51results about "Quinone separation/purification" patented technology

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 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 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 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 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 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 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.

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.

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.

The invention relates to the technical field of microbial drugs and anti-infection drugs, in particular to dianthraquinone compounds, a preparation method and application thereof.The dianthraquinone compounds dothideomin A and derivatives dothideomin C and dothideomin D of the dianthraquinone compounds dothideomin A have good in-vitro bacteriostasis and sterilization effects on MRSA and can remarkably inhibit growth of the MRSA, the minimum inhibitory concentration is 0.8-1.3 mu g / mL, dothideomin A has a unique anti-MRSA action mechanism, and dothideomin D has a unique anti-MRSA action mechanism and can remarkably inhibit growth of the MRSA. The compound has good safety to red blood cells and mammalian cells, and drug resistance of MRSA is not easy to generate. The invention provides the inhibition effect of the dothimine A and the derivative thereof on methicillin-resistant staphylococcus aureus, and the dothimine A and the derivative thereof have wide application value in the fields of medicines and the like.

The purification process comprises the following steps: (1) crushing; (2) crude extraction; (3) silica gel acidification; (4) silica gel chloropropylation; then carrying out gradient elution by using an eluent to obtain an aurantio-obtusin crude product; and (7) purification and crystallization: purifying the crude product of the aurantio-obtusin, and crystallizing to separate out aurantio-obtusin crystals. According to the present invention, the process steps are simple and easy to perform, the time consumption is short, the solvent consumption is low, the separation purity is high, the yield is high, the purity of the obtained aurantio-obtusin can achieve more than 99.9%, the yield can achieve 73%, the requirements of scientific research on the aurantio-obtusin purity can be met, and the method is suitable for large-scale production.

The invention discloses a novel synthetic method of naphthazarin, which comprises the following steps of: 1, reacting 1, 4, 5, 8-tetramethoxynaphthalene with boron tribromide or aluminum trichloride, crystallizing to obtain a high-purity product, and distilling a solvent under reduced pressure to obtain 5, 8-dihydroxy-2, 3-dihydronaphthalene-1, 4-diketone; 2, 5, 8-dihydroxy-2, 3-dihydronaphthalene-1, 4-diketone is added into another reaction kettle, an alkali solution is added, an oxygen micro-positive pressure (0.01-0.03 MPa) is performed for a reaction, and after the reaction is finished, high-purity 5, 8-dihydroxy-2, 3-dihydronaphthalene-1, 4-diketone salt is obtained through ethanol crystallization and filtration; and adding the salt of the 5, 8-dihydroxy-2, 3-dihydronaphthalene-1, 4-diketone into another reaction kettle, adding a hydrochloric acid ethyl acetate solution, heating and reacting, and then filtering and pulping to obtain a final product. The total preparation yield gt of naphthazarin; the HPLC purity is gt; the yield is 99.6%. The route is simple and convenient to operate and easy to implement, raw materials are cheap and easy to obtain, reaction conditions are mild, high-temperature and high-pressure reaction is not needed, and requirements on equipment are reduced. The whole route is safer to the environment, and green and pollution-free production can be realized.

The invention belongs to the technical field of natural product chemical synthesis and antibacterial application, and provides a preparation method and application of an alkannin polymer, and the preparation method comprises the following steps: dissolving an alkannin pure product or a derivative thereof as an initial raw material in an organic solvent, adding an acid catalyst, and reacting for 6-24 hours in a pressure-resistant pipe at 80-120 DEG C; performing reduced-pressure evaporation drying and reduced-pressure suction filtration on the reaction liquid, and performing vacuum drying for 1-12 hours to obtain an alkannin dimer crude product; dissolving the crude product with methanol or acetone which is 2-3 times of the weight of the crude product, adding silica gel which is 1-3 times of the weight of the crude product, and stirring; purifying the mixed material by normal phase column chromatography; carrying out silica gel thin layer chromatography detection, combining fractions with the same color development characteristics and separation coefficients, and concentrating to obtain a pure product; according to the invention, gram-scale synthesis is realized by combining biogenic approach analysis with a biomimetic synthesis strategy, and meanwhile, the antibacterial activity of the antibacterial agent is determined, so that a novel natural antibacterial agent is provided for the fields of agriculture and food.

The present invention provides soil conditioners, nitrification inhibitors, fertilizers, and methods for inhibiting nitrification, which can be used in a wide range of regions from tropical to temperate zones and utilize compounds or derivatives thereof that can be easily obtained from naturally derived materials. [Solution] A soil conditioner comprising one or more compounds selected from the group consisting of 5-hydroxy-2-methyl-1,4-naphthoquinone, 2,3-dichloro-5,8-dihydroxy-1,4-naphthoquinone, and 2,7-dimethoxy-1,4-naphthoquinone, or salts thereof, or solvates thereof, as an active ingredient.

A method of preparing a diterpenoid composition is provided. The method comprises the following steps: extracting a lysimachia capillipes material to obtain an extracted composition; and performing a series of separation steps to obtain at least one target extract of isolated diterpenoids of lysimachia capillipes. There is also provided a diterpenoid composition obtained by the method, an oral composition comprising the diterpenoid composition, a composition comprising at least one diterpenoid extract of lysimachia capillipes, the use of the composition in the preparation of a medicament for the treatment of hyperglycemia and / or hyperlipidemia in a subject, and the use of the composition in the treatment of hyperglycemia and / or hyperlipidemia in a subject. And methods of treating hyperglycemia and / or hyperlipidemia in a subject.

This invention discloses a rhein-piperazine cocrystal, its preparation method, its composition, and its uses. Specifically, this invention discloses a novel chemical entity with rhein-piperazine cocrystal as a pharmaceutically active ingredient; a method for preparing the rhein-piperazine cocrystal; and the application of the rhein-piperazine cocrystal 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 treatments, belonging to the field of pharmaceutical technology.

The utility model relates to the technical field of purification barrels, and discloses a rectification purification barrel for anthraquinone production, which comprises a stirring mechanism, a purification mechanism and a discharging mechanism. During use, a material enters the stirring barrel through the feeding pipe, a solvent is added according to the proportion and enters the stirring barrel through the solvent pipe, at the moment, a heating rod heats the material in the stirring barrel through heating, meanwhile, a fixing block is fixed to the inner wall of the stirring barrel, a fixing column is fixed to the outer wall of the fixing block, and a motor is fixed to the interior of the fixing column. The fixing column protects the motor from being damaged by high temperature and liquid, the fixing rod is fixed to the output end of the motor, the stirring blades are fixed to the outer wall of the fixing rod, the contact area between a solvent and raw materials is increased through slow stirring, the solvent and the raw materials make full contact, and therefore the solubility is improved, and the dissolution process of the solvent and solute is accelerated through full mixing; and meanwhile, the consistency of the product quality can be ensured, and the efficiency of the production process can be improved.

The utility model discloses a dynamic countercurrent extraction unit system for coenzyme Q10 production and extraction, and belongs to the technical field of biochemical engineering. The top of the front end of the extractor is provided with a feeding hole for adding Q10 mud, and the rear end of the extractor is provided with a slag drawing hole; the head part and the tail part are provided with communicating ports for introducing cleaning liquid; the head communication port of the current stage of extractor is communicated with the tail communication port of the previous stage of extractor, and the head communication port of the current stage of extractor is connected with the tail communication port of the next stage of extractor; the residue drawing machine corresponding to the last-stage extractor conveys the residues into the residue extruding machine; a liquid outlet of the residue squeezing machine is connected with a tail communicating opening of the last-stage extractor through a liquid return pipeline; a head communicating port of the first-stage extractor is connected with an extract liquid tank through a liquid conveying pipeline; according to the countercurrent extraction device, raw materials are in full contact with an extraction solvent in a countercurrent extraction manner, so that the extraction efficiency is improved.

The invention belongs to the technical field of traditional Chinese medicine extraction and medicine, and particularly relates to an anthraquinone compound and an extraction method and application thereof. The anthraquinone compound is extracted from oldenlandia diffusa. The invention provides an anthraquinone compound extracted from oldenlandia diffusa, and the anthraquinone compound has a novel structure and pharmacological activity, and provides a material basis for research on the medical effect of the oldenlandia diffusa. The data result of the embodiment of the invention shows that the anti-leukemia effect of the anthraquinone compound provided by the invention provides a powerful basis for exploring potential anti-leukemia new drugs. In addition, the invention also provides a method for preparing the compound from oldenlandia diffusa, and the whole preparation process is simple to operate, easy to control and suitable for industrial production.

The invention discloses a preparation method of a polyisopentenyl acyl phloroglucinol compound, the compound is subjected to a tumor multidrug resistance reversing activity test, under the same concentration, hyperiumono C shows a reversing effect superior to that of a positive drug verapamil, the reversing multiple reaches 56, and the compound has a good anti-tumor effect. A lead compound with development potential is provided for overcoming breast cancer chemotherapy drug resistance.

The invention relates to the technical field of organic synthesis, and relates to ultra-high-purity 2-methyl-1, 4-naphthoquinone and a purification method thereof. The method comprises the following steps: a) a distillation or rectification step: adding a first composite additive into a to-be-purified material containing 2-methyl-1, 4-naphthoquinone, and then carrying out distillation or rectification; b) a melt crystallization step: carrying out melt crystallization on the product obtained in the step a); in the melt crystallization process, a second composite additive is added. The method is high in adaptability, universal and flexible, the product purity grading function can be directly achieved for 2-methyl-1, 4-naphthoquinone of different synthesis routes, the separation process of ultra-high-purity finished products can be obtained, and meanwhile the industry bottleneck problem that heavy metal of the products exceeds the standard is solved.