119results about "Quinone separation/purification" patented technology

The invention relates to the technical field of separation and purification of radix arnebiae seu lithospermi, in particular to a naphthoquinone compound in radix arnebiae seu lithospermi, a preparation method of the naphthoquinone compound and application of the naphthoquinone compound in preparation of drugs for treating cervical carcinoma, the naphthoquinone compound in radix arnebiae seu lithospermi is chemically named as (Z)-2-ethoxy-5, 8-dihydroxy-3-(4-methyl-1, 3-pentadiene-1-yl) naphthalene-1, 4-diketone, and the structural formula of the naphthoquinone compound is shown in the description. The naphthoquinone compound in the lithospermum is disclosed for the first time, in-vitro anti-tumor pharmacodynamic experiments are carried out on the naphthoquinone compound in the lithospermum, and the experiments show that the naphthoquinone compound in the lithospermum has a certain inhibition effect on human Hela cells; therefore, the naphthoquinone compound in the radix arnebiae seu lithospermi can be applied to preparation of drugs for preventing / treating cervical cancer.

This invention relates to a drug for treating neuroinflammation and its application, belonging to the field of pharmaceutical technology. This invention isolates and identifies novel terphenyl compounds from the acetone extract of *Thelephora ganbajun* Zang, and provides a method for the extraction and separation of these new compounds. The acetone extract is obtained by extracting dried fruiting bodies of *Thelephora ganbajun* Zang with acetone, and then separated by normal-phase silica gel column chromatography, reversed-phase silica gel (ODS) column chromatography, and high-performance liquid chromatography (HPLC). The novel compounds of this invention can serve as potential lead compounds for the preparation of drugs for treating neuroinflammation-related diseases.

The utility model discloses a self-cleaning type 2-ethyl anthraquinone reaction kettle, which comprises a kettle body, a plurality of ingress pipes outwards penetrate through the inner part of the upper side of the cylindrical outer wall of the kettle body, the plurality of ingress pipes are vertical to the central axis of the kettle body and are arranged in a central symmetry manner, and a stirring motor is arranged at the center of the upper end of the kettle body. A stirring shaft is rotatably connected to the center of the lower end of the stirring motor, a plurality of stirring rods are fixedly connected to the cylindrical outer wall of the stirring shaft, the outer side of the lower end of the kettle body is communicated with a guide-out pipe, a plurality of supporting legs are fixedly connected to the outer side of the lower end of the kettle body, and a flow dividing baffle ring is fixedly connected to the lower side of the cylindrical inner wall of the kettle body; a blocking ring, a limiting ring, a blocking spring, a connecting sliding rod and a blocking check block are arranged in one end, far away from the kettle body, of the ingress pipe, when a raw material pipeline is connected with the ingress pipe, the number of the ingress pipe is selected according to the variety and number of raw materials, the raw materials are introduced to push the blocking check block to form a flow guide gap to enable the raw materials to enter, and the unused ingress pipe can be automatically blocked; raw material leakage is prevented.

The invention discloses a two-dimensional organic transverse heterogeneous crystal and a preparation method and application thereof.According to the preparation method, a step-by-step micro-spacing air sublimation method is adopted, the growth temperature of a secondary crystal is precisely regulated, effective control over the molecular diffusion and deposition process is achieved, and the yield of the two-dimensional organic transverse heterogeneous crystal is improved. And the two-dimensional organic transverse heterogeneous crystal with the adjustable epitaxial layer thickness can be simply and conveniently prepared. According to the invention, unique optical characteristics of the two single-component crystals are fully utilized, and optical signal emission of different wavebands can be realized at different polarization angles. By means of the characteristic, the wide application potential is achieved in the fields of optical sensing, optical communication and the like, and the requirement for diversity of optical signal wavebands can be met.

The application provides a method for preparing 2-hydroxy-1,4-naphthoquinone, which comprises the following steps: S1: dispersing 2-naphthol, a phase transfer catalyst and a base in water to obtain a 2-naphthol alkali solution; S2: adding a hypochlorite aqueous solution to the 2-naphthol alkali solution at 5-30 DEG C, and then increasing the temperature to 50-60 DEG C to react, so that 2-naphthol is oxidized to an intermediate isomerization and rearrangement to generate 2-hydroxy-1,4-naphthoquinone salt, and a 2-hydroxy-1,4-naphthoquinone salt solution is obtained; S3: adjusting the pH of the 2-hydroxy-1,4-naphthoquinone salt solution, so that the 2-hydroxy-1,4-naphthoquinone salt is converted into 2-hydroxy-1,4-naphthoquinone and precipitated, and a 2-hydroxy-1,4-naphthoquinone crude product is obtained. The method uses 2-naphthol as a raw material, and high-purity and high-yield 2-hydroxy-1,4-naphthoquinone is obtained, while the safety hazards and environmental burdens caused by the use of a large amount of peroxide oxidants and metal catalysts are avoided, the process flow is simplified, and the method is more suitable for industrialization.

The invention discloses a naphthocycline type pentacyclic aromatic polyketone compound. The structural formula of the naphthocycline type pentacyclic aromatic polyketone compound is as shown in a formula (I): # imgabs0 #. According to the invention, six naphthocycline type pentacyclic aromatic polyketone compounds are separated from a rice fermentation product of actinomycetes Streptomyces sp.NAK5495 for the first time, and the six naphthocycline type pentacyclic aromatic polyketone compounds are separated from rice fermentation products of actinomycetes Streptomyces sp.NAK5495; according to the present invention, with the medium-pressure liquid chromatography (MPLC) system and the semi-preparative HPLC separation and purification technology, the efficient separation and purification of the naphthocycline pentacyclic aromatic polyketones are achieved, and the recovery rate and the purity of the target compound are improved.

The invention discloses a novel crystal form of menadione and a preparation method, and relates to the technical field of organic chemistry. The novel crystal form comprises a crystal form T, and the crystal form T has diffraction peaks when the 2theta value is 9.970 + / -0.2 degrees, 12.250 + / -0.2 degrees, 14.978 + / -0.2 degrees and 19.141 + / -0.2 degrees. The preparation method of the novel crystal form comprises the following steps: dissolving a menadione crude product in a mixed solvent composed of an ester solvent and an alcohol solvent, cooling to 10-20 DEG C, and crystallizing to obtain the menadione crystal form T; the menadione crystal form T obtained through the method is a novel crystal form, the crystal form is good in stability and solubility, a solvent system is environmentally friendly, solvent residues are very small, the risk is low, the medication safety is better guaranteed, the defects of an existing crystal form can be overcome, and high economic benefits and social benefits are achieved.

The present invention relates to the field of chemical synthesis technology, and in particular to a 2-ethylanthraquinone synthesis production line. According to the order of synthesis, it includes an acylation hydrolysis reaction module, a precipitation and dehydration module, a closed-loop reaction module, a crude product cleaning and separation module, and a crude product refining module connected by pipelines; acylation and hydrolysis are first completed inside the acylation hydrolysis reaction module. Then enter the precipitation and dehydration module for precipitation and dehydration, and then enter the closed-loop reaction module to complete the closed-loop reaction. After the closed loop is completed, enter the crude product cleaning and separation module for alkali washing separation and water washing separation to obtain a crude product, and these crude products finally enter the crude product refining module for refining to obtain a final product. The synthesis production line of the present invention has a simple structure, can be reacted using a solid catalyst, is more environmentally friendly, and has lower cost.

The application belongs to the field of photodynamic therapy, and specifically discloses a vitamin K co-crystal material for photodynamic therapy and a preparation method thereof. The vitamin K co-crystal material takes vitamin K as an electron acceptor, and the two carbonyl groups at the para positions of the vitamin K quinoid six-membered ring make the vitamin K exhibit electron deficiency, form an organic charge transfer complex with the electron acceptor, and self-assemble to form a co-crystal, so that the absorption spectrum of the system is widened, a wider wave band of light is more effectively utilized, the photodynamic therapy response wavelength of the vitamin K is adjusted from the ultraviolet region to the visible region and the near infrared region, the problem of low penetration depth and light damage caused by photodynamic therapy using light in the ultraviolet region is avoided, and the vitamin K has excellent photodynamic performance and good application prospects in surface sterilization and disinfection, treatment of body surface infection, and directional cancer treatment based on visible light or near infrared light.

The present invention relates to a cocrystal of coenzyme QH and nicotinamide, its preparation method and use. Compared with conventional coenzyme QH, the cocrystal has a higher melting point and better stability. The preparation method of the cocrystal of coenzyme QH is simple, easy to control, and has good reproducibility. The present invention greatly improves the convenience of using coenzyme QH, saves costs during storage, transportation and use, and expands the application scope of coenzyme QH.

The invention discloses a cassia seed anthraquinone extraction process parameter optimization method based on machine learning, particularly relates to the field of medicinal material extraction processes, and is used for solving the problem that the same group of extraction process parameters are difficult to stably reuse due to fluctuation of different batches of cassia seed raw materials. The method comprises the following steps: by taking a dry basis free anthraquinone content index as a unique batch characterization parameter, retrieving a batch similar sample set to generate an initial parameter group, performing short-time probe extraction under the initial parameter group, collecting a primary stage sample solution, calculating a dry basis release to miscellaneous peak ratio, and comprehensively analyzing to obtain a net release coefficient; an optimization mode mark is generated according to the net release coefficient to limit a process window and operable rule strength, then a regression prediction model is trained in the limited window to output a target parameter set, an executable target parameter set is determined, and stability and reusability of process parameter optimization are achieved.

The invention discloses a method for extracting and separating effective components of traditional Chinese medicine polygonum multiflorum, which comprises the following steps of: firstly, crushing the polygonum multiflorum into powder by using a crusher, and sufficiently drying the polygonum multiflorum powder; adding the dried polygonum multiflorum powder into a solution formed by mixing benzene and sulfuric acid, thoroughly stirring, and standing for a period of time for later use; filtering the polygonum multiflorum solution after standing so as to obtain polygonum multiflorum mother liquor and polygonum multiflorum filter residues; the method comprises the following steps: adding a mixed solution of benzene and benzene-ethyl acetate into polygonum multiflorum filter residues, and stirring at the same time; according to the method for extracting and separating the effective components of the traditional Chinese medicine polygonum multiflorum, the requirement on equipment required for extracting the effective components in the polygonum multiflorum is reduced by adopting a multi-time extraction mode, so that the cost required for extracting the effective components in the polygonum multiflorum is reduced, and the technical requirement required for extraction is reduced.

The application discloses a tobacco endophytic fungus metabolite, a preparation method and application in tobacco alternaria alternata prevention and treatment, and relates to the technical field of microbial natural product pesticides. The tobacco endophytic fungus metabolite is a benzoquinone compound peniquinone L, and a structural formula is as follows: The benzoquinone compound peniquinone L is produced by fermentation of tobacco endophytic fungus Aspergillus aculeatus Aspergillus aculeatus Aa-1, and scale fermentation and preparation production are easy to carry out. The tobacco endophytic fungus metabolite benzoquinone compound peniquinone L of the application has inhibitory activity on various agricultural pathogens, and has significant bacteriostatic activity on tobacco alternaria alternata in particular, with an MIC value of 2 μg / mL, which is superior to positive drug carbendazim, and can be used as a leading compound or a new microbial natural product pesticide for tobacco alternaria alternata prevention and treatment.

The invention belongs to the technical field of extraction of plant extracts, and particularly relates to an extraction method and an identification method of a 2-methoxy-1, 4-naphthoquinone compound in impatiens balsamina. The method comprises the following steps: soaking the overground part of impatiens balsamina with ethyl acetate, and then carrying out ultrasonic disruption, flash extraction, standing and solid-liquid separation to obtain a crude extract; the crude extract is sequentially subjected to first silica gel column chromatography, second silica gel column chromatography and recrystallization, and the 2-methoxy-1, 4-naphthoquinone compound is obtained. According to the extraction method provided by the invention, the high-purity 2-methoxy-1, 4-naphthoquinone compound can be obtained, meanwhile, the extraction method is simple, convenient, stable and reliable, and is suitable for large-scale production, and conditions are created for development and utilization of the 2-methoxy-1, 4-naphthoquinone compound.

The invention discloses a method for preparing menadione and heptaene menadione by utilizing supercritical fluid chromatography. The method for preparing the menadione and the heptaene menadione by using the supercritical fluid chromatography comprises the following steps: dissolving a sample containing the menadione and the heptaene menadione by using a dissolving reagent to prepare a test solution; carrying out supercritical fluid chromatographic separation on the test solution to respectively prepare the menadione and the heptaene menadione; the supercritical fluid chromatographic separation conditions are as follows: a mobile phase is a mixture of supercritical CO2 and an alkane solvent; the stationary phase comprises silica gel. The provided method for preparing menadione and heptaene menadione by using supercritical fluid chromatography realizes the separation of heptaene menadione and heptaene menadione, can reduce the use of organic reagents, and has the advantages of short separation time and good separation effect.

The invention relates to the technical field of organic synthesis, in particular to a synthetic method of 2, 5-dibromobenzoquinone, which takes hydroquinone as an initial raw material and comprises the following two steps: step 1, adding 0.5-2% (based on the mass of hydroquinone) of a phase transfer catalyst (such as tetrabutylammonium bromide) into a glacial acetic acid solvent, reacting with bromine at 10-15 DEG C to generate 2, 5-dibromohydroquinone, and reacting for 2-4 hours at the temperature of 10-15 DEG C to obtain 2, 5-dibromohydroquinone; after the reaction, stably storing an intermediate under the protection of inert gas; 2, oxidizing the 2, 5-dibromohydroquinone into 2, 5-dibromobenzoquinone at the temperature of 45-50 DEG C by taking acetonitrile as a solvent and adopting a tert-butyl hydroperoxide (TBHP)-sodium nitrite composite oxidant (the molar ratio is (10: 1)-(15: 1)); meanwhile, glacial acetic acid and acetonitrile mother liquor generated in the reaction process are subjected to vacuum rectification recovery (the acetonitrile recovery rate is greater than or equal to 90%, and the glacial acetic acid recovery rate is greater than or equal to 88%) for recycling. The invention solves the problems of more brominated byproducts, low oxidation efficiency, solvent waste and unstable intermediate in the prior art.

The invention discloses an organic photo-thermal eutectic material based on crown ether derivatives and a preparation method and application thereof, and relates to the technical field of organic photo-thermal materials. Wherein the organic eutectic material is a host-guest eutectic formed by assembling an electron-rich donor molecule crown ether derivative and an electron-deficient acceptor molecule through a charge transfer effect. Compared with a single subject or object, the eutectic material has a remarkable near-infrared light absorption characteristic and can be applied to interface water evaporation. Tedious and complex molecular design and synthesis processes are avoided, the preparation process is simple and easy to implement, and meanwhile, the polyurethane foam loaded with the organic photo-thermal eutectic material shows an excellent water evaporation advantage and shows a great potential application value in the fields of seawater desalination and the like.

It is an object of the present disclosure to provide a method for producing a reduced coenzyme Q10 Form II crystal or a crystalline solid thereof, which is excellent in the filterability of a slurry containing a reduced coenzyme Q10 Form II crystal.The present embodiment is a method for producing a reduced coenzyme Q10 Form II crystal or a crystalline solid thereof, including: adding a reduced coenzyme Q10 Form II crystal as a seed crystal to a mixed solution containing an alcohol and a reduced coenzyme Q10; and precipitating a reduced coenzyme Q10 Form II crystal in the mixed solution after adding the seed crystal, wherein a change rate of formazin turbidity (FTU) is maintained at 15 FTU / min or more for 80% or more of a period during which the formazin turbidity (FTU) shifts from 1,000 to 10,000 in the precipitation.

The invention relates to the technical field of preparation of natural products, in particular to a high-efficiency preparation method of active ingredients of semen cassiae seeds, anthraquinone compounds are purified by adopting linear gradient countercurrent chromatography, and two gradient mobile phases are adopted: n-hexane / ethyl acetate / methanol / water (5: 5: 5: 5, v / v) and (5: 5: 8: 2, v / v); n-hexane / ethyl acetate / methanol / water (5: 5: 5.5: 4.5, v / v) and (5: 5: 7: 3, v / v) are solvent systems for internal circulation separation; n-hexane / ethanol / water (1: 1: 0.2, v / v) is used as a solvent system of an off-line two-dimensional separation mode, and the separated substances are detected and analyzed through high performance liquid chromatography to obtain nine anthraquinone compounds.

The application discloses a diterpenoid compound and a preparation method and application thereof, and belongs to the technical field of medicines.The diterpenoid compound provided by the application has a structure as shown in the following formula (I): in the formula (I), R1 is selected from hydrogen or acetoxy; R2 is selected from hydrogen, hydroxyl or methoxy; and R3 is selected from hydrogen or hydroxyl.The diterpenoid compound has high affinity to a PXR target point, has a significant anti-inflammatory effect, can activate the PXR target point in the intestinal tract, regulate the level of inflammatory factors, has a significant effect on treating inflammatory bowel disease, and is a natural extract, has the advantages of significant curative effect and low toxicity, and has wide application in the preparation of a PXR agonist or a medicine for treating inflammatory bowel disease.

The invention provides an anthraquinone dimer compound which is extracted from fermentation liquor of plant endophytic fungi and has an antibacterial effect.

The invention belongs to the technical field of deep sea microbial materials, and discloses a perylenequinone compound of Alternaria sp. Xiao20, a derivative of the perylenequinone compound, or a pharmaceutically acceptable salt of the perylenequinone compound, a preparation method of the perylenequinone compound, and an application of the perylenequinone compound and the derivative or the pharmaceutically acceptable salt of the perylenequinone compound in preparation of medicines for preventing and / or treating neuroinflammation diseases. The invention provides a perylenequinone compound or a derivative thereof separated from a fermentation product of alternaria alternata, and the perylenequinone compound or the derivative thereof has important significance on development of marine drugs; the perylenequinone compound or the derivative or the pharmaceutically acceptable salt of the perylenequinone compound disclosed by the invention can be used for inhibiting the release of a neuromicroglia inflammatory factor NO; according to the present invention, the release level of the LPS-induced nerve microglial cell inflammatory factor NO is significantly reduced, the technical effect of neuroinflammation disease treatment is achieved, and the LPS-induced nerve microglial cell inflammatory factor NO can be prepared, such that the LPS-induced nerve microglial cell inflammatory factor NO can be used for preparing the neuroinflammation disease prevention and / or treatment drug, and has important significance on neuroinflammation disease treatment and new drug development.

The invention relates to the technical field of biological medicine, in particular to a method for purifying vitamin K2 (MK-7) from bacillus natto fermentation liquor. The method comprises the following steps: concentrating a fermentation stock solution, carrying out high-pressure homogenization on the concentrated fermentation stock solution and an organic solvent, extracting vitamin K2 in the fermentation stock solution into an organic phase through high-pressure homogenization, and separating to obtain an organic phase component; the preparation method comprises the following steps: washing an organic phase component with a saturated saline solution to remove impurities, further concentrating and crystallizing to obtain a vitamin K2 crude product, further purifying the vitamin K2 crude product through melt crystallization to obtain a vitamin K2 pure product, and the purity of the obtained vitamin K2 pure product is greater than 99.9%. The method disclosed by the invention is simple in process flow and low in equipment cost, can be used for preparing a high-purity vitamin K2 product, and is convenient to apply in actual production.

The invention provides a preparation method of high-purity MK-7, which comprises the following steps: (1) putting bacillus subtilis natto dry powder into subcritical extraction equipment, and adding a mixed solvent for subcritical extraction; (2) after the extraction is completed, carrying out separation, and carrying out reduced pressure distillation to obtain a concentrated solution; (3) adding an organic solvent into the concentrated solution, stirring and dissolving, and cooling and crystallizing; (4) carrying out suction filtration separation, recrystallization and vacuum drying on the crystallized substance to obtain high-purity MK-7; in the step (1), the subcritical extraction temperature is 0-30 DEG C, and the extraction pressure is 0.5-3 MPa. The MK-7 prepared by the preparation method of the high-purity MK-7 provided by the invention has high yield and purity, the drying weight loss is obviously reduced, and the MK-7 has no fermentation peculiar smell.

The invention discloses a clean production method of a 1, 4-dihydroxy anthraquinone medical intermediate for an anti-tumor drug, a 1, 4-dihydroxy anthraquinone product is produced by the steps of feeding, reaction, hydrolysis, suction filtration and drying, and mother liquor wastewater generated in the suction filtration step is sequentially subjected to cooling crystallization and resin adsorption, so that the 1, 4-dihydroxy anthraquinone medical intermediate is obtained. Phthalic acid is obtained after phthalic acid desorption, resin regeneration and phthalic acid refining treatment, phthalic acid is dried and then reused for synthesis of the 1, 4-dihydroxy anthraquinone medical intermediate, and filtrate is merged into the next batch of synthesis mother liquor wastewater to be treated. The resource recycling of the mother liquor wastewater and the clean production of the 1, 4-dihydroxyquinone can be realized, and the resource is effectively saved.

This invention discloses a cocrystal of emodin and ligustrazine, its preparation method, its composition, and its uses. Specifically, this invention discloses a novel chemical entity with a cocrystal of emodin and ligustrazine as a pharmaceutically active ingredient; a method for preparing the cocrystal of emodin and ligustrazine; and the application of the cocrystal of emodin and ligustrazine as a pharmaceutically active ingredient in the preparation of drugs for the prevention and treatment of bacterial, fungal, and viral infections, as well as for antitumor, antimalarial, diabetes, Alzheimer's disease, and sepsis, belonging to the field of pharmaceutical technology.

The present application relates to a kind of compound 2-[(full-E)3,7,11,15,19,23,27,31,35,39-decamethyl-2,6,10,14,18,22,26,30,34,38-tetracosaalkyl]-5,6-dimethoxy-3-methyl-p-benzoquinone crystal form and its preparation method and application, belong to chemical engineering crystallization field.The technical problem to be solved is to provide a crystal form with significantly improved stability, significantly improve the light stability of the compound, and further more conducive to storage and transportation, better ensure the consistency of therapeutic effect, reduce the effect fluctuation or adverse reaction caused by dissolution difference.Characteristic diffraction peak of X-ray powder diffraction pattern expressed by 2θ value ± 0.2° using Cu-Kα radiation includes 4.70, 6.25, 15.65, 17.22, 19.18, 20.45, 27.39.

The present description discloses a method for storing reduced coenzyme Q10 (QH), which is capable of controlling oxidation. A first embodiment of the present invention relates to a method for storing QH, including storing a composition containing QH and having a water activity at 25°C of 0.45 or less. A second embodiment of the present invention relates to a method for controlling oxidation of QH, including storing a composition containing QH and having a water activity at 25°C of 0.45 or less. A third embodiment of the present invention relates to a composition containing QH and having a water activity at 25°C of 0.45 or less.

The invention provides a carclazyte bed waste aluminum oxide circulating cleaning and recycling system and method, relates to the technical field, and solves the problems that an existing carclazyte bed only has an aromatic hydrocarbon feeding pipeline and is not provided with a discharging pipeline, and the aromatic hydrocarbon circulating cleaning effect cannot be achieved. The device comprises a carclazyte bed, a working liquid storage tank, a preparation kettle and a waste aromatic hydrocarbon storage tank, the bottom of the carclazyte bed is connected with a waste liquid discharge pipe, the waste liquid discharge pipe is connected with the inlet ends of a waste liquid cooler, an oil separation tank and a material pressing filter in a split-flow mode, and the outlet end of the material pressing filter is connected with the inlet end of the working liquid storage tank. The outlet end of the waste aromatic hydrocarbon storage tank is connected with the inlet ends of the working liquid storage tank and the configuration kettle through a third working pump in a shunting manner, the outlet end of the working liquid storage tank is connected with the inlet end of the configuration kettle through a first working pump, and the outlet end of the configuration kettle is connected with a waste liquid discharge pipe through a second working pump. The method has the beneficial effects that the effect of fully recycling effective auxiliary materials in the waste aluminum oxide is achieved, and the purposes of saving energy and reducing consumption are achieved.

This invention relates to a method for recovering anthraquinones from spent activated alumina using a Soxhlet extractor. The method first involves adding a solvent or mixed solvent to a reactor, then adding dried spent activated alumina to the Soxhlet extractor, which is then installed on the reactor. Heating causes the solvent to vaporize, rise, condense, and flow back into the reactor, repeating this cycle. After the experiment, the extract is rotary evaporated under reduced pressure until no more solvent is distilled off; the remaining solid is the product. This invention maximizes the recovery of anthraquinones and hydroanthraquinones. Furthermore, ethanol and cyclohexane have lower boiling points than the working solvents, resulting in lower energy consumption and a more environmentally friendly approach.