190°C and outlet air temperature controlled at 75–95°C.

[0048] Comparative Example 2:

[0049] A method for preparing hemp seed extract includes the following steps:

[0050] (1) Grind hemp seed slices into the coarsest powder;

[0051] (2) Put the coarsest hemp seed powder and 8 times its weight of water into an extraction tank, keep it at a gentle boil and simmer for 2 hours, filter while hot to obtain the first extract and the residue.

[0052] (3) Put the dregs and water, which is 6 times the weight of the coarsest powder of hemp seeds, into the extraction tank, keep it at a gentle boil and simmer for 1.5 hours, filter while hot to obtain the second extract;

[0053] (4) Combine the first extract and the second extract, centrifuge at a drum speed of 12,000 rpm to obtain centrifuged liquid;

[0054] (5) The centrifuged liquid was concentrated under low-temperature reduced pressure in a vacuum concentrator at a temperature of 65–85°C and a vacuum degree of -0.04–-0.08 MPa until a relative density of 1.05–1.15 (measured at 60°C) was obtained, yielding a concentrated solution. The concentrated solution was then spray-dried to obtain hemp seed extract. The spray-drying conditions were: inlet air temperature controlled at 140–190°C and outlet air temperature controlled at 75–95°C.

[0055] Comparative Example 3:

[0056] A method for preparing hemp seed extract includes the following steps:

[0057] (1) Grind hemp seed slices into the coarsest powder;

[0058] (2) Put the coarsest powder of hemp seeds and 8 times its weight of water into the extraction tank. At the same time, put the β-cyclodextrin solution prepared by dissolving 2% of the weight of the coarsest powder of hemp seeds in 10 times its weight of purified water into the extraction tank. Keep it boiling gently for 2 hours, filter while hot, and obtain the first extract and the residue.

[0059] (3) Put the dregs and water, which is 6 times the weight of the coarsest powder of hemp seeds, into the extraction tank, keep it at a gentle boil and simmer for 1.5 hours, filter while hot to obtain the second extract;

[0060] (4) Combine the first extract and the second extract, centrifuge at a drum speed of 12,000 rpm to obtain centrifuged liquid;

[0061] (5) The centrifuged liquid was concentrated under low-temperature reduced pressure in a vacuum concentrator at a temperature of 65–85°C and a vacuum degree of -0.04–-0.08 MPa until a relative density of 1.05–1.15 (measured at 60°C) was obtained, yielding a concentrated solution. The concentrated solution was then spray-dried to obtain hemp seed extract. The spray-drying conditions were: inlet air temperature controlled at 140–190°C and outlet air temperature controlled at 75–95°C.

[0062] Comparative Example 4:

[0063] A method for preparing hemp seed extract includes the following steps:

[0064] (1) Grind hemp seed slices into the coarsest powder, wrap and simmer;

[0065] (2) Put the coarsest powder of hemp seeds and 8 times its weight of water into an extraction tank. At the same time, put the β-cyclodextrin solution prepared by dissolving 2% of the weight of the coarsest powder of hemp seeds in 10 times its weight of purified water into the extraction tank. Dynamically stir and extract the product. The stirring speed is 20-50 rpm. Maintain a gentle boil for 2 hours. Filter while hot to obtain the first extract and the residue.

[0066] (3) Add water equal to 6 times the weight of the dregs and the coarsest powder of hemp seeds into the extraction tank, stir dynamically and extract, with a stirring speed of 20-50 rpm, maintain a gentle boil and decoct for 1.5 hours, filter while hot to obtain the second extract;

[0067] (4) Combine the first extract and the second extract, centrifuge at a drum speed of 12,000 rpm to obtain centrifuged liquid;

[0068] (5) The centrifuged liquid was concentrated under low-temperature reduced pressure in a vacuum concentrator at a temperature of 65–85°C and a vacuum degree of -0.04–-0.08 MPa until a relative density of 1.05–1.15 (measured at 60°C) was obtained, yielding a concentrated solution. The concentrated solution was then spray-dried to obtain hemp seed extract. The spray-drying conditions were: inlet air temperature controlled at 140–190°C and outlet air temperature controlled at 75–95°C.

[0069] The hemp seed extracts prepared in Examples 1-2 and Comparative Examples 1-4 were tested, and the results are shown in the table below:

[0070] Method for detecting total fatty oil: Take an appropriate amount of sample (about 1g), grind it finely, weigh it accurately, place it in a Soxhlet extractor, add an appropriate amount of petroleum ether (60-90℃), heat and reflux to extract (5 hours) until the fatty oil is completely extracted, collect the extract, place it in an evaporating dish that has been dried to constant weight, evaporate it to dryness at low temperature in a water bath, dry it at 100℃ for 1 hour, transfer it to a desiccator, cool it for 30 minutes, weigh it accurately, and calculate the result.

[0071]

[0072] As can be seen from the table above, the total fat content, extract yield, and extract content of the hemp seed water extracts obtained in Examples 1 and 2 are significantly higher than those in Comparative Examples 1-4, indicating that the process of the present invention is more thorough and effective in extracting hemp seeds.

[0073] Compared with Comparative Example 3, Example 1 shows that the total fatty oil content of hemp seed water extract obtained by dynamic extraction (Example 1) is more than double that obtained by static extraction (Comparative Example 3), and the yield and extract content are also significantly improved. This indicates that dynamic extraction can improve the inclusion efficiency of β-cyclodextrin in hemp seed oil, making the extraction more thorough and effective.

[0074] Compared with Comparative Example 4, Example 1 shows that wrapping and decocting significantly affects the total fat content, yield, and extract of hemp seed water extract. Therefore, extraction without wrapping and decocting yields better results.

[0075] Compared with Comparative Example 3, it can be seen that the total fatty oil content and yield of hemp seed water extract with the addition of excipient β-cyclodextrin (Comparative Example 3) are significantly higher, indicating that β-cyclodextrin can improve the extraction of hemp seed oil, increase the total fatty oil content of the extract, and increase the yield.

[0076] Compared with Comparative Example 2, it can be seen that processing hemp seed slices into the coarsest powder and then extracting them with water can effectively increase the dissolution of hemp seed oil. The total fat content, yield, and extract of the hemp seed water extract are all significantly higher.

[0077] Thin-layer chromatography was performed on the hemp seed extracts and hemp seed control solutions prepared in Examples 1-2 and Comparative Examples 1-4. The results are as follows: Figure 2 As shown.

[0078] Thin-layer chromatography identification method: Take about 0.25g of hemp seed extract, grind it into a fine powder, add 30ml of methanol, sonicate for 30 minutes, filter, evaporate the filtrate to dryness, dissolve the residue in 1ml of methanol to prepare the test solution. Separately, take 2g of hemp seed reference material, add 50ml of water, boil for 30 minutes, filter, evaporate the filtrate to dryness, add the residue in 30ml of methanol, and prepare the reference material solution in the same way. Perform thin-layer chromatography (Chinese Pharmacopoeia 2015 Edition, Part IV, General Chapter 0502), take 5μl of the above test solution and 2μl of the reference material solution, and spot them separately on the same silica gel G thin-layer plate. Use toluene-ethyl acetate-formic acid (15:1:0.3) as the developing solvent, develop, remove, air dry, spray with vanillin-sulfuric acid reagent, and heat at 105℃ until the spots are clearly visible. In the chromatogram of the test sample, spots of the same color appear at the corresponding positions as in the chromatogram of the reference material. Detection environment temperature: 25℃, humidity: 58%.

[0079] from Figure 2 It can be seen that, under the same sampling amount, the spots of the hemp seed extract obtained in Examples 1 and 2 are more obvious and darker in color than the spots of the samples in Comparative Examples 1 to 4, which indirectly shows that the process of the invention has a significant improvement in the extraction of hemp seed oil.

[0080] The technical solutions provided by the embodiments of the present invention have been described in detail above. Specific examples have been used to illustrate the principles and implementation methods of the embodiments of the present invention. The descriptions of the embodiments above are only for helping to understand the principles of the embodiments of the present invention. At the same time, for those skilled in the art, there will be changes in the specific implementation methods and application scope based on the embodiments of the present invention. Therefore, the content of this specification should not be construed as a limitation of the present invention.

Claims

1. A method for preparing hemp seed extract, characterized in that, Includes the following steps: (1) Grind hemp seed slices into the coarsest powder; (2) Put the coarsest powder of hemp seeds and 8 times its weight of water into an extraction tank. At the same time, put the β-cyclodextrin solution prepared by dissolving 2% of the weight of the coarsest powder of hemp seeds in 10 times its weight of water into the extraction tank. Dynamically stir and extract the product. The stirring speed is 20-50 rpm. Maintain a gentle boil for 2 hours. Filter while hot to obtain the first extract and the residue. (3) Add water equal to 6 times the weight of the dregs and the coarsest powder of hemp seeds into the extraction tank, stir dynamically and extract, with a stirring speed of 20-50 rpm, maintain a gentle boil and decoct for 1.5 hours, filter while hot to obtain the second extract; (4) Combine the first and second extracts and centrifuge to obtain centrifuged liquid; (5) The centrifuged liquid was concentrated under low temperature and reduced pressure in a vacuum concentrator at a temperature of 65-85℃ and a vacuum degree of -0.04--0.08 MPa to a relative density of 1.05-1.15, which was measured at 60℃. The liquid was then spray-dried to obtain hemp seed extract. The centrifugation in step (4) specifically involves centrifuging at a drum speed of 12,000 rpm to 16,000 rpm in a tubular centrifuge. The conditions for spray drying in step (5) are: control the inlet air temperature to be 140-190℃ and the outlet air temperature to be 75-95℃.

2. A hemp seed-derived preparation, characterized in that, The active ingredient of the hemp seed derivative preparation is the hemp seed extract obtained by the preparation method described in claim 1.

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