A kind of Senecio extract, preparation method and use thereof

Abstract

The invention discloses a Senecio radiata extract, a preparation method and a use thereof, and belongs to the field of medical technology. The preparation method comprises the following steps: (1) using sugar bran to fry Senecio radiata, sieving to remove bran, and obtaining processed Senecio radiata; (2) extracting the processed Senecio radiata with water to obtain a water extract; (3) adjusting the pH of the water extract, filtering, and concentrating the filtrate to obtain a thick paste; (4) adding ethanol to the thick paste, standing for precipitation, filtering, concentrating, drying, and crushing the obtained filtrate to obtain the Senecio radiata extract. The invention can control the content of adonifrin alkaloids in the Senecio radiata extract to be below 30 μg / g by improving the processing and water extraction process of Senecio radiata. Compared with the prior art, the invention significantly reduces the content of adonifrin alkaloids in the Senecio radiata extract, and effectively ensures the clinical drug safety of the Senecio radiata medicinal material.

Description

Technical Field

[0001] The invention belongs to the technical field of medicines, and in particular relates to a Senecio radiata extract, a preparation method and application thereof. Background Art

[0002] Qingre Sanjie Capsule is a Chinese patent medicine registered with the State Food and Drug Administration. It is used for acute conjunctivitis, acute pharyngitis, acute tonsillitis, acute enteritis, acute bacillary dysentery, upper respiratory tract inflammation, acute bronchitis, lymphadenitis, sore and furunculosis pain, otitis media, and dermatitis and eczema.

[0003] Senecio radiata is the main raw material of Qingre Sanjie Capsule. The specific preparation method is to take 3000g of Senecio radiata, add water and decoct twice, each time for 2 hours, filter, combine the filtrate, concentrate to a thick paste with a relative density of 1.18-1.19 (25℃), add ethanol equivalent to 1 times the amount of the thick paste, let it stand for 12 hours to precipitate, filter, recover ethanol from the filtrate, concentrate to a thick paste with a relative density of 1.30 (80℃), vacuum dry, and crush into fine powder. Senecio radiata is rich in a variety of chemical components, including volatile oil compounds, flavonoids, organic acids and pyrrolizidine alkaloid compounds. Among them, adonifrin alkaloid has severe liver toxicity. The Chinese Pharmacopoeia stipulates that the content of adonifrin alkaloid in Senecio radiata shall not exceed 0.004%. How to reduce the content of adonifrin alkaloid is of great significance to ensure the clinical drug safety of Senecio radiata medicinal materials.

[0004] CN114306406A discloses a method for preparing the effective ingredients of Senecio radiata and removing adonifrin base, comprising the following steps: (1) soaking a dried Senecio radiata sample in distilled water, heating and refluxing, and filtering while hot to obtain an extract; (2) concentrating the extract under reduced pressure, precipitating the obtained concentrate with an organic solvent, centrifuging to obtain a supernatant, retaining the precipitate and drying it; (3) concentrating the supernatant under reduced pressure, dispersing it with distilled water, separating it with a macroporous adsorption resin column, and gradient eluting it with an ethanol-water solution to obtain an eluate; (4) concentrating the eluate under reduced pressure and freeze-drying it, analyzing the content of adonifrin base in the eluate and the precipitate by LCMS technology, discarding the components with high adonifrin base content, combining the remaining components to obtain the effective ingredients, and calculating the effective ingredient yield and the content of adonifrin base. This invention can effectively reduce the content of adonifrine in the Senecio radiata extract, but this invention abandons the 10% ethanol-water solution eluate, resulting in a low yield of the Senecio radiata extract, and the complex process leads to high costs, which is not suitable for large-scale production.

[0005] In a study on the changes in the content of pyrrolizidine alkaloids in Atractylodes lancea before and after bran frying, Zan Ke et al. found that bran frying can reduce the content of pyrrolizidine alkaloids (PAs) in Atractylodes lancea (China Pharmaceutical Affairs [J], March 2023, Vol. 37, No. 3, pp. 298-303). After searching, there is no research on the removal of adonifrine from Senecio lancea using bran frying technology. Summary of the invention

[0006] The purpose of the present invention is to provide a Senecio radiata extract, a preparation method and use thereof. The preparation method can effectively reduce the content of adonifrine in the Senecio radiata extract by improving the bran frying and water extraction processes, which is of great significance for ensuring the clinical drug safety of Senecio radiata medicinal materials.

[0007] In order to achieve the above object, the present invention adopts the following technical solutions:

[0008] The invention provides a method for preparing a Senecio radiata extract, comprising the following steps.

[0009] (1) stir-frying Senecio radiata with sugar bran, sieving to remove the bran, and obtaining processed Senecio radiata;

[0010] (2) extracting the processed Senecio radix from step (1) with water to obtain a water extract;

[0011] (3) adjusting the pH of the aqueous extract obtained in step (2), filtering, and concentrating the filtrate to obtain a thick paste;

[0012] (4) adding ethanol to the thick paste obtained in step (3), allowing to stand for precipitation, filtering, concentrating, drying, and crushing the obtained filtrate to obtain the Senecio oleifera extract.

[0013] Preferably, the mass ratio of the sugar bran to the Senecio radiata in step (1) is 100:20-30.

[0014] Preferably, the preparation method of the sugar bran is: dissolving brown sugar and cyclodextrin in water, heating and refining until fish-eye bubbles appear, adding wheat bran, frying until slightly sticky to the hand, sieving, cooling, and obtaining the sugar bran.

[0015] Further preferably, the mass ratio of brown sugar, cyclodextrin and wheat bran is 30-40:5-8:100; most preferably 35:6.5:100.

[0016] Further preferably, the amount of water added is 50-70% of the mass of brown sugar.

[0017] Preferably, the water extraction in step (2) is: boiling at 98-100° C. for 4-6 hours.

[0018] Preferably, the pH value in step (3) is 10.5-11.5.

[0019] Preferably, the filtration in step (3) is as follows: cooling to room temperature (25° C.), standing for more than 10 hours, and filtering through a 0.22 μm cellulose acetate membrane.

[0020] Preferably, the amount of ethanol added in step (4) is 2-3 times the mass of the thick paste.

[0021] The invention also provides the Senecio radiata extract obtained by the preparation method.

[0022] The present invention also provides use of the Senecio radiata extract obtained by the preparation method in preparing medicines.

[0023] The present invention also provides a medicine prepared from the Senecio radiata extract obtained by the above preparation method.

[0024] Preferably, the medicine includes but is not limited to Qingre Sanjie Capsule.

[0025] The beneficial effects of the present invention are:

[0026] (1) The present invention improves the processing and water extraction process of Senecio radiata, and can control the content of adonifrin alkaloids in the Senecio radiata extract to below 30 μg / g. Compared with the prior art, the present invention significantly reduces the content of adonifrin alkaloids in the Senecio radiata extract, and effectively ensures the clinical drug safety of Senecio radiata medicinal materials.

[0027] (2) The process of the present invention is simple, low-cost, and suitable for large-scale production. DETAILED DESCRIPTION

[0028] The following describes the embodiments of the present invention in conjunction with specific examples, and those skilled in the art can easily understand other advantages and effects of the present invention from the contents disclosed in this specification. The present invention can also be implemented or applied through other different specific embodiments, and the details in this specification can also be modified or changed in various ways based on different viewpoints and applications without departing from the spirit of the present invention.

[0029] Before further describing the specific embodiments of the present invention, it should be understood that the scope of protection of the present invention is not limited to the specific embodiments described below; it should also be understood that the terms used in the examples of the present invention are for describing specific embodiments rather than for limiting the scope of protection of the present invention.

[0030] The present invention does not limit the sources of the raw materials used. Unless otherwise specified, the raw materials used in the present invention are all common commercial products in the technical field. The Senecio radiata is produced in Jiangxi, and the dried aerial part is about 5 mm in length.

[0031] Example 1

[0032] A method for preparing a Senecio radiata extract comprises the following steps.

[0033] (1) Heat a wok over medium heat, add sugar bran until smoke appears, then add Senecio radix and stir-fry until the surface color of the Senecio radix deepens, sieve to remove the bran, let cool, and obtain the processed Senecio radix;

[0034] The mass ratio of the sugar bran and Senecio is 100:25;

[0035] The preparation method of the sugar bran comprises the following steps: adding water to dissolve brown sugar and cyclodextrin, heating and refining until fish-eye bubbles appear, adding wheat bran, frying until slightly sticky to the hand, sieving, cooling, and obtaining the sugar bran; wherein the mass ratio of the brown sugar, cyclodextrin and wheat bran is 30:5:100; and the amount of water added is 50% of the mass of the brown sugar.

[0036] (2) The processed Senecio radiata in step (1) is decocted at 98-100° C. for 5 hours to obtain a water extract, wherein the mass ratio of water to Senecio radiata is 12:1.

[0037] (3) The pH of the aqueous extract obtained in step (2) was adjusted to 11, cooled to room temperature (25°C), allowed to stand for more than 10 hours, filtered through a 0.22 μm cellulose acetate membrane, and the filtrate was concentrated to obtain a thick paste with a relative density of 1.18 (25°C).

[0038] (4) Add ethanol in an amount 2.5 times the mass of the thick paste to the thick paste obtained in step (3), let it stand for precipitation, and use a 0.22 μm cellulose acetate membrane to concentrate, dry, and crush the obtained filtrate to obtain the Senecio grandiflora extract.

[0039] Example 2

[0040] A method for preparing a Senecio radiata extract comprises the following steps.

[0041] (1) Heat a wok over medium heat, add sugar bran until smoke appears, then add Senecio radix and stir-fry until the surface color of the Senecio radix deepens, sieve to remove the bran, let cool, and obtain the processed Senecio radix;

[0042] The mass ratio of the sugar bran to the Senecio radiata is 100:25;

[0043] The preparation method of sugar bran is as follows: adding water to dissolve brown sugar and cyclodextrin, heating and refining until fish-eye bubbles appear, adding wheat bran, frying until slightly sticky to the hand, sieving, cooling, and obtaining sugar bran; wherein the mass ratio of the brown sugar, cyclodextrin and wheat bran is 40:8:100; and the amount of water added is 70% of the mass of the brown sugar.

[0044] (2) The processed Senecio radiata in step (1) is decocted at 98-100° C. for 5 hours to obtain a water extract, wherein the mass ratio of water to Senecio radiata is 12:1.

[0045] (3) The pH of the aqueous extract obtained in step (2) was adjusted to 11, cooled to room temperature (25°C), allowed to stand for more than 10 hours, filtered through a 0.22 μm cellulose acetate membrane, and the filtrate was concentrated to obtain a thick paste with a relative density of 1.18 (25°C).

[0046] (4) Add ethanol in an amount 2.5 times the mass of the thick paste to the thick paste obtained in step (3), let it stand for precipitation, and use a 0.22 μm cellulose acetate membrane to concentrate, dry, and crush the obtained filtrate to obtain the Senecio grandiflora extract.

[0047] Example 3

[0048] A method for preparing a Senecio radiata extract comprises the following steps.

[0049] (1) Heat a wok over medium heat, add sugar bran until smoke appears, then add Senecio radix and stir-fry until the surface color of the Senecio radix deepens, sieve to remove the bran, let cool, and obtain the processed Senecio radix;

[0050] The mass ratio of the sugar bran to the Senecio radiata is 100:25;

[0051] The preparation method of sugar bran is as follows: brown sugar and cyclodextrin are dissolved in water, heated and refined until fish-eye bubbles appear, and then wheat bran is added and fried until it is slightly sticky to the hand, sieved, cooled, and the sugar bran is obtained; wherein the mass ratio of the brown sugar, cyclodextrin and wheat bran is 35:6.5:100; and the amount of water added is 60% of the mass of the brown sugar.

[0052] (2) The processed Senecio radiata in step (1) is decocted at 98-100° C. for 5 hours to obtain a water extract, wherein the mass ratio of water to Senecio radiata is 12:1.

[0053] (3) The pH of the aqueous extract obtained in step (2) was adjusted to 11, cooled to room temperature (25°C), allowed to stand for more than 10 hours, filtered through a 0.22 μm cellulose acetate membrane, and the filtrate was concentrated to obtain a thick paste with a relative density of 1.18 (25°C).

[0054] (4) Add ethanol in an amount 2.5 times the mass of the thick paste to the thick paste obtained in step (3), let it stand for precipitation, and use a 0.22 μm cellulose acetate membrane to concentrate, dry, and crush the obtained filtrate to obtain the Senecio grandiflora extract.

[0055] Example 4

[0056] The difference between this embodiment and embodiment 3 is that: the mass ratio of sugar bran to Senecio radiata in step (1) is 100:20; the water extraction in step (2) is: decocting at 98-100° C. for 4 hours, and the mass ratio of water to Senecio radiata is 10:1; the pH value in step (3) is 10.5; and the amount of ethanol added in step (4) is twice the mass of the thick paste.

[0057] Example 5

[0058] The difference between this embodiment and embodiment 3 is that: the mass ratio of the sugar bran to the Senecio radiata in step (1) is 100:30; the water extraction in step (2) is: boiling at 98-100° C. for 6 hours, and the mass ratio of water to the Senecio radiata is 15:1; the pH value in step (3) is 11.5; and the amount of ethanol added in step (4) is 3 times the mass of the thick paste.

[0059] Comparison Example

[0060] The difference between this embodiment and embodiment 2 is that the Senecio radiata is not subjected to the sugar bran frying treatment, and the pH value is not adjusted before the filtrate is concentrated in step (3).

[0061] Test method for the content of adonifrine: The content of adonifrine in the Senecio radiata extract was tested by referring to UPLC-MS for simultaneous determination of the contents of adonifrine and senecioide in Senecio radiata and Senecio radiata (Chinese Journal of Traditional Chinese Medicine Impurities [J], Vol. 36, No. 6, March 2011).

[0062] According to the above test method, the content of adonifrine in the Senecio radiata extracts prepared in different embodiments was detected, and the test was repeated 3 times to take the average value. The results are shown in Table 1.

[0063] Table 1 Content of adonifrine in the Senecio radiata extract of Examples 1-5

[0064]

[0065] It can be found from the above that, compared with the control example, the content of adonifrine in the Senecio radix extract obtained by the sugar bran stir-frying and water extraction method of the present invention is significantly reduced, indicating that sugar bran stir-frying can reduce the content of adonifrine in Senecio radix.

[0066] In order to further verify the technical effect achieved by the present invention, the content of adonifrine in the Senecio radiata extracts prepared in different comparative examples was detected according to the above determination method.

[0067] Comparative Example 1

[0068] The difference between this embodiment and embodiment 3 is that in the process of preparing the sugar bran, the mass ratio of brown sugar, cyclodextrin and wheat bran is 30:10:100.

[0069] Specifically:

[0070] A method for preparing a Senecio radiata extract comprises the following steps.

[0071] (1) Heat a wok over medium heat, add sugar bran until smoke appears, then add Senecio radix and stir-fry until the surface color of the Senecio radix deepens, sieve to remove the bran, let cool, and obtain the processed Senecio radix;

[0072] The mass ratio of the sugar bran to the Senecio radiata is 100:25;

[0073] The preparation method of sugar bran is as follows: adding water to dissolve brown sugar and cyclodextrin, heating and refining until fish-eye bubbles appear, adding wheat bran, frying until slightly sticky to the hand, sieving, cooling, and obtaining sugar bran; wherein the mass ratio of the brown sugar, cyclodextrin and wheat bran is 30:10:100; and the amount of water added is 60% of the mass of the brown sugar.

[0074] (2) The processed Senecio radiata in step (1) is decocted at 98-100° C. for 5 hours to obtain a water extract, wherein the mass ratio of water to Senecio radiata is 12:1.

[0075] (3) The pH of the aqueous extract obtained in step (2) was adjusted to 11, cooled to room temperature (25°C), allowed to stand for more than 10 hours, filtered through a 0.22 μm cellulose acetate membrane, and the filtrate was concentrated to obtain a thick paste with a relative density of 1.18 (25°C).

[0076] (4) Add ethanol in an amount 2.5 times the mass of the thick paste to the thick paste obtained in step (3), let it stand for precipitation, and use a 0.22 μm cellulose acetate membrane to concentrate, dry, and crush the obtained filtrate to obtain the Senecio grandiflora extract.

[0077] Comparative Example 2

[0078] The difference between this embodiment and embodiment 3 is that: cyclodextrin is not added during the preparation process of the sugar bran, and the mass ratio of brown sugar to wheat bran is 42:100.

[0079] Specifically:

[0080] A method for preparing a Senecio radiata extract comprises the following steps.

[0081] (1) Heat a wok over medium heat, add sugar bran until smoke appears, then add Senecio radix and stir-fry until the surface color of the Senecio radix deepens, sieve to remove the bran, let cool, and obtain the processed Senecio radix;

[0082] The mass ratio of the sugar bran to the Senecio radiata is 100:25;

[0083] The preparation method of sugar bran is as follows: adding water to brown sugar to dissolve it, heating and refining until bubbles appear, adding wheat bran, frying until it is slightly sticky to the hand, sieving, cooling, and obtaining sugar bran; wherein the mass ratio of the brown sugar to the wheat bran is 42:100; and the amount of water added is 60% of the mass of the brown sugar.

[0084] (2) The processed Senecio radiata in step (1) is decocted at 98-100° C. for 5 hours to obtain a water extract, wherein the mass ratio of water to Senecio radiata is 12:1.

[0085] (3) The pH of the aqueous extract obtained in step (2) was adjusted to 11, cooled to room temperature (25°C), allowed to stand for more than 10 hours, filtered through a 0.22 μm cellulose acetate membrane, and the filtrate was concentrated to obtain a thick paste with a relative density of 1.18 (25°C).

[0086] (4) Add ethanol in an amount 2.5 times the mass of the thick paste to the thick paste obtained in step (3), let it stand for precipitation, and use a 0.22 μm cellulose acetate membrane to concentrate, dry, and crush the obtained filtrate to obtain the Senecio grandiflora extract.

[0087] Comparative Example 3

[0088] The difference between this embodiment and embodiment 3 is that in step (3), the pH value of the water extract is adjusted to 12.

[0089] Specifically:

[0090] A method for preparing a Senecio radiata extract comprises the following steps.

[0091] (1) Heat a wok over medium heat, add sugar bran until smoke appears, then add Senecio radix and stir-fry until the surface color of the Senecio radix deepens, sieve to remove the bran, let cool, and obtain the processed Senecio radix;

[0092] The mass ratio of the sugar bran to the Senecio radiata is 100:25;

[0093] The preparation method of sugar bran is as follows: brown sugar and cyclodextrin are dissolved in water, heated and refined until fish-eye bubbles appear, and then wheat bran is added and fried until it is slightly sticky to the hand, sieved, cooled, and the sugar bran is obtained; wherein the mass ratio of the brown sugar, cyclodextrin and wheat bran is 35:6.5:100; and the amount of water added is 60% of the mass of the brown sugar.

[0094] (2) The processed Senecio radiata in step (1) is decocted at 98-100° C. for 5 hours to obtain a water extract, wherein the mass ratio of water to Senecio radiata is 12:1.

[0095] (3) The pH of the aqueous extract obtained in step (2) was adjusted to 12, cooled to room temperature (25°C), allowed to stand for more than 10 hours, filtered through a 0.22 μm cellulose acetate membrane, and the filtrate was concentrated to obtain a thick paste with a relative density of 1.18 (25°C).

[0096] (4) Add ethanol in an amount 2.5 times the mass of the thick paste to the thick paste obtained in step (3), let it stand for precipitation, and use a 0.22 μm cellulose acetate membrane to concentrate, dry, and crush the obtained filtrate to obtain the Senecio grandiflora extract.

[0097] The results are shown in Table 2 below.

[0098] Table 2 Content of adonifrine in the Senecio radiata extracts of Comparative Examples 1-3

[0099]

[0100] It can be seen from Comparative Examples 1, 2 and 3 in the above table that the amounts of brown sugar, cyclodextrin and wheat bran in the bran and the step of adjusting the pH and filtering before concentration have a greater impact on the adonifrin base in Senecio radiata. The present invention uses specific amounts of brown sugar, cyclodextrin and wheat bran and combines the step of adjusting the pH and filtering before concentration to significantly reduce the adonifrin base in Senecio radiata, achieving unexpected technical effects.

Claims

1. A method for preparing a Senecio radiata extract, characterized in that: The following steps are involved: (1) stir-frying Senecio radiata with sugar bran, sieving to remove the bran, and obtaining processed Senecio radiata; (2) extracting the processed Senecio radix from step (1) with water to obtain a water extract; (3) adjusting the pH of the aqueous extract obtained in step (2), filtering, and concentrating the filtrate to obtain a thick paste; (4) adding ethanol to the thick paste obtained in step (3), allowing to stand for precipitation, filtering, concentrating, drying, and crushing the obtained filtrate to obtain the Senecio radiata extract; The mass ratio of the sugar bran to the Senecio radiata in step (1) is 100:20-30; The preparation method of the sugar bran is as follows: brown sugar and cyclodextrin are dissolved in water, heated and smelted until fish eye bubbles appear, and then wheat bran is added and fried until it is slightly sticky to the hand, sieved, and cooled to obtain the sugar bran. The mass ratio of brown sugar, cyclodextrin and wheat bran is 30-40:5-8:100; The water extraction in step (2) is as follows: boiling at 98-100° C. for 4-6 hours; The pH value in step (3) is 10.5-11.

5.

2. The preparation method according to claim 1, characterized in that: The mass ratio of the brown sugar, cyclodextrin and wheat bran is 35:6.5:

100.

3. The Senecio macrophylla extract prepared by the preparation method according to any one of claims 1-2.

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