Hypericum perforatum extract and preparation method thereof

Abstract

The invention discloses a hyperforin perforatum extract and a preparation method thereof. The preparation method comprises the following steps: A / firstly, cleaning and screening collected hyperforin perforatum herbs, and drying the screened hyperforin perforatum; b, pretreating the clean and dry hyperforin perforatum raw material, and crushing the hyperforin perforatum raw material by using a coarse crusher to prepare the hyperforin perforatum raw material into a powder state suitable for extraction; c, mixing the crushed hyperforin perforatum powder with an acetone solvent, and dissolving effective components in the hyperforin perforatum in a soaking manner to obtain a leaching solution; according to the method, the hyperforin perforatum is dissolved and extracted through the acetone solvent, and effective components, flavonoid compounds, volatile oil and other active substances in the hyperforin perforatum can be effectively dissolved, so that a relatively high extraction rate can be obtained, and the purity and quality of the hyperforin perforatum extract can be improved; acetone can be recycled and reused through a distillation method, so that the solvent consumption and the cost in the extraction process are reduced.

Description

Technical Field

[0001] The invention relates to the technical field of preparation of a Hypericum perforatum extract, in particular to a Hypericum perforatum extract and a preparation method thereof. Background Art

[0002] Hypericum perforatum extract can be used as a safe neurotrophic product to prevent and treat depression, regulate affective disorders and mood disorders, eliminate tension and depression, restore self-confidence and improve sleep. The active ingredient hypericin extracted from Hypericum perforatum has a significant anti-DNA and RNA virus effect, and can directly act on viral DNA such as avian influenza, swine fever, foot-and-mouth disease, interfere with the replication and reproduction of the virus and has a strong inhibitory effect on the virus;

[0003] According to Chinese patent application No.: 202310735128.1, a Hypericum perforatum extract and a preparation method thereof are disclosed, and the preparation method comprises the following steps: S1, crushing the Hypericum perforatum and then soaking and filtering; S2, adding an alkaline aqueous solution, standing and then adding ethanol to extract, concentrating, and obtaining an extract; S3, removing alcohol from the extract, allowing it to settle, and obtaining a precipitate; S4, adding a low eutectic solvent to the precipitate for treatment and precipitation; S5, adding an alcohol solvent to the precipitate treated with S4 to dissolve, filter, add activated carbon to the filtrate for treatment, filter, concentrate and dry, and obtain a Hypericum perforatum extract; the activated carbon in step S5 is successively treated with sulfuric acid acidification and weak polar solvent and then used, and has the characteristics of obtaining a Hypericum perforatum extract with a higher content of hypericin and a lower content of benzopyrene;

[0004] The existing technology effectively solves the problem of excessive benzopyrene in the extract, and has the advantage of obtaining a Hypericum perforatum extract with a higher hypericin content and a lower benzopyrene content. However, this extraction method uses multiple solvents for extraction, which not only increases the content of compounds and active substances in the Hypericum perforatum extract, but also makes it inconvenient to recycle the solvent after extraction, thereby increasing the preparation cost of the Hypericum perforatum extract.

[0005] To this end, a Hypericum perforatum extract and a preparation method thereof are provided. Summary of the invention

[0006] The object of the present invention is to provide a Hypericum perforatum extract and a preparation method thereof, which has the advantages of improving the quality of the Hypericum perforatum extract and reducing the active substances in the Hypericum perforatum, and solves the problem that the extraction method uses multiple solvents for extraction, which not only increases the content of compounds and active substances in the Hypericum perforatum extract, but also makes it inconvenient to recycle the solvent after extraction, thereby increasing the preparation cost of the Hypericum perforatum extract.

[0007] To achieve the above object, the present invention provides the following technical solution: a Hypericum perforatum extract and a preparation method thereof, the preparation method comprising:

[0008] A. First, the collected whole herb of Hypericum perforatum is washed and screened, and the screened Hypericum perforatum is dried;

[0009] B. Then, the clean and dry Hypericum perforatum raw material is pre-treated and crushed by a coarse crusher to make it into a powder state suitable for extraction;

[0010] C. Then, the crushed Hypericum perforatum powder is mixed with an acetone solvent, and the active ingredients in the Hypericum perforatum are dissolved by soaking to obtain an extract;

[0011] D. Then, the extract is filtered through a centrifuge to remove the solid residue in the extract to obtain an extract;

[0012] E. Then, the extract is concentrated by evaporating and concentrating the extract by a rotary evaporator to remove most of the solvent in the extract to obtain an extract;

[0013] F. then drying the concentrated extract by a spray dryer to obtain a powdered Hypericum perforatum extract;

[0014] G. Then, the dried Hypericum perforatum extract is sieved by a sieving machine to remove large particles to ensure uniform particle size of the Hypericum perforatum extract product;

[0015] H. Then, the obtained Hypericum perforatum extract is tested to determine the total hypericin content of the Hypericum perforatum extract to ensure the product quality of the Hypericum perforatum extract, and finally the Hypericum perforatum extract is packaged and stored.

[0016] Preferably, the Hypericum perforatum raw material in step A should be collected during the flowering period of the plant, and the content of active ingredients in the medicinal material is relatively high. The washed Hypericum perforatum raw material can be naturally dried.

[0017] Preferably, in step B, the particle size of the raw material of Hypericum perforatum is controlled to be between 2 and 5 mm to ensure that the medicinal material is fully exposed to the solvent and improve the extraction efficiency. The coarse crusher model can be GPF-630.

[0018] Preferably, in step C, the crushed Hypericum perforatum powder is added to the extraction pot, and then a sufficient amount of acetone solvent is added to cover the Hypericum perforatum powder, and the ratio of the Hypericum perforatum powder to the acetone solvent is 1:5 to 1:10, the ratio is the weight of the medicinal material: the volume of the solvent, and the solution volume formula is:

[0019] V=n / c

[0020] Where n is the amount of solute in the solution, in mol, and c is the molar concentration of the solution, in mol / L.

[0021] Preferably, the acetone may be heated during the extraction in step C, the heating temperature is controlled between 40° C. and 50° C., and the heating time is controlled between 30 minutes and 1 hour.

[0022] Preferably, in step E, the initial speed of the rotary evaporator is set at 50 to 100 rpm and gradually increases, the normal operating range is 100 to 300 rpm, and the heating temperature of the rotary evaporator is controlled between 40°C and 50°C, avoiding exceeding 50°C.

[0023] Preferably, the detection instruments in step H are HP8453UV-Vis absorption spectrometer, RE-52A rotary evaporator and HHS21-N electric constant temperature water bath, the test drugs are thin layer chromatography silica gel G, ether, ethanol, methanol, ethyl acetate ether and 85% Hypericum standard sample, and the measurement calculation formula is:

[0024] Mass content of total hypericin = (A589 × 600) / (sample mass × 870)

[0025] Where A589 is the absorbance at 589nm of HP8453UV-Vis absorption spectrometer. The measurement was performed 3 times each time and the average value was taken as the measurement result.

[0026] Compared with the prior art, the present invention has the following beneficial effects:

[0027] The present invention uses acetone solvent to dissolve and extract Hypericum perforatum, which can effectively dissolve effective ingredients, flavonoid compounds, volatile oils and other active substances in the Hypericum perforatum, thereby obtaining a higher extraction rate and improving the purity and quality of the Hypericum perforatum extract. The acetone can be recovered and reused by a distillation method, thereby reducing solvent consumption and costs in the extraction process. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 It is a schematic diagram of the preparation process of the present invention. DETAILED DESCRIPTION

[0029] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0030] The present invention provides a technical solution, a Hypericum perforatum extract and a preparation method thereof, wherein the preparation method comprises:

[0031] A. First, the collected whole herb of Hypericum perforatum is washed and screened, and the screened Hypericum perforatum is dried;

[0032] B. Then, the clean and dry Hypericum perforatum raw material is pre-treated and crushed by a coarse crusher to make it into a powder state suitable for extraction;

[0033] C. Then, the crushed Hypericum perforatum powder is mixed with an acetone solvent, and the active ingredients in the Hypericum perforatum are dissolved by soaking to obtain an extract;

[0034] D. Then, the extract is filtered through a centrifuge to remove the solid residue in the extract to obtain an extract;

[0035] E. Then, the extract is concentrated by evaporating and concentrating the extract by a rotary evaporator to remove most of the solvent in the extract to obtain an extract;

[0036] F. then drying the concentrated extract by a spray dryer to obtain a powdered Hypericum perforatum extract;

[0037] G. Then, the dried Hypericum perforatum extract is sieved by a sieving machine to remove large particles to ensure uniform particle size of the Hypericum perforatum extract product;

[0038] H. Then, the obtained Hypericum perforatum extract is tested to determine the total hypericin content of the Hypericum perforatum extract to ensure the product quality of the Hypericum perforatum extract, and finally the Hypericum perforatum extract is packaged and stored.

[0039] Embodiment 2:

[0040] In the first embodiment, the following process is added:

[0041] In step A, the raw material of Hypericum perforatum should be collected during the flowering period of the plant, and the content of active ingredients in the medicinal material is relatively high. The washed raw material of Hypericum perforatum can be naturally dried.

[0042] The preparation method comprises the following steps:

[0043] A. First, the collected whole herb of Hypericum perforatum is washed and screened, and the screened Hypericum perforatum is dried;

[0044] B. Then, the clean and dry Hypericum perforatum raw material is pre-treated and crushed by a coarse crusher to make it into a powder state suitable for extraction, and the coarse crushing particle size is controlled between 2 and 5 mm;

[0045] C. Then the crushed Hypericum perforatum powder is mixed with acetone solvent, and the active ingredients in the Hypericum perforatum are dissolved by soaking to obtain an extract, wherein the ratio of the Hypericum perforatum powder to the acetone solvent is 1:6, the heating temperature is controlled at 40°C, and the heating time is controlled at 30 minutes;

[0046] D. Then, the extract is filtered through a centrifuge to remove the solid residue in the extract to obtain an extract;

[0047] E. Then, the extract is concentrated by evaporating and concentrating the extract by a rotary evaporator to remove most of the solvent in the extract to obtain an extract. The speed of the rotary evaporator is set at 200 rpm, the heating temperature is 45° C., and the heating time is 50 minutes;

[0048] F. then drying the concentrated extract by a spray dryer to obtain a powdered Hypericum perforatum extract;

[0049] G. Then, the dried Hypericum perforatum extract is sieved by a sieving machine to remove large particles to ensure the uniform particle size of the Hypericum perforatum extract product. The drying temperature is controlled at 60° C., the drying time is 24 hours, and the sieve mesh number is 80 meshes;

[0050] H. Then, the obtained Hypericum perforatum extract is tested to determine the total hypericin content of the Hypericum perforatum extract to ensure the product quality of the Hypericum perforatum extract, and finally the Hypericum perforatum extract is packaged and stored.

[0051] Embodiment three:

[0052] In the second embodiment, the following process is added:

[0053] In step B, the particle size of the raw material of Hypericum perforatum is controlled between 2 and 5 mm to ensure that the medicinal material is fully exposed to the solvent and improve the extraction efficiency. The coarse crusher model can be GPF-630.

[0054] The preparation method comprises the following steps:

[0055] A. First, the collected whole herb of Hypericum perforatum is washed and screened, and the screened Hypericum perforatum is dried;

[0056] B. Then, the clean and dry Hypericum perforatum raw material is pre-treated and crushed by a coarse crusher to make it into a powder state suitable for extraction, and the coarse crushing particle size is controlled between 2 and 5 mm;

[0057] C. Then the crushed Hypericum perforatum powder is mixed with acetone solvent, and the active ingredients in the Hypericum perforatum are dissolved by soaking to obtain an extract, the ratio of the Hypericum perforatum powder to the acetone solvent is 1:8, the heating temperature is controlled at 45°C, and the heating time is controlled at 45 minutes;

[0058] D. Then, the extract is filtered through a centrifuge to remove the solid residue in the extract to obtain an extract;

[0059] E. Then, the extract is concentrated by evaporating and concentrating the extract by a rotary evaporator to remove most of the solvent in the extract to obtain an extract. The speed of the rotary evaporator is set at 200 rpm, the heating temperature is 45° C., and the heating time is 50 minutes;

[0060] F. then drying the concentrated extract by a spray dryer to obtain a powdered Hypericum perforatum extract;

[0061] G. Then, the dried Hypericum perforatum extract is sieved by a sieving machine to remove large particles to ensure the uniform particle size of the Hypericum perforatum extract product. The drying temperature is controlled at 60° C., the drying time is 24 hours, and the sieve mesh number is 80 meshes;

[0062] H. Then, the obtained Hypericum perforatum extract is tested to determine the total hypericin content of the Hypericum perforatum extract to ensure the product quality of the Hypericum perforatum extract, and finally the Hypericum perforatum extract is packaged and stored.

[0063] Embodiment 4:

[0064] In the third embodiment, the following process is added:

[0065] In step C, the crushed Hypericum perforatum powder is added to the extraction pot, and then a sufficient amount of acetone solvent is added to cover the Hypericum perforatum powder. The ratio of Hypericum perforatum powder to acetone solvent is 1:5 to 1:10, which is the weight of the medicinal material: the volume of the solvent. The solution volume formula is:

[0066] V=n / c

[0067] Where n is the amount of solute in the solution, in mol, and c is the molar concentration of the solution, in mol / L.

[0068] The preparation method comprises the following steps:

[0069] A. First, the collected whole herb of Hypericum perforatum is washed and screened, and the screened Hypericum perforatum is dried;

[0070] B. Then, the clean and dry Hypericum perforatum raw material is pre-treated and crushed by a coarse crusher to make it into a powder state suitable for extraction, and the coarse crushing particle size is controlled between 2 and 5 mm;

[0071] C. Then the crushed Hypericum perforatum powder is mixed with acetone solvent, and the active ingredients in the Hypericum perforatum are dissolved by soaking to obtain an extract, the ratio of the Hypericum perforatum powder to the acetone solvent is 1:10, the heating temperature is controlled at 50° C., and the heating time is controlled at 50 minutes;

[0072] D. Then, the extract is filtered through a centrifuge to remove the solid residue in the extract to obtain an extract;

[0073] E. Then, the extract is concentrated by evaporating and concentrating the extract by a rotary evaporator to remove most of the solvent in the extract to obtain an extract. The speed of the rotary evaporator is set at 200 rpm, the heating temperature is 45° C., and the heating time is 50 minutes;

[0074] F. then drying the concentrated extract by a spray dryer to obtain a powdered Hypericum perforatum extract;

[0075] G. Then, the dried Hypericum perforatum extract is sieved by a sieving machine to remove large particles to ensure the uniform particle size of the Hypericum perforatum extract product. The drying temperature is controlled at 60° C., the drying time is 24 hours, and the sieve mesh number is 80 meshes;

[0076] H. Then, the obtained Hypericum perforatum extract is tested to determine the total hypericin content of the Hypericum perforatum extract to ensure the product quality of the Hypericum perforatum extract, and finally the Hypericum perforatum extract is packaged and stored.

[0077] Embodiment five:

[0078] In the fourth embodiment, the following process is added:

[0079] The acetone may be heated during the leaching in step C, the heating temperature is controlled between 40° C. and 50° C., and the heating time is controlled between 30 minutes and 1 hour.

[0080] The preparation method comprises the following steps:

[0081] A. First, the collected whole herb of Hypericum perforatum is washed and screened, and the screened Hypericum perforatum is dried;

[0082] B. Then, the clean and dry Hypericum perforatum raw material is pre-treated and crushed by a coarse crusher to make it into a powder state suitable for extraction;

[0083] C. Then, the crushed Hypericum perforatum powder is mixed with an acetone solvent, and the active ingredients in the Hypericum perforatum are dissolved by soaking to obtain an extract;

[0084] D. Then, the extract is filtered through a centrifuge to remove the solid residue in the extract to obtain an extract;

[0085] E. Then, the extract is concentrated by evaporating and concentrating the extract by a rotary evaporator to remove most of the solvent in the extract to obtain an extract;

[0086] F. then drying the concentrated extract by a spray dryer to obtain a powdered Hypericum perforatum extract;

[0087] G. Then, the dried Hypericum perforatum extract is sieved by a sieving machine to remove large particles to ensure uniform particle size of the Hypericum perforatum extract product;

[0088] H. Then, the obtained Hypericum perforatum extract is tested to determine the total hypericin content of the Hypericum perforatum extract to ensure the product quality of the Hypericum perforatum extract, and finally the Hypericum perforatum extract is packaged and stored.

[0089] Embodiment six:

[0090] In the fifth embodiment, the following process is added:

[0091] In step E, the initial speed of the rotary evaporator is set at 50 to 100 rpm and gradually increased. The normal operating range is 100 to 300 rpm. The heating temperature of the rotary evaporator is controlled between 40°C and 50°C, avoiding exceeding 50°C.

[0092] The preparation method comprises the following steps:

[0093] A. First, the collected whole herb of Hypericum perforatum is washed and screened, and the screened Hypericum perforatum is dried;

[0094] B. Then, the clean and dry Hypericum perforatum raw material is pre-treated and crushed by a coarse crusher to make it into a powder state suitable for extraction;

[0095] C. Then, the crushed Hypericum perforatum powder is mixed with an acetone solvent, and the active ingredients in the Hypericum perforatum are dissolved by soaking to obtain an extract;

[0096] D. Then, the extract is filtered through a centrifuge to remove the solid residue in the extract to obtain an extract;

[0097] E. Then, the extract is concentrated by evaporating and concentrating the extract by a rotary evaporator to remove most of the solvent in the extract to obtain an extract;

[0098] F. then drying the concentrated extract by a spray dryer to obtain a powdered Hypericum perforatum extract;

[0099] G. Then, the dried Hypericum perforatum extract is sieved by a sieving machine to remove large particles to ensure uniform particle size of the Hypericum perforatum extract product;

[0100] H. Then, the obtained Hypericum perforatum extract is tested to determine the total hypericin content of the Hypericum perforatum extract to ensure the product quality of the Hypericum perforatum extract, and finally the Hypericum perforatum extract is packaged and stored.

[0101] Embodiment seven:

[0102] In the sixth embodiment, the following process is added:

[0103] In step H, the detection instruments are HP8453UV-Vis absorption spectrometer, RE-52A rotary evaporator and HHS21-N electric constant temperature water bath, and the test drugs are thin layer chromatography silica gel G, ether, ethanol, methanol, ethyl acetate ether and 85% Hypericum standard sample, and the measurement calculation formula is:

[0104] Mass content of total hypericin = (A589 × 600) / (sample mass × 870)

[0105] Where A589 is the absorbance at 589nm of HP8453UV-Vis absorption spectrometer. The measurement was performed 3 times each time and the average value was taken as the measurement result.

[0106] The preparation method comprises the following steps:

[0107] A. First, the collected whole herb of Hypericum perforatum is washed and screened, and the screened Hypericum perforatum is dried;

[0108] B. Then, the clean and dry Hypericum perforatum raw material is pre-treated and crushed by a coarse crusher to make it into a powder state suitable for extraction;

[0109] C. Then, the crushed Hypericum perforatum powder is mixed with an acetone solvent, and the active ingredients in the Hypericum perforatum are dissolved by soaking to obtain an extract;

[0110] D. Then, the extract is filtered through a centrifuge to remove the solid residue in the extract to obtain an extract;

[0111] E. Then, the extract is concentrated by evaporating and concentrating the extract by a rotary evaporator to remove most of the solvent in the extract to obtain an extract;

[0112] F. then drying the concentrated extract by a spray dryer to obtain a powdered Hypericum perforatum extract;

[0113] G. Then, the dried Hypericum perforatum extract is sieved by a sieving machine to remove large particles to ensure uniform particle size of the Hypericum perforatum extract product;

[0114] H. Then, the obtained Hypericum perforatum extract is tested to determine the total hypericin content of the Hypericum perforatum extract to ensure the product quality of the Hypericum perforatum extract, and finally the Hypericum perforatum extract is packaged and stored.

[0115] The total Hypericum content of the Hypericum perforatum extract obtained by extracting Hypericum perforatum according to the method in the above embodiment was tested, and the test results are shown in the following table:

[0116] Total Hypericum content determination results %

[0117]

[0118] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device. In the absence of further restrictions, the elements defined by the sentence "comprise a ..." do not exclude the existence of other identical elements in the process, method, article or device including the elements.

[0119] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A Hypericum perforatum extract and a preparation method thereof, characterized in that: The preparation method thereof comprises: A. First, the collected whole herb of Hypericum perforatum is washed and screened, and the screened Hypericum perforatum is dried; B. Then, the clean and dry Hypericum perforatum raw material is pre-treated and crushed by a coarse crusher to make it into a powder state suitable for extraction; C. Then, the crushed Hypericum perforatum powder is mixed with an acetone solvent, and the active ingredients in the Hypericum perforatum are dissolved by soaking to obtain an extract; D. Then, the extract is filtered through a centrifuge to remove the solid residue in the extract to obtain an extract; E. Then, the extract is concentrated by evaporating and concentrating the extract by a rotary evaporator to remove most of the solvent in the extract to obtain an extract; F. then drying the concentrated extract by a spray dryer to obtain a powdered Hypericum perforatum extract; G. Then, the dried Hypericum perforatum extract is sieved by a sieving machine to remove large particles to ensure uniform particle size of the Hypericum perforatum extract product; H. Then, the obtained Hypericum perforatum extract is tested to determine the total hypericin content of the Hypericum perforatum extract to ensure the product quality of the Hypericum perforatum extract, and finally the Hypericum perforatum extract is packaged and stored.

2. The Hypericum perforatum extract and the preparation method thereof according to claim 1, characterized in that: In the step A, the raw material of Hypericum perforatum should be collected during the flowering period of the plant, and the content of active ingredients in the medicinal material is relatively high. The washed raw material of Hypericum perforatum can be naturally dried.

3. The Hypericum perforatum extract and the preparation method thereof according to claim 1, characterized in that: In the step B, the particle size of the raw material of Hypericum perforatum is controlled to be between 2 and 5 mm to ensure that the medicinal material is fully exposed to the solvent and improve the extraction efficiency. The coarse crusher model can be GPF-630.

4. The Hypericum perforatum extract and the preparation method thereof according to claim 1, characterized in that: In step C, the crushed Hypericum perforatum powder is added to the extraction pot, and then a sufficient amount of acetone solvent is added to cover the Hypericum perforatum powder. The ratio of the Hypericum perforatum powder to the acetone solvent is 1:5 to 1:10, which is the weight of the medicinal material: the volume of the solvent. The solution volume formula is: V=n / c Where n is the amount of solute in the solution, in mol, and c is the molar concentration of the solution, in mol / L.

5. The Hypericum perforatum extract and the preparation method thereof according to claim 1, characterized in that: The acetone may be heated during the leaching in step C, the heating temperature is controlled between 40° C. and 50° C., and the heating time is controlled between 30 minutes and 1 hour.

6. The Hypericum perforatum extract and the preparation method thereof according to claim 1, characterized in that: In step E, the initial speed of the rotary evaporator is set at 50 to 100 rpm and gradually increases. The normal operating range is 100 to 300 rpm. The heating temperature of the rotary evaporator is controlled between 40° C. and 50° C., avoiding exceeding 50° C.

7. The Hypericum perforatum extract and the preparation method thereof according to claim 1, characterized in that: In the step H, the detection instruments are HP8453UV-Vis absorption spectrometer, RE-52A rotary evaporator and HHS21-N electric constant temperature water bath, and the test drugs are thin layer chromatography silica gel G, ether, ethanol, methanol, ethyl acetate ether and 85% Hypericum standard sample, and the measurement calculation formula is: Mass content of total hypericin = (A589 × 600) / (sample mass × 870) Where A589 is the absorbance at 589nm of HP8453UV-Vis absorption spectrometer. The measurement was performed 3 times each time and the average value was taken as the measurement result.

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