Fructus alpiniae oxyphyllae extract and preparation method thereof

Abstract

The invention belongs to the field of fructus alpiniae oxyphyllae fine processing, and particularly relates to a fructus alpiniae oxyphyllae extract and a preparation method thereof. The preparation method mainly comprises the processes of extraction, concentration, purification, drying and crushing. By optimizing an extraction solvent, extraction conditions and a purification method, the problems of low extraction efficiency, high impurity content, complex process, solvent residue and the like in the prior art are effectively solved, and the preparation method of the fructus alpiniae oxyphyllae extract, which is efficient, stable and suitable for industrial production, is provided. The process has the advantages of high extraction efficiency, high product purity, simplicity and convenience in operation, good safety and the like, and has a wide application prospect.

Description

Technical Field

[0001] The present invention belongs to the field of fine processing of Alpinia oxyphylla, and specifically relates to an extract of Alpinia oxyphylla and a preparation method thereof. Background Art

[0002] Alpinia oxyphylla is a traditional Chinese medicinal material with effects such as tonifying the kidney and consolidating essence, warming the spleen and stopping diarrhea, and its active ingredients include flavonoids, polysaccharides, volatile oils, etc. Flavonoid compounds are one of the important active ingredients in Alpinia oxyphylla and have various pharmacological effects such as antioxidant, anti-inflammatory, and cardiovascular protection. With the development of modern Chinese medicine extraction technology, how to efficiently extract and purify the active ingredients in Alpinia oxyphylla has become a research hotspot.

[0003] In the field of Chinese medicine extraction, the water extraction method is the most traditional and widely used method, but this method has the following disadvantages:

[0004] (1) Low extraction efficiency: The traditional water extraction method has a low extraction efficiency for lipophilic components (such as flavonoid compounds) because the solubility of lipophilic components in water is limited, resulting in a large loss of active ingredients.

[0005] (2) High impurity content: After extraction by the traditional water extraction method, a large amount of other impurities will be dissolved in the extract, increasing the difficulty of subsequent purification.

[0006] (3) Complex process: In the prior art, the purification step mostly uses multiple extractions or column chromatography, with cumbersome operations, long time consumption, high production costs, and is not suitable for industrial production.

[0007] (4) Solvent residue: After using organic solvents in some processes, they cannot be completely removed, resulting in solvent residue problems in the final product, affecting the safety and quality of drugs.

[0008] Therefore, based on this, the technical solution of the present invention is proposed. Summary of the Invention

[0009] In order to solve the problems existing in the prior art, the present invention provides a preparation method of an extract of Alpinia oxyphylla, and the preparation method includes the following steps:

[0010] (1) Extraction: Mix the Alpinia oxyphylla medicinal material with an aqueous methanol solution, reflux and extract, and then collect the extract;

[0011] (2) Concentration: Concentrate the extract under reduced pressure to obtain a concentrated solution;

[0012] (3) Purification: Purify and elute the concentrated solution with an adsorption resin column to obtain an eluate;

[0013] (4) Drying: Concentrate the eluate under reduced pressure, and then dry it under vacuum to obtain a solid powder;

[0014] (5) Crushing: Further grind the solid powder into fine powder to obtain the semen alpiniae oxyphyllae extract.

[0015] Preferably, in step (1), the mass ratio of the semen alpiniae oxyphyllae medicinal material to the methanol aqueous solution is 1:10 - 12.

[0016] Preferably, in step (1), in the methanol aqueous solution, the volume concentration of methanol is 70 - 80 vol%.

[0017] Preferably, in step (1), the reflux extraction time is 1.5 - 2 h, and the number of reflux extraction times is 2 - 3 times.

[0018] It should be noted that in step (1), the 70 - 80 vol% methanol aqueous solution is a medium-polarity solvent, which can not only effectively dissolve the liposoluble components (such as flavonoids) in semen alpiniae oxyphyllae, but also take into account the extraction of some water-soluble components, and has a higher extraction efficiency than the traditional water extraction method; in addition, the reflux extraction method makes the solvent recycled by heating, improves the contact efficiency between the solvent and the medicinal material, and also avoids the loss of solvent volatilization, ensuring sufficient extraction; finally, through two extractions, the extraction rate of the target component is further improved, and the residual of the active ingredients in the medicinal material is reduced.

[0019] Preferably, in step (2), the temperature of the vacuum concentration is 60 - 65 °C.

[0020] Preferably, in step (3), pass the concentrated solution through an AB-8 macroporous adsorption resin column, first wash off the impurities with deionized water, and then elute the target component with 70 vol% ethanol, and collect the ethanol eluate.

[0021] It should be noted that the AB-8 resin has a large specific surface area and a specific pore size distribution, which can selectively adsorb flavonoids, and has a weak adsorption capacity for impurities such as polysaccharides and proteins; deionized water can effectively wash off water-soluble impurities (such as polysaccharides and proteins), while the target component (flavonoids) remains on the resin; 70% ethanol can effectively desorb flavonoids and avoid introducing new impurities.

[0022] Preferably, in step (4), the temperature of the vacuum concentration is 50 - 55 °C.

[0023] It should be noted that vacuum concentration at 50 - 55 °C can effectively remove the solvent in the extract and avoid solvent residue; while the vacuum drying method is carried out at a lower temperature, which can not only further remove the residual solvent, but also avoid the decomposition or inactivation of the target component due to high temperature.

[0024] Preferably, in step (5), after grinding into fine powder, pass through an 80 - 100 mesh sieve to obtain the semen alpiniae oxyphyllae extract.

[0025] Based on the same inventive concept, another solution of the present invention is to provide an Alpinia oxyphylla extract obtained by the above preparation method.

[0026] In addition, it should be noted that during the preparation process, relevant extraction devices (including heating reflux devices, filtration devices), concentration devices (including vacuum concentration devices), purification devices (including AB-8 macroporous adsorption resin columns, eluent collection devices), drying devices (including vacuum concentration devices, vacuum drying devices) and pulverization devices (including grinders) will be applied.

[0027] The beneficial effects of the present invention are as follows:

[0028] By optimizing the extraction solvent, extraction conditions and purification method, the present invention effectively solves the problems of low extraction efficiency, high impurity content, complex process and solvent residue in the prior art, and provides a preparation method of Alpinia oxyphylla extract that is efficient, stable and suitable for industrial production. This process has the advantages of high extraction efficiency, high product purity, simple operation, good safety, etc., and has broad application prospects. Specifically:

[0029] (1) High-efficiency extraction: The present invention uses 70-80 vol% methanol as the extraction solvent and combines the reflux extraction method, which significantly improves the extraction rate of fat-soluble components in Alpinia oxyphylla, increases by more than 30% compared with the traditional water extraction method, and shortens the extraction time to 1.5 hours.

[0030] (2) High-purity product: Through purification with AB-8 macroporous adsorption resin, the impurity content in the extract can be reduced to less than 5%, and the purity of the target component can reach more than 90%, meeting the quality requirements of drugs and health products.

[0031] (3) Process simplification: The present invention optimizes the extraction and purification steps into two steps, with simple operation, shortens the production cycle by 50%, is suitable for industrial production, and reduces the production cost.

[0032] (4) High safety: Through the concentration and vacuum drying processes, the residual organic solvents are completely removed, ensuring that the final product meets the drug safety standards and has no risk of solvent residue. Detailed implementation manners

[0033] To make the objectives, technical solutions and advantages of the present invention clearer, the technical solutions of the present invention will be described in detail below. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. All other implementation manners obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts fall within the scope protected by the present invention.

[0034] Example 1

[0035] This embodiment provides a method for preparing an extract of Alpiniae Oxyphyllae Fructus, and the preparation method includes the following steps:

[0036] (1) Extraction: Take 100 g of Alpiniae Oxyphyllae Fructus medicinal materials, add them to 1000 g of a methanol aqueous solution with a concentration of 70 vol%, mix well, heat under reflux for 1.5 h, then filter, and collect the filtrate; add the medicinal residues to 1000 g of a methanol aqueous solution with a concentration of 70 vol% again, repeat the extraction for 1.5 h, filter, and combine the two filtrates to obtain an extract.

[0037] (2) Concentration: Concentrate the extract under reduced pressure at 60 °C until there is no alcohol smell to obtain a concentrated solution.

[0038] (3) Purification: Pass the concentrated solution through an AB-8 macroporous adsorption resin column, first wash off impurities with deionized water, and then elute the target component with 70 vol% ethanol, and collect the eluate.

[0039] (4) Drying: Concentrate the eluate under reduced pressure at 50 °C, and then dry it under vacuum to obtain a solid powder.

[0040] (5) Crushing: Further grind the solid powder into a fine powder, and pass it through an 80-mesh sieve to obtain the extract of Alpiniae Oxyphyllae Fructus.

[0041] Example 2

[0042] This embodiment provides a method for preparing an extract of Alpiniae Oxyphyllae Fructus, and the preparation method includes the following steps:

[0043] (1) Extraction: Take 100 g of Alpiniae Oxyphyllae Fructus medicinal materials, add them to 1200 g of a methanol aqueous solution with a concentration of 70 vol%, mix well, heat under reflux for 2 h, then filter, and collect the filtrate; add the medicinal residues to 1200 g of a methanol aqueous solution with a concentration of 70 vol% again, repeat the extraction for 2 h, filter, and combine the two filtrates to obtain an extract.

[0044] (2) Concentration: Concentrate the extract under reduced pressure at 65 °C until there is no alcohol smell to obtain a concentrated solution.

[0045] (3) Purification: Pass the concentrated solution through an AB-8 macroporous adsorption resin column, first wash off impurities with deionized water, and then elute the target component with 70 vol% ethanol, and collect the eluate.

[0046] (4) Drying: Concentrate the eluate under reduced pressure at 55 °C, and then dry it under vacuum to obtain a solid powder.

[0047] (5) Crushing: Further grind the solid powder into a fine powder, and pass it through a 100-mesh sieve to obtain the extract of Alpiniae Oxyphyllae Fructus.

[0048] Example 3

[0049] This embodiment provides a preparation method of Alpiniae Oxyphyllae Fructus extract, and the preparation method comprises the following steps:

[0050] (1) Extraction: Take 100 g of Alpiniae Oxyphyllae Fructus medicinal materials, add them to 1100 g of methanol aqueous solution with a concentration of 80 vol%, mix well, heat under reflux for 2 h and then filter, and collect the filtrate; Add 1100 g of methanol aqueous solution with a concentration of 80 vol% to the medicinal residues again, repeat the extraction for 2 h and then filter, and combine the two filtrates to obtain an extract;

[0051] (2) Concentration: Concentrate the extract under reduced pressure at 63 °C until there is no alcohol smell to obtain a concentrated solution;

[0052] (3) Purification: Pass the concentrated solution through an AB-8 macroporous adsorption resin column, first wash off impurities with deionized water, and then elute the target component with 70 vol% ethanol, and collect the eluate;

[0053] (4) Drying: Concentrate the eluate under reduced pressure at 53 °C, and then dry it under vacuum to obtain a solid powder;

[0054] (5) Pulverization: Further grind the solid powder into a fine powder, and pass through a 90-mesh sieve to obtain the Alpiniae Oxyphyllae Fructus extract.

[0055] Inspection Example

[0056] Take the Alpiniae Oxyphyllae Fructus extract obtained in Example 1 as the object (sample group) to conduct the content test of total flavonoids. The specific method is as follows:

[0057] (I) Sample treatment

[0058] Reference substance solution: Reference substance (rutin, batch number: PS013644, content calculated as 92.4%), accurately weigh 48.04 mg of the reference substance, dissolve it with methanol and make up the volume to 25 mL in a volumetric flask. Accurately measure 10 mL of the reference substance solution and place it in a 100 mL volumetric flask, dilute it with water and accurately make up the volume. Accurately measure 1 mL, 2 mL, 3 mL, 4 mL, 5 mL, and 6 mL of the reference substance respectively, place them in 25 mL volumetric flasks, add water to 6 mL in each flask, add 1 mL of 5% sodium nitrite solution, mix well, let stand for 6 minutes, add 1 mL of 10% aluminum nitrate solution, shake well, let stand for 6 minutes, add 10 mL of sodium hydroxide test solution, and then add water to the scale, shake well, let stand for 15 minutes. Using the corresponding reagent as the blank, according to the ultraviolet-visible spectrophotometry (General Principles 0401), measure the absorbance at a wavelength of 500 nm.

[0059] Sample solution: Weigh accurately 59.66 mg of the sample, dissolve it with methanol and make up the volume to 25 mL in a volumetric flask. Accurately measure 10 mL of the sample solution and transfer it to a 100 mL volumetric flask, dilute it with water and make up the volume accurately. Accurately measure 3 mL of the sample, transfer it to a 25 mL volumetric flask, add water to 6 mL, add 1 mL of 5% sodium nitrite solution, mix well, let it stand for 6 minutes, add 1 mL of 10% aluminum nitrate solution, shake well, let it stand for 6 minutes, add 10 mL of sodium hydroxide test solution, then add water to the scale, shake well, let it stand for 15 minutes, and measure the absorbance at a wavelength of 500 nm.

[0060] (2) Instrument parameters

[0061] Instrument: UV-2600, FX-03-051.

[0062] Colorimetric cuvette: Wonda Quantz fused silica colorimetric cuvette, 10 mm, 45 - 12.5 * 12.5 (mm).

[0063] Detection wavelength: 500 nm.

[0064] (3) Detection results

[0065] The detection results of the control group are shown in Table 1, and the detection results of the sample group are shown in Table 2.

[0066] Table 1

[0067] Control ID Concentration μg / mL WL500 0 mL 0.00000 -0.00006 1 mL 7.10223 0.09329 2 mL 14.20447 0.18281 3 mL 21.30670 0.27917 4 mL 28.40893 0.37437 5 mL 35.51117 0.46876 6 mL 42.61340 0.55880

[0068] Table 2

[0069]

[0070] It can be seen from the results that the total flavonoid content in the semen myristicae extract obtained in Example 1 is 26.5%.

[0071] As mentioned above, the above are only specific embodiments of the present invention, but the protection scope of the present invention is not limited thereto. Any person skilled in the art within the technical scope disclosed by the present invention can easily think of changes or substitutions, which should all be covered within the protection scope of the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope of the claims.

Claims

1. A method for preparing an Alpinia oxyphylla extract, characterized in that: The preparation method comprises the following steps: (1) Extraction: Mix Alpinia oxyphylla with methanol aqueous solution, reflux extraction and collect the extract; (2) Concentrating: concentrating the extract under reduced pressure to obtain a concentrated solution; (3) Purification: purifying and eluting the concentrated solution with an adsorption resin column to obtain an eluate; (4) Drying: concentrating the eluate under reduced pressure, and then vacuum drying to obtain a solid powder; (5) Crushing: The solid powder is further ground into fine powder to obtain the Alpinia oxyphylla extract.

2. The method for preparing the Alpinia oxyphylla extract according to claim 1, characterized in that: In step (1), the mass ratio of the Alpinia oxyphyllae medicinal material to the methanol aqueous solution is 1:10-12.

3. The method for preparing the Alpinia oxyphylla extract according to claim 1, characterized in that: In step (1), the volume concentration of methanol in the methanol aqueous solution is 70-80 vol%.

4. The method for preparing the Alpinia oxyphylla extract according to claim 1, characterized in that: In step (1), the reflux extraction time is 1.5 to 2 hours, and the number of reflux extractions is 2 to 3 times.

5. The method for preparing the Alpinia oxyphylla extract according to claim 1, characterized in that: In step (2), the temperature of the reduced pressure concentration is 60-65°C.

6. The method for preparing the Alpinia oxyphylla extract according to claim 1, characterized in that: In step (3), the concentrated solution is passed through an AB-8 macroporous adsorption resin column, impurities are first eluted with deionized water, and then the target component is eluted with 70 vol% ethanol, and the ethanol eluate is collected.

7. The method for preparing the Alpinia oxyphylla extract according to claim 1, characterized in that: In step (4), the temperature of the reduced pressure concentration is 50-55°C.

8. The method for preparing the Alpinia oxyphylla extract according to claim 1, characterized in that: In step (5), the powder is ground into fine powder and then passed through a 80-100 mesh sieve to obtain the Alpinia oxyphylla extract.

9. The Alpinia oxyphylla seed extract obtained by the preparation method according to any one of claims 1 to 8.

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