CN115260144B - Method for quickly preparing acacetin based on roasting and hydrolyzing herba cephalanoploris - Google Patents
Method for quickly preparing acacetin based on roasting and hydrolyzing herba cephalanoploris Download PDFInfo
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- CN115260144B CN115260144B CN202211185827.5A CN202211185827A CN115260144B CN 115260144 B CN115260144 B CN 115260144B CN 202211185827 A CN202211185827 A CN 202211185827A CN 115260144 B CN115260144 B CN 115260144B
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- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
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- C07D311/30—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only not hydrogenated in the hetero ring, e.g. flavones
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Abstract
The invention discloses a method for quickly preparing acacetin based on charring and hydrolysis of herba cephalanoploris, belonging to the technical field of preparation and separation of traditional Chinese medicine components. The preparation method specifically comprises the steps of frying the common cephalanoplos herb into charcoal, hydrolyzing a sample after the charcoal frying, separating after hydrolysis to obtain the farnesoid, and separating by utilizing a preparative high-performance liquid phase technology. Compared with the direct hydrolysis of raw herba cepbalanoplosis segeti, the fried carbon of herba cepbalanoplosis segeti can obviously improve the content of the acacetin, which indicates that the fried carbon of herba cepbalanoplosis segeti can be hydrolyzed into a method for effectively improving the content of the acacetin. The method for preparing the acacetin by using the common cephalanoplos herb which is widely distributed and low in price as the raw material can effectively save the preparation cost, has the advantages of simple operation, economy and environmental protection, can effectively improve the yield of the acacetin, realizes the one-step preparation of the acacetin, and provides a new technical method for preparing the expensive acacetin.
Description
Technical Field
The invention belongs to the technical field of preparation and separation of traditional Chinese medicine components, and particularly relates to a method for quickly preparing acacetin based on charring and hydrolysis of herba cepbalanoplosis segeti.
Background
Herba Cephalanoploris is Cephalanoploris belonging to CompositaeCirsium setosum(wild.) dried aerial parts of MB. The sources are very wide and distributed in most regions in China. Harvesting in spring and autumn, removing impurities, and sun drying. It is sweet, bitter and cool in nature. It enters heart and liver meridians. Has effects of cooling blood, stopping bleeding, removing blood stasis, removing toxic substance, and resolving carbuncle. It is commonly used to treat epistaxis, hematemesis, hematuria, stranguria with blood, hemafecia, metrorrhagia, traumatic hemorrhage, carbuncle, swelling, sore, etc. Herba Cephalanoploris mainly contains flavonoids, phenylpropanoids, lignans, terpenes, organic acids, etc., and has antiinflammatory, antibacterial, antitumor, blood pressure lowering, hemostatic, and blood coagulation effects. Clinically, the raw product is mainly used for cooling blood, and the cool property is weakened after the raw product is stir-baked to charcoal, so that the astringency and hemostasis effects are enhanced.
At present, farnesol is mostly used in scientific research and cosmetic industries, and modern researches find that the farnesol has various biological activities besides the traditional effects of resolving depression, soothing nerves, regulating qi and dredging collaterals. In recent years, farnesoid pharmacological actions studied include antioxidant action, antibacterial action, anti-osteoporosis action, cardioprotection, immunoregulation and anti-inflammatory action, neuroprotection and the like, and particularly, a wide range of antitumor actions including receptor and transcription factor inhibition, carcinogenic metabolite inhibition, cancer cell proliferation inhibition, signal pathway regulation, antitumor migration action, pro-apoptotic action, pro-angiogenic factor VEGF production inhibition and the like, thereby possibly making it an antitumor drug with a good curative effect. Therefore, the acacetin has wide medicinal prospect for preventing and treating diseases.
Farnesin is a common flavonoid in nature, and is contained in various plants such as acacia, locust tree, japanese thistle, taraxacum, cammon flower, chrysanthemum, etc., but because of its low solubility, most of them are glycosides extracted and separated from plants, and because farnesin is difficult to prepare, it is expensive at present. Most of the previous methods for extracting acacetin are chemical methods, for example, the academician extracts 95% ethanol from Chuzhou chrysanthemum by petroleum ether, then the extracts are separated by macroporous resin, 30% ethanol elution part is separated by silica gel column chromatography, chloroform-methanol (V: V,10, 2 → 2). Or extracting flos Chrysanthemi Indici ethanol extract with ethyl acetate to obtain yellow crystal, refluxing total flavone with ethanol to obtain off-white insoluble substance, and recrystallizing with pyridine and water (1. The method has the defects of long time consumption, complicated operation and large using amount of organic reagents, and the glycosides of the farnesoid are obtained by separation, so the search for the preparation method of the farnesoid, which has relatively simple method and relatively high extraction rate, has very important significance for further development and utilization of the farnesoid.
Disclosure of Invention
Aiming at the problems of complex preparation and extraction processes and low conversion rate of the acacetin in the prior art, the invention provides a method for quickly preparing the acacetin based on stir-frying and hydrolyzing of herba cepbalanoplosis segeti, the method is simple to operate, the acacetin can be quickly extracted and separated from the herba cepbalanoplosis segeti, and a technical support is provided for the preparation and research of the acacetin.
The invention is realized by the following technical scheme:
a method for rapidly preparing acacetin based on charring and hydrolysis of herba Cephalanoploris comprises charring herba Cephalanoploris, hydrolyzing the charred sample, and separating to obtain acacetin.
Further, the separation utilizes preparative high performance liquid phase technology.
Further, the hydrolysis is to crush the sample after the charring, add hydrochloric acid, ethyl acetate and water, carry out reflux hydrolysis in a water bath at 80 to 100 ℃, take the ethyl acetate layer, wash the ethyl acetate layer with water, evaporate the solvent to dryness and dissolve the solvent with methanol.
Further, the charcoal frying temperature is 350 to 400 ℃, and the frying time is 10 to 25min.
Further, the volume ratio of the hydrochloric acid to the ethyl acetate to the water is 1.
Further, the water bath reflux hydrolysis time is 10 to 15min.
Further, the preparative high performance liquid phase conditions are that a chromatographic column: CST C18, media:12nm,10 μm; the elution gradient was methanol to water (75) at a flow rate of 6mL · min -1 The detection wavelength is 350nm, and the peak emergence time of the farnesoid is 37 to 44min.
Herba Cephalanoploris contains linarin, but no albizin component, and linarin can be converted into farnesin proper conditions (acid hydrolysis or enzyme hydrolysis), but the conversion rate is low under normal conditions. The invention creatively discovers that in the frying process of the field thistle, the content of the linarin is reduced, the content of the farnesin is increased, the linarin is desugared after being heated and converted into the farnesin, but the linarin cannot be completely converted into the farnesin in the frying process, the content of the farnesin is firstly increased and then reduced along with the prolonging of the frying time, and the conversion rate of the linarin into the farnesin can be maximized by combining the frying and the acid hydrolysis. Therefore, the method creatively combines the charcoal frying and the hydrolysis, the charcoal frying temperature is 350-400 ℃, the frying time is 10-25min, the water bath reflux hydrolysis time is 10-15min, the hydrolysis time is greatly shortened, the conversion speed and the conversion rate are improved, the preparation processes of the farnesoid are adopted, and the utilization rate of the Cirsium setosum charcoal is improved.
Advantageous effects
(1) The method for preparing the acacetin by using the herba cepbalanoplosis segeti which is widely distributed and low in price as the raw material can effectively save the preparation cost, has the advantages of simple operation, economy and environmental protection, can effectively improve the yield of the acacetin, realizes the one-step preparation of the acacetin, provides a new technical method for preparing the expensive acacetin, and can provide thinking and reference for similar related researches by adopting the method of preparing chemical monomers by combining the traditional processing and modern means;
(2) The invention establishes a preparation method of the acacetin, which is rapid, environment-friendly and effective in cost reduction, provides effective sustainable resource guarantee for the acacetin, and has important significance for promoting further development and application of the acacetin.
Drawings
FIG. 1 is TLC identification spectrum of Cirsium setosum charcoal with different stir-frying degrees, wherein 1 is linarin, 2 is acacetin, 3 is Cirsium setosum reference medicinal material, and 4-8 are Cirsium setosum charcoal samples with stir-frying time of 10min,15min,20min,25min and 30min respectively;
FIG. 2 shows TLC identification spectra of herba Cephalanoploris, herba Cephalanoploris charcoal, herba Cephalanoploris hydrolysis, and herba Cephalanoploris charcoal hydrolysis, wherein 1 is linarin, 2 is acacetin, 3-4 is herba Cephalanoploris, 5-6 is herba Cephalanoploris charcoal, 7-8 is herba Cephalanoploris direct hydrolysis sample, and 9-10 is herba Cephalanoploris charcoal hydrolysis sample;
FIG. 3 is a liquid chromatogram of an acacetin control and a preparation solution of example 2, wherein 1 is an acacetin control peak and 2 is an acacetin peak in the preparation solution;
FIG. 4 is a total ion flow graph of an acacetin control (in negative ion mode);
FIG. 5 is a graph of the second level fragment of the farnesoid control;
FIG. 6 is a total ion flow graph (in negative ion mode) of the acacetin sample prepared in example 3;
fig. 7 is a secondary fragment pattern of the farnesin sample prepared in example 3.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the following clear and complete description of the technical solution of the present invention shall be included in the scope of the present application, and other similar embodiments obtained by those skilled in the art without creative efforts shall be included based on the embodiments in the present application.
In the embodiment of the invention, the common cephalanoplos herb is purchased from Shandong Baiweitang Chinese medicine decoction piece limited company, and the batch number is 210701; the composition comprises a linarin control (111528-202112, china food and drug testing institute), an acacetin control (BP 0114 Chengdupu method science and technology development Co., ltd.), and a herba Cephalanoploris control (121436-201803, china food and drug testing institute).
Example 1
(1) Respectively parching herba Cephalanoploris 50g at 400 deg.C for 10min,15min,20min,25min and 30min to obtain herba Cephalanoploris charcoal sample;
(2) Taking 1g of each of the Cirsium setosum charcoal powder with different stir-frying degrees, adding 10ml of methanol, treating for 15 minutes by ultrasonic (power 300W, frequency 40 kHz), and filtering to obtain a test solution; preparing herba Cephalanoploris reference medicinal material (raw herba Cephalanoploris) into herba Cephalanoploris reference medicinal material solution by the same method; taking appropriate amount of linarin and farnesin as reference substances, and adding methanol to obtain linarin concentrations of 0.50 mg/mL -1 The concentration of farnesoid was 0.55 mg/mL -1 The solution of (4) as a control solution;
according to the general rule of the four parts of the world in the 2020 edition of "chinese pharmacopoeia", thin layer chromatography 0502, sucking 2 μ L of each of the test solution, the control solution and the control solution, respectively spotting on a silica gel G plate, spreading to about 4cm with an ethyl acetate-methanol-water volume ratio (100: 20); as can be seen from fig. 1, after the Cirsium setosum is roasted to charcoal, the chemical components of the Cirsium setosum are changed obviously, and both the chemical components are changed to be quantitative and qualitative, wherein farnesin spots are newly appeared, the spot area of the linarin tends to be gradually reduced along with the increase of the roasting time, and when the roasting time is 30min, the linarin spots basically disappear, the area of the farnesin spots is also reduced, and the color is lightened. The acacetin is aglycone of linarin, and the acacetin generated in the process of charring is possibly obtained by desugarization of linarin after heating and is consistent with the thin-layer identification map result. Combining with the appearance of the Cirsium setosum charcoal and TLC identification results, frying at 400 deg.C for 20min is the most suitable condition for preparing Cirsium setosum charcoal.
Example 2
(1) And (3) hydrolysis of the Cirsium setosum charcoal: weighing about 6g of herba Cephalanoploris carbon powder (sieved with sieve IV) of the best stir-fried degree (400 deg.C, 20 min) of example 1, placing into round bottom flask, adding 1mL of hydrochloric acid, 25mL of ethyl acetate, 25mL of water, refluxing and hydrolyzing in 100 deg.C water bath for 10min, filtering, placing filtrate into separating funnel, collecting ethyl acetate layer, and discarding lower layer; washing the ethyl acetate layer with 20mL of water for 3 times, discarding a water layer, placing the ethyl acetate layer in an evaporation dish, evaporating to dryness, and adding methanol to dissolve to obtain a preparation solution;
(2) According to the hydrolysis method in the step (1), the raw herba cepbalanoplosis segeti is directly hydrolyzed, and the sample amount and the solvent amount are completely the same as those of the hydrolysis of the herba cepbalanoplosis segeti carbon;
(3) The identification of the raw Cirsium setosum and the hydrolysate of Cirsium setosum charcoal by TLC according to example 1 is shown in FIG. 2, in which 1 is linarin control (0.50 mg. Multidot.mL) -1 ) Spots of the solution, 2, was farnesoid control (0.55 mg. Multidot.mL) -1 ) Spots of the solution, 3-4 for the control herba Cirsii in example 1, 5-6 for the best stir-fried herba Cirsii charcoal 1g, adding methanol 10mL, treating with ultrasound (power 300W, frequency 40 kHz) for 15min, filtering the spots of the test solution, 7-8, 9-10 for hydrolyzing herba Cirsii and herba Cirsii charcoal according to step (1), evaporating ethyl acetate layer, and dissolving the spots with methanol. As shown in FIG. 2, when the Cirsium setosum is charred or hydrolyzed directly, acacetin spots are generated, but when the Cirsium setosum is charred and hydrolyzed, the acacetin spots are increased obviously compared with that of the Cirsium setosum which is just charred or hydrolyzed. Further adopting an HPLC method for content determination, and obtaining the result that the albizzia julibrissin in the sample hydrolyzed after the Cirsium setosum is fried to be charcoalThe content is 0.56mg g -1 The content of albizim in the sample which is not hydrolyzed after the fried carbon of common cephalanoplos herb is 0.49mg g -1 The content of the albizim in the sample directly hydrolyzed by the common cephalanoplos herb is 0.03 mg/g -1 The contents are the albizim content in per gram of herba Cephalanoploris or herba Cephalanoploris carbon. Although the charring of the herba cephalanoploris can cause loss, the content of the albizim in the hydrolyzed sample after the charring of the herba cephalanoploris is still far lower after conversion. The results show that compared with the hydrolysis effect, the method for improving the content of the acacetin by frying the field thistle into charcoal is more obvious, and the method for improving the content of the acacetin by frying the field thistle into charcoal and hydrolyzing the field thistle into charcoal is shown;
(4) The high performance liquid chromatogram of the acacetin reference substance and the preparation solution is shown in figure 3, wherein 1 is an acacetin reference peak, 2 is an acacetin peak in the preparation solution, the peak which can be derived from the acacetin is far away from the front impurity peak compared with the acacetin reference substance solution, and is completely separated, and the acacetin can be separated by the preparation type high performance liquid chromatography technology.
Example 3
(1) Preparation of farnesin: the prepared solution in step (1) of example 2 was injected into a preparative high performance liquid chromatograph equipped with CTS C18 Media of 12nm 10 μm, a sample size of 0.3mL, a detection wavelength of 350nm, and an elution gradient of methanol: water (75 -1 The peak time of farnesoid is 37 to 44min. When the sample introduction is carried out for 37min, the peak of the albizin in the sample is generated, the eluent is retained, the eluent is stopped to be connected after the peak generation is finished, and the eluent is concentrated to obtain an acacetin sample;
(2) Confirmation of farnesin: performing UPLC-Q-exact Orbitrap MS analysis on an acacetin reference substance and an acacetin sample, wherein the chromatographic conditions are as follows: an ACQUITY UPLC C18 column (100 mm. Times.2.1 mm,1.7 μm); mobile phase 0.1% aqueous formic acid (a) -acetonitrile (B), gradient elution: 0-3 min (95%; B)), 3-20 min (95% → 5.0% -1 (ii) a The column temperature is 35 ℃; the sample injection amount is 5 mu L;
mass spectrum conditions: ESI ion source, negative ion mode, scanning range 100-1500 m/z, and spray voltage 3500V. The temperature of the gasification tube is 350 ℃, the temperature of the capillary tube is 350 ℃, the temperature of the auxiliary gas is 320 ℃, the flow rate of the sheath gas is 40, and the flow rate of the auxiliary gas is 10.
The total ion flow graph (in negative ion mode) of the acacetin reference substance is shown in fig. 4, the secondary fragment spectrum of the acacetin reference substance is shown in fig. 5, the total ion flow graph (in negative ion mode) of the acacetin sample is shown in fig. 6, and the secondary fragment spectrum of the acacetin sample is shown in fig. 7; farnesin control and prepared farnesin profile information are shown in table 1.
TABLE 1 Acacia Senegal reference and preparation of Acacia Senegal Mass Spectroscopy information
Claims (4)
1. A method for rapidly preparing acacetin based on charring and hydrolysis of herba Cephalanoploris is characterized in that the herba Cephalanoploris is charred, a sample after charring is hydrolyzed, and the acacetin is obtained by separation after hydrolysis;
the hydrolysis is to crush the sample after the charcoal frying, add hydrochloric acid, ethyl acetate and water, carry out reflux hydrolysis in a water bath at the temperature of 80-100 ℃, wash an ethyl acetate layer with water, evaporate the solvent to dryness and dissolve the solvent with methanol;
the charcoal frying temperature is 350-400 ℃, and the frying time is 10-25 min;
the water bath reflux hydrolysis time is 10-15 min.
2. The method for rapidly preparing acacetin based on the charring and hydrolysis of Cirsium setosum as claimed in claim 1, wherein the separation is performed by preparative high performance liquid chromatography.
3. The method for rapidly preparing acacetin based on the roasted and hydrolyzed Cirsium setosum charcoal according to claim 1, wherein the volume ratio of the hydrochloric acid to the ethyl acetate to the water is 1.
4. The rapid preparation of acacetin based on charring and hydrolysis of Cirsium setosum as claimed in claim 2The method is characterized in that the preparative high performance liquid phase conditions are that a chromatographic column: CST C18, media:12nm,10 μm; the elution gradient was methanol to water 75, and the flow rate was 6mL min -1 The detection wavelength is 350nm, and the peak emergence time of the farnesoid is 37-44 min.
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| CN101891727A (en) * | 2009-05-22 | 2010-11-24 | 湖北中烟工业有限责任公司 | Method for separating and extracting apigenin, acacetin-7-O-beta-D-glucoside and apigenin-7-O-beta-D-glucoside from dendranthema indicum |
| CN102204945A (en) * | 2011-05-18 | 2011-10-05 | 江西中医学院 | Extraction method of herba cirsii japonici carbonisatum general flavone liquid |
| CN103012346B (en) * | 2012-12-27 | 2014-12-31 | 成都普思生物科技有限公司 | Preparation method of pectolinarigenin monomer |
| CN106701856A (en) * | 2015-07-28 | 2017-05-24 | 中国科学院大连化学物理研究所 | Method for preparing acacetin by enzymatic hydrolysis of buddleoside |
| CN105294628B (en) * | 2015-11-11 | 2017-07-07 | 同济大学 | A kind of method that separation from chrysanthemum indicum prepares flavones ingredient |
| CN110721178A (en) * | 2019-11-08 | 2020-01-24 | 河南中医药大学 | Application of acacetin extracted from Huai chrysanthemum in preparing estrogen-like medicine |
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