Cinnamomum camphora flavone component with anti-aging effect as well as preparation method and application of Cinnamomum camphora flavone component
Through UPLC-QTOF-MS/MS and other technologies, combined with membrane separation and high-performance liquid chromatography, the problems of resin particles crushing, high cost and toxic substance emissions during the extraction of flavonoid components in the existing technology have been successfully solved, and the efficient, environmentally friendly extraction and refining of camphor red flavonoid components have been achieved, with good anti-aging effects.
Patent Information
- Application Number
- CN202411820926.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-11
- Publication Date
- 2025-03-18
AI Technical Summary
The existing methods for purification and enrichment of flavonoid components have problems such as crushing resin particles, high cost, high energy consumption and emission of toxic and harmful substances, and it is difficult to effectively extract the red flavonoid components of camphor heads with anti-aging effects.
Ultra-high pressure liquid chromatography tandem quadratic rod time-of-flight mass spectrometry (UPLC-QTOF-MS/MS) combined with membrane separation and high-performance liquid chromatography extraction-purification coupling process, the high yield and high-purity powder of camphor red flavonoid components were obtained through multi-step extraction and purification.
It realizes efficient extraction and refining of camphor red flavonoid ingredients, with high yield and content, environmentally friendly and toxic and harmful reagent emissions during the preparation process. The obtained ingredients have good anti-aging effects and can be used for the application of drugs or health products.
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Abstract
Description
Technical Field
[0001] The invention relates to the field of extraction of functional components of plants with medicinal and edible properties, and in particular to a camphor red flavonoid component with anti-aging effect, and a preparation method and application thereof.
[0002] UPLC-QTOF-MS / MS: ultra-high pressure liquid chromatography tandem quadrupole time-of-flight mass spectrometry. Background Art
[0003] C.reticulate'Zhangshuensis', as one of the cultivated varieties of dried orange peel, has the effects of regulating qi and strengthening the spleen, drying dampness and resolving phlegm. It is not only a local specialty tree species in Zhangshu City, Jiangxi Province, China, but also identified by the Jiangxi Provincial People's Government as one of the "Ten Foods of Jiangxi", and is an authentic medicinal material for both food and medicine. It has good effects in the fields of anti-inflammatory, anti-asthmatic, inhibiting gastrointestinal smooth muscle motility, anti-tumor, and liver protection.
[0004] Aging is an inevitable natural physiological process, which is accompanied by systemic changes starting from cell structure and a general decline in the function of body tissues, leading to an increased risk of many age-related diseases (hypertension, diabetes, cardiovascular disease, and neurodegenerative diseases, etc.). At present, the aging of the global population is becoming increasingly prominent, and the necessity of anti-aging research is also increasing.
[0005] Flavonoids are a class of active phenolic compounds that are widely found in a variety of natural plants. Their structure contains a basic skeleton of C6-C3-C6, and most of them use 2-phenylchromone as the basic nucleus. They have a wide range of pharmacological activities, such as anti-oxidation, anti-aging, anti-tumor, anti-bacterial, anti-inflammatory, anti-cancer, and regulating vascular permeability. In the 2020 edition of the Chinese Pharmacopoeia, hesperidin, the content-determined component of tangerine peel, is a flavonoid compound, and relevant research reports show that the main active substance in tangerine peel is a flavonoid compound.
[0006] At present, the commonly used method for purifying and enriching flavonoid components is mainly macroporous resin adsorption, but the resin is not rigid, and excessive flow rate may cause resin particles to break, affecting adsorption efficiency; and the pretreatment and regeneration methods in the instructions for use of macroporous resins provided by different manufacturers lack unified industry standards. In the scale-up production, it increases costs, energy consumption, and the emission of toxic and hazardous substances. Summary of the invention
[0007] The purpose of the present invention is to solve at least one of the technical problems existing in the prior art, and to provide a camphor red flavonoid component with anti-aging effect and a preparation method and application thereof.
[0008] The technical solution of the present invention is as follows:
[0009] A method for preparing a camphor red flavonoid component comprises the following steps:
[0010] S1: Take the medicinal material of Camphora chinensis, cut it into strips, extract it with pure water, centrifuge it, take the supernatant as the sample test solution, perform mass spectrometry analysis by UPLC-QTOF-MS / MS method, analyze and clarify the time range of the flavonoid components of Camphora chinensis in the spectrum, and obtain the target interval for the preparation of the subsequent flavonoid components of Camphora chinensis;
[0011] S2: Take the medicinal material of Camphor Red, cut it into strips, add the extraction solvent, soak it for 30-60 minutes, then decoct it for 20-40 minutes, and filter it to obtain the medicinal liquid; add the extraction solvent to the medicinal residue again and decoct it 1-2 times, decoct it for 20-40 minutes each time, filter the medicinal liquid, and combine the medicinal liquids filtered after each decoction to obtain the crude extract of Camphor Red;
[0012] S3: removing insoluble particles and exogenous toxic and harmful substances from the crude extract of camphor red obtained in step S2 through membrane separation to obtain a clarified camphor red water extract;
[0013] S4: according to the preparation target interval of the flavonoid components of the camphor red obtained in step S1, the clarification liquid of the camphor red water extract obtained in step S3 is refined and purified by high performance preparative liquid chromatography, and the column eluate is collected to obtain a refined liquid of the flavonoid components of the camphor red;
[0014] S5: The purified liquid of the camphor red flavonoid component obtained in step S4 is concentrated and dried to obtain a camphor red flavonoid component powder.
[0015] As a preferred embodiment of the present invention, in step S1, the mass spectrometry analysis conditions are as follows:
[0016] Chromatographic column ZORBAX SB-C18, specification: 2.1×100mm, particle size 1.8μm, column temperature 30-40°C, flow rate 0.3-0.5mL / min, injection volume 0.5-2μL, detection wavelength 283nm, acetonitrile as mobile phase A, formic acid with a volume percentage concentration of 0.1-0.5% as mobile phase B for gradient elution; the elution gradient conditions are: 0-2min, 8%A; 2-10min, 8%-18%A; 10-15min, 18%-22%A; 15-20min, 22%-37%A; 20-28min, 37%A; 28-30min, 37%-90%A; 30-35min, 90%A; the ion source is an electrospray dual-spray ion source; scanning mode: positive / negative ion mode; using Auto The mass spectrum information was acquired by MS / MS information acquisition mode, ion scanning range: MS m / z 100-1500, MS / MSm / z 50-1000; curtain gas temperature 320°C; sheath gas temperature 320°C; drying gas volume flow rate 8L / min; ionization voltage +3500V / -3200V, capillary voltage 75V, collision energy 20, 40, 60eV.
[0017] As a preferred embodiment of the present invention, in step S1, the time range of the camphor red flavonoid component in the spectrum is 6-30min, that is, the target interval for the preparation of the subsequent camphor red flavonoid component is the component between 6-30min;
[0018] The main components of the target preparation interval of the camphor red flavonoid component include:
[0019] Vecinin-2, Limonin 17-β-D-glucopyranoside, Naringin, Hesperidin, Methyl Dicaffeoylquinate, 6-Demethoxytangeretin, Nobiletin, Tangeretin, 5-Demethyltangeretin.
[0020] As a preferred embodiment of the present invention, in step S2, the extraction solvent is water, the weight of the extraction solvent added each time is 5-10 times the weight of the Zhangtouhong medicinal material, and the decoction temperature is 90°C-100°C.
[0021] As a preferred solution of the present invention, step S3 at least includes the following technical features:
[0022] The filter membrane used in membrane separation is an inorganic membrane or an organic membrane, the membrane assembly is at least one of a hollow fiber membrane, a ceramic membrane, a spiral membrane, a tubular membrane or a flat membrane, the pore size of the filter membrane is 100nm-500nm, the membrane filtration flux is 0.05-2.50L / min, the membrane inlet pressure is 0-0.4MPa, and the membrane temperature is 15-35°C;
[0023] The residue on the filter membrane is washed with water, and the amount of washing water added for every 1kg-10kg of Zhangtouhong medicinal material is 5-50L.
[0024] As a preferred embodiment of the present invention, the preparation method of high-efficiency preparative liquid chromatography is as follows: the solid content of the sample is 10-30 mg / mL, the preparative liquid chromatography column is first activated with 3-6 column volumes of methanol, and then the chromatographic column is washed with 3-6 column volumes of pure water balance solution, and the loading speed is 200-400 mL / min; one or at least two of isocratic elution or step gradient elution are used;
[0025] Specifically, the preparation method comprises the steps of loading, eluting and eluting in sequence; wherein the loading volume is 10-25 L; the elution method is one elution, the elution solvent is an ethanol aqueous solution with a volume concentration of 0%-10%, the elution volume is 3-6 times the column volume, and the flow rate is 200-400 mL / min; the method for eluting the camphor red flavonoid components is one elution, the elution solvent is an ethanol aqueous solution with a volume concentration of 70%-90%, the elution volume is 3-6 times the column volume, and the flow rate is 200-400 mL / min, and the eluate is collected to obtain the camphor red flavonoid component refined liquid.
[0026] As a preferred embodiment of the present invention, in step S4, the high performance preparative liquid chromatography column filler type is silica gel, preferably including one or more of C18 (ODS), C8, C4, and C18YE.
[0027] As a preferred embodiment of the present invention, in step S5, the concentration method is one or at least two of atmospheric pressure evaporation, reduced pressure evaporation, thin film evaporation, and multi-effect evaporation;
[0028] The drying method is one or at least two of reduced pressure drying, freeze drying, microwave drying, and spray drying.
[0029] The invention also discloses a camphor red flavonoid component, which is prepared by any of the above preparation methods.
[0030] The invention also discloses an application of the camphor red flavonoid component in preparing medicines or health products with anti-aging effects.
[0031] The beneficial effects of the present invention are as follows: the present invention provides a new method for preparing flavonoid components with anti-aging effects, the method uses camphor red as a raw material, and the prepared camphor red flavonoid components have high yield and content; the preparation process has strong specificity for camphor red flavonoid components, and has the characteristics of clear preparation goals, high efficiency, high sample yield, and no toxic and harmful reagent emissions; the obtained camphor red flavonoid components have clear composition, no reagent residue, no exogenous pollutants detected, good consistency and stability, and good anti-aging effects. In addition, the present invention establishes a method for preparing camphor red flavonoid components with anti-aging effects, and has practical applications in animal models, with anti-aging potential. The method can be directly industrialized for production, and can provide technical support for the promotion of camphor red, in-depth research on the anti-aging effects of camphor red flavonoid compounds, the development of new functional foods, and the development of new drugs. BRIEF DESCRIPTION OF THE DRAWINGS
[0032] Figure 1 This is the liquid phase spectrum of the camphor red extract and the characteristic peak diagram for identification.
[0033] Figure 2 This is the liquid chromatography result of the preparation process of flavonoid components of camphor red.
[0034] Figure 3 This is a morphological diagram of L4 stage Caenorhabditis elegans.
[0035] Figure 4 Survival curve for the long-term lifespan experiment in Caenorhabditis elegans.
[0036] Figure 5 This is a graph showing the results of Caenorhabditis elegans' resistance to oxidative stress. DETAILED DESCRIPTION
[0037] In order to facilitate the understanding of the present invention, the present invention will be described more fully below with reference to the relevant drawings. Several embodiments of the present invention are given in the drawings. However, the present invention can be implemented in many different forms and is not limited to the embodiments described herein. On the contrary, the purpose of providing these embodiments is to make the disclosure of the present invention more thorough and comprehensive.
[0038] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art of the present invention. The terms used herein in the specification of the present invention are only for the purpose of describing specific embodiments and are not intended to limit the present invention. The term "and / or" used herein includes any and all combinations of one or more related listed items.
[0039] Example 1: Definition of flavonoid components of camphor red
[0040] 1) Take 5g of the medicinal material of Camphora chinensis, cut it into strips, extract it with pure water, centrifuge it, and take the supernatant as the UPLC-QTOF-MS / MS mass spectrometry sample detection liquid. The mass spectrometry analysis conditions are: chromatographic column ZORBAX SB-C18 (2.1×100mm, 1.8μm), column temperature is 35°C, flow rate is 0.4mL / min, injection volume is 1μL, detection wavelength is 283nm, acetonitrile is used as mobile phase A, and formic acid with a volume percentage concentration of 0.1% is used as mobile phase B for gradient elution; the elution gradient conditions are: 0-2min, 8%A; 2-10min, 8%-18%A; 10-15min, 18%-22%A; 15-20min, 22%-37%A; 20-28min, 37%A; 28-30min, 37%-90%A; 30-35min, 90%A. The ion source is a dual AJS ESI electrospray ion source (Dual AJS ESI); scanning mode: positive / negative ion mode; the mass spectrum information is obtained by Auto MS / MS information acquisition mode, ion scanning range: MS m / z100~1500, MS / MS m / z 50-1000; air curtain gas temperature 320℃; sheath gas temperature 320℃; drying gas volume flow rate 8L / min; ionization voltage +3500V / -3200V, capillary voltage 75V, collision energy 20, 40, 60eV. The chromatographic analysis results are shown in Figure 1 shown.
[0041] 2) According to the main components in the liquid phase results, the mass spectrometry results are analyzed to analyze the components. The analysis results are shown in Table 1 below.
[0042] Table 1 Definition results of flavonoid components in camphor red
[0043]
[0044] 3) According to the definition results of the flavonoid components of camphor red, it is clear that the time range of the flavonoid components of camphor red in the spectrum is 6-30min, that is, the target interval for the preparation of the subsequent flavonoid components of camphor red is the components between 6-30min.
[0045] Example 2: Preparation of flavonoid components of camphor red
[0046] Step 1: Cut the medicinal material of Camphor Red into shreds, take 1 kg and put it into a decoction machine, add 9.0L of pure water, soak for 30 minutes, boil at 100℃ for 30min, filter with a 200-mesh filter, collect the filtrate, add 6L of pure water to the residue, put it into the decoction machine again and boil at 100℃ for 20min, filter with a 200-mesh filter, collect the filtrate, combine the two filtrates to obtain the Camphor Red crude extract, and perform ultra-high performance liquid chromatography analysis on the crude extract sample. The chromatographic analysis results are as follows: Figure 2 As shown;
[0047] Step 2: Filter the crude extract of Camphor Red obtained in step 1 through a 500nm ceramic membrane on a membrane filtration system, with a membrane temperature of 25°C, a membrane pressure of 0.3MPa, and a membrane flux of 0.5L / min. Collect the membrane permeate, take 13L of pure water, add 500mL every 5 minutes to wash the membrane, collect the membrane permeate, and remove substances larger than 500nm. Combine the ceramic membrane permeate and the ceramic membrane permeate to obtain the Camphor Red water extract clarified liquid, and perform ultra-high performance liquid chromatography analysis on the clarified liquid sample. The chromatographic analysis results are shown in Figure 2 As shown;
[0048] Step 3: Connect the preparative liquid chromatography column (filler type: C18YE, specification: 100×153mm, filler weight 800g, particle size 30μm, column volume about 1200mL) to the high pressure liquid phase system, design the flow rate to 320mL / min, first activate the preparative liquid chromatography column with 3 times the column volume of methanol, and then rinse the chromatographic column with 3 times the column volume of pure water for balance. Subsequently, the clarified solution of the water extract of Camphor Red (sample concentration is 16.05mg / mL) is passed through the chromatographic column for purification through the system pump, and then rinsed with 3 times the column volume of pure water to remove impurities. Elute the target substance with 3 times the column volume of 70% ethanol aqueous solution, and collect the 70% ethanol eluate, which is the refined solution of Camphor Red flavonoid components. Take all the solutions for ultra-high performance liquid chromatography analysis, and the chromatographic analysis results are shown in Figure 2 As shown in the figure, it can be seen that under this preparation process, the target components are effectively retained and collected.
[0049] Step 4: After the refined liquid is subjected to rotary evaporation at 55°C to remove ethanol, it is placed in a -80°C refrigerator for 6 hours, and the pre-frozen refined liquid is placed in a vacuum freeze dryer, and vacuum freeze-dried at 0.2MPa and -80°C until all the water is removed, and the freeze-dried powder is collected, i.e., the camphor red flavonoid component powder, and the weight of the obtained sample is weighed. The content of total flavonoids in the camphor red flavonoid component sample is calculated by weighing and analyzing using ultraviolet spectrophotometry, and the total flavonoid content is about 11.00%.
[0050] Example 3: Anti-aging application test of camphor red flavonoid components
[0051] 3.1 Experimental preparation for the Caenorhabditis elegans model
[0052] 3.1.1 Preparation of buffer and culture medium
[0053] (1) M9 buffer
[0054] Accurately weigh 6g Na2HPO4, 3g KH2PO4 and 5g NaCl, add distilled water to make up to 1L, sterilize with high-pressure steam at 121℃ for 30min, add 1mL of 1mol / LMgSO4 solution sterilized by filtration through a 0.22μm filter membrane, cool and store in a 4℃ refrigerator for later use.
[0055] (2) Potassium phosphate buffer
[0056] Accurately weigh 35.6 g K2HPO4 and 108.3 g KH2PO4, add distilled water to make up to 1 L, sterilize with high-pressure steam at 121°C for 30 min, and store in a 4°C refrigerator after cooling for later use.
[0057] (3) Nematode Growth Medium (NGM)
[0058] Accurately weigh 3g NaCl, 2.5g peptone and 17g agar, add 975mL distilled water, sterilize at 121℃ high pressure steam for 30min, add 25mL potassium phosphate buffer sterilized by 0.22μm filter membrane, 1mL 1mol / L MgSO4 solution, 1mL 1mol / L CaCl2 solution and 1mL 5mg / mL cholesterol ethanol solution in sequence, mix well, pour into a culture dish, cool and solidify for use.
[0059] 3.1.2 Preparation of E. coli OP50 culture medium
[0060] Under sterile conditions, pick a single clone of E. coli OP50 and inoculate it into 6 mL of liquid culture medium, culture it in a shaker at 37°C overnight, and measure the OD value to be 0.4-0.6. Add a certain amount of E. coli OP50 bacterial solution to each NGM plate, and evenly spread the bacterial solution with a spreader. After leaving it at room temperature (20-25°C) overnight, the nematodes can be cultured.
[0061] 3.1.3 Synchronization and culture of nematodes
[0062] The nematodes were rinsed 3 times with isotonic solution M9 and centrifuged (1300r / min, 3min), 5mL of freshly prepared lysis solution (3.5mL water, 0.5mL 5M sodium hydroxide solution, 1mL bleach) was added and vortexed for 5min, then rinsed 3 times with M9 and the supernatant was removed. The lysed eggs were transferred to NGM plates pre-coated with E. coli OP50, and cultured at 20℃ for 48-60h. After synchronization to the L4 stage, the culture can be continued. The morphology of the nematodes in the L4 stage is shown in the figure. Figure 3 shown.
[0063] 3.2 Determination of long-term lifespan in C. elegans
[0064] Nematodes are a commonly used model for evaluating anti-aging effects. 5-Fluoro-2'-deoxyuridine at a final concentration of 150 μmol / L was added to the nematode growth medium to inhibit the reproduction of offspring. The surface was coated with 500 μL E. coli OP50 and 500 μL 2 mg / mL camphor red flavonoid sample solution. The blank control group was coated with 500 μL E. coli OP50 and 500 μL pure water solution. There were 3 plates in each group, and at least 30 nematodes in the L4 stage were selected for each plate. The administration time was recorded as day 0. Abnormal dead worms were removed, and the number of normal dead nematodes was recorded every day until all the nematodes died, and a survival curve was drawn. The results are as follows. Figure 4 As shown in the figure. From the results in the figure, it can be seen that compared with the blank control group, the life span of nematodes was extended to a certain extent after adding the flavonoids of camphor red. From 28 days in the blank group, it was extended to 35 days, and the life span was extended by 25.00%. This result shows that the flavonoids of camphor red have a certain anti-aging effect and can extend the life span of nematodes.
[0065] 3.3 Determination of the antioxidant stress capacity of Caenorhabditis elegans
[0066] Oxidative stress treatment has been shown to accelerate the oxidation of cells in organisms, leading to aging. Therefore, improving the body's ability to resist stress can help delay aging. Nematodes synchronized to the L4 stage were transferred to a nematode growth medium containing 150μmol / L 5-fluoro-2'-deoxyuridine, and the surface was coated with 500μL E.coliOP50 and 500μL 2mg / mL camphor red flavonoid sample solution. The blank control group was coated with 500μL E.coli OP50 and 500μL pure water solution. Cultured at 20℃ for 3d. Subsequently, exposed to 20mmoL hydrogen peroxide solution and soaked for 30min. At least 30 nematodes were taken from each group and inoculated onto a clean nematode growth medium. The number of nematodes killed in each group was recorded every hour. The results are shown in the figure. Figure 5 As shown. From the results, it can be found that all nematodes in the blank group died in 14 hours, and all nematodes in the flavonoid component group died in 19 hours. Compared with the blank group, the life span of nematodes in the flavonoid component was extended by 35.71% after hydrogen peroxide treatment. This result shows that after adding flavonoid components of flavonoids, the survival time of nematodes in a peroxidation environment can be extended to a certain extent.
[0067] In summary, the present invention proposes for the first time an extraction-refining coupling process and an engineering technology system that integrates green manufacturing technologies such as advanced extraction, membrane separation and efficient preparation as the core, which is used for the extraction and preparation of flavonoid components of camphor red, and evaluates its application potential in the process of delaying aging. On this basis, an in vivo anti-aging evaluation model for nematodes is established, and the in vivo anti-aging ability of flavonoid components of camphor red is evaluated by indicators such as nematode life span and nematode oxidative stress, providing new ideas for the prevention and treatment of global population aging. It can not only provide a new method for the large-scale extraction and preparation of functional components of medicinal and edible plants, but also provide scientific support for the use of flavonoid components of camphor red as new anti-aging food raw materials.
[0068] The invention has the characteristics of clear preparation target, high efficiency, high sample yield, no toxic and harmful reagent discharge, etc.; the obtained camphor red flavonoid component composition is clear, no reagent residue, no exogenous pollutants are detected, good consistency and stability, and has good anti-aging effect. The invention can provide technical support for the in-depth study of the biological activity of camphor red flavonoid compounds, new drug research and development, functional food development and industrial production.
[0069] The above-mentioned embodiments only express several implementation methods of the present invention, and the description thereof is relatively specific and detailed, but it cannot be understood as limiting the scope of the patent of the present invention. It should be pointed out that, for ordinary technicians in this field, several variations and improvements can be made without departing from the concept of the present invention, which all belong to the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention shall be subject to the attached claims.
Claims
1. A method for preparing a flavonoid component of camphor red, characterized in that: The following steps are involved: S1: Take the medicinal material of Camphora chinensis, cut it into strips, extract it with pure water, centrifuge it, take the supernatant as the sample test solution, perform mass spectrometry analysis by UPLC-QTOF-MS / MS method, analyze and clarify the time range of the flavonoid components of Camphora chinensis in the spectrum, and obtain the target interval for the preparation of the subsequent flavonoid components of Camphora chinensis; S2: Take the medicinal material of Camphor Red, cut it into strips, add the extraction solvent, soak it for 30-60 minutes, then decoct it for 20-40 minutes, and filter it to obtain the medicinal liquid; add the extraction solvent to the medicinal residue again and decoct it 1-2 times, decoct it for 20-40 minutes each time, filter the medicinal liquid, and combine the medicinal liquids filtered after each decoction to obtain the crude extract of Camphor Red; S3: removing insoluble particles and exogenous toxic and harmful substances from the crude extract of camphor red obtained in step S2 through membrane separation to obtain a clarified camphor red water extract; S4: according to the preparation target interval of the flavonoid components of the camphor red obtained in step S1, the clarification liquid of the camphor red water extract obtained in step S3 is refined and purified by high performance preparative liquid chromatography, and the column eluate is collected to obtain a refined liquid of the flavonoid components of the camphor red; S5: The purified liquid of the camphor red flavonoid component obtained in step S4 is concentrated and dried to obtain a camphor red flavonoid component powder.
2. The method for preparing a flavonoid component of camphor red according to claim 1, characterized in that: In step S1, the mass spectrometry analysis conditions are as follows: Chromatographic column ZORBAX SB-C18, specification: 2.1×100mm, particle size 1.8μm, column temperature 30-40°C, flow rate 0.3-0.5mL / min, injection volume 0.5-2μL, detection wavelength 283nm, acetonitrile as mobile phase A, formic acid with a volume percentage concentration of 0.1-0.5% as mobile phase B for gradient elution; the elution gradient conditions are: 0-2min, 8%A; 2-10min, 8%-18%A; 10-15min, 18%-22%A; 15-20min, 22%-37%A; 20-28min, 37%A; 28-30min, 37%-90%A; 30-35min, 90%A; the ion source is an electrospray dual-spray ion source; scanning mode: positive / negative ion mode; using Auto The mass spectrum information was acquired by MS / MS information acquisition mode, ion scanning range: MSm / z 100-1500, MS / MSm / z 50-1000; curtain gas temperature 320°C; sheath gas temperature 320°C; drying gas volume flow rate 8L / min; ionization voltage +3500V / -3200V, capillary voltage 75V, collision energy 20, 40, 60eV.
3. The method for preparing a flavonoid component of camphor red according to claim 1, characterized in that: In step S1, the time range of the camphor red flavonoid component in the spectrum is 6-30min, that is, the target interval for the preparation of the subsequent camphor red flavonoid component is the component between 6-30min; The main components of the target preparation interval of the camphor red flavonoid component include: Vecinin-2, Limonin 17-β-D-glucopyranoside, Naringin, Hesperidin, Methyl Dicaffeoylquinate, 6-Demethoxytangeretin, Nobiletin, Tangeretin, 5-Demethyltangeretin.
4. The method for preparing the flavonoid component of camphor red according to claim 1, wherein: In step S2, the extraction solvent is water, the weight of the extraction solvent added each time is 5-10 times the weight of the Zhangtouhong medicinal material, and the decoction temperature is 90°C-100°C.
5. The method for preparing the flavonoid component of camphor red according to claim 1, characterized in that: Step S3 includes at least the following technical features: The filter membrane used in membrane separation is an inorganic membrane or an organic membrane, the membrane assembly is at least one of a hollow fiber membrane, a ceramic membrane, a spiral membrane, a tubular membrane or a flat membrane, the pore size of the filter membrane is 100nm-500nm, the membrane filtration flux is 0.05-2.50L / min, the membrane inlet pressure is 0-0.4MPa, and the membrane temperature is 15-35°C; The residue on the filter membrane is washed with water, and the amount of washing water added for every 1kg-10kg of Zhangtouhong medicinal material is 5-50L.
6. The method for preparing the flavonoid component of camphor red according to claim 1, characterized in that: In step S4, the preparation method of high performance preparative liquid chromatography is as follows: the solid content of the sample is 10-30 mg / mL, the preparative liquid chromatography column is first activated with 3-6 column volumes of methanol, and then the chromatographic column is rinsed with 3-6 column volumes of pure water balance solution, and the loading speed is 200-400 mL / min; one or at least two of isocratic elution or step gradient elution are used.
7. The method for preparing the flavonoid component of camphor red according to claim 1, characterized in that: In step S4, the high performance preparative liquid chromatography column packing type is silica gel.
8. The method for preparing the flavonoid component of camphor red according to claim 1, characterized in that: In step S5, the concentration method is one or at least two of normal pressure evaporation, reduced pressure evaporation, thin film evaporation, and multi-effect evaporation; The drying method is one or at least two of reduced pressure drying, freeze drying, microwave drying, and spray drying.
9. A camphor red flavonoid component, characterized in that: The method is prepared by any one of claims 1 to 8.
10. Use of the camphor red flavonoid component as claimed in claim 9 in the preparation of medicines or health products with anti-aging effects.