33 results about "Methylomonas methanolica" patented technology

The invention discloses a method for simultaneous determination of six active components consisting of chrysophanol, emodin, liquiritin, forsythin, baicalin and berberine hydrochloride in a Niuhuang Ninggong tablet through HPLC. Chromatographic conditions employed in the invention are as follows: a chromatographic column is TC-C18 (4.6 mm * 250 mm, 5 [mu]m); detection wavelength is 280 nm; a mobile phase is methanol-0.05% phosphoric acid; gradient elution comprises three parts, i.e., elution with methanol with a concentration varying in a range of 10 to 80% in the time period from 0 min to 35 min, then elution with methanol with a concentration of 80% in the time period from 35 to 50 min, and finally elution with methanol with a concentration varying in a range of 80 to 10% in the time period from 50 to 60 min; flow velocity is 1.0 mL / min; column temperature is 25 DEG C; and sample size is 10 [mu]L. Under the above-mentioned chromatographic conditions, chromatographic peaks are perfectly separated, and concentrations and peak areas of chrysophanol, emodin, liquiritin, forsythin, baicalin and berberine hydrochloride show good linear relation. The method is simple, rapid and accurate, has good repeatability and can provide quality bases for comprehensive evaluation and control of the Niuhuang Ninggong tablet.

The invention discloses a method for measuring the relative correction factor of methanol in methoxymethanol without a standard sample. Methoxymethanol is a product of equimolar condensation of methanol and formaldehyde. The formaldehyde in methoxymethanol is used to react with the reagent to release methanol in methoxymethanol. The ratio of the reduction is the correction factor for methanol in methoxymethanol relative to free methanol. During the analysis process, adding a reference reagent is convenient for area normalization determination. After the response standard of the reference reagent is finally unified, the content of methanol and methoxymethanol after calibration under different reaction reagent additions is plotted, and linear fitting is performed. Then the relative correction factor for methanol in methoxymethanol was obtained. Using this method, the methanol content in methoxymethanol can be accurately determined without a standard sample. This method has the advantages of simple operation and accurate results.

The invention discloses a method for recycling cyanoacetamide in mother liquor. The method comprises the following steps of: adding primary mother liquor into a reaction kettle, and stirring; slowly rising the temperature of the reaction kettle, evaporating methanol, starting to discharge methanol when the kettle temperature achieves about 65 DEG C, cooling the methanol by using a condenser and collecting the methanol; and finishing the evaporation when the temperature inside the reaction kettle achieves 90-92 DEG C; decreasing the temperature of the reaction kettle to about 50+ / -10 DEG C, subsequently adding water, toluene or heptane and the like into the reaction kettle, decreasing the temperature to 10-20 DEG C, filtering, centrifuging and drying so as to obtain a cyanoacetamide product. The method has the advantages of high recycling rate, emission reduction and pollution reduction.

The invention relates to a preparation method of irinotecan hydrochloride. The preparation method comprises the following steps: 1, reacting 4-piperidylpiperidine with dimethyl carbonate in a dipolar aprotic solvent to generate 4-piperidylpiperidine dimethyl carbonate; 2, reacting 4-piperidylpiperidine dimethyl carbonate with 7-ethyl-10-hydroxycamptothecin in a nonpolar solvent to generate irinotecan monomers; and 3, adding water to dissolve the irinotecan monomers, adding a hydrochloric acid solution to adjust the pH value of the obtained solution to 3-4, adding acetone, crystallizing, filtering, and carrying out vacuum drying to obtain finished irinotecan hydrochloride. The preparation method which introduces carbonyl groups to the active substance dimethyl carbonate during preparation of irinotecan hydrochloride has the characteristics of safe use, convenience, small pollution, easy transportation and the like in production; the preparation method which allows use of phosgene substances to be completely avoided and pollution to the environment to be correspondingly migrated is green; and an acid binding agent is not needed by the method, and methanol which is the only byproduct is a volatile substance with a low boiling point, so post-processing is simple.

The invention relates to sesquiterpene dimmers in vernonia anthelmintica, and a preparation method and application. The dimers comprises vernodalin dimer I, vernodalin dimer J and vernodalin dimer K. The preparation method comprises crushing vernonia anthelmintica seeds, percolating and degreasing by petroleum ether, so as to obtain total extractives, then performing gradient elution respectively by using petroleum ether / ethyl acetate, chloroform / methanol and methanol / water, and then performing repeated purification by using semi-preparative high performance liquid chromatograph. Three new sesquiterpene dimers, vernodalin dimer I, J and K are proved to be separated from vernonia anthelmintica seed through analysis on spectrum and mass spectrum data. In-vitro anti-tumor activity research shows that the provided compounds possess relatively obvious cytotoxic activity on human lung cancer cell A-549, human colon cancer cell HCT-15 and human prostate cancer cell PC-3, are applicable to low-toxicity anti-tumor medicines, and are new lead compounds for developing anti-tumor medicines.

A method for producing methane-enriched gas, liquefied petroleum gas and gasoline from synthesis gas. After being heated, the raw material synthesis gas enters a methanol reactor equipped with a methanol synthesis catalyst to react to generate methanol; the outlet material of the methanol reactor enters a methanol reactor equipped with a Catalyst reacts in the methanation reactor to generate methane; the outlet material of the methanation reactor enters the synthetic oil reactor equipped with synthetic oil catalyst to be converted into liquefied petroleum gas and gasoline; the outlet material of the synthetic oil reactor enters the oil-water-gas three-phase separator , the gas phase product obtained by separation is methane-rich gas, and the water phase product is sent to the outside for treatment; the oil phase product enters the rectification tower for rectification separation, and the liquefied petroleum gas product is obtained at the top of the tower, and the gasoline product is obtained at the bottom of the tower. The invention has the advantages of low energy consumption and high efficiency.

The invention discloses a glucosamine donor and application thereof. According to the glucosamine donor, N, N-dimethylformamide is introduced into a C-2 position nitrogen atom for performing N, N-diacetyl protection; an electron-rich activated (armed) protecting group is introduced to at least one position of glucosamine C-3, C-4 and C-6, wherein the N, N-diacetyl has an ortho-group participationeffect, can generate a single beta-selective glycosylation product, and can be removed from acyl groups at other positions by a one-kettle method under mild conditions such as methanol / sodium methoxide and the like so that the synthesis efficiency is improved. The iso-head leaving group of the glucosamine donor can be halogen, glucosinolate, imine ester, pentene alkoxy, hydroxyl and the like, andcan react with different receptors to construct a beta-glucosidic bond so that the reaction efficiency is high.

The invention provides a method for preparing a method for preparing an aprepitant intermediate 2-(2-chloro-1-ethidene)hydrazide methyl formate. The method comprises the following steps: carrying out a condensation reaction between chloroacetonitrile and methyl hydrazinocarboxylate in a methanol / sodium methylate reaction solution by virtue of catalysis of glacial acetic acid, and performing after-treatment purification on the reaction solution by adopting acetone. The operation is simple, the purity of the obtained product is over 99%, and the method is high in yield and suitable for industrial production.

The invention specifically relates to an evaporation system and a production process of dimethylformamide. Using carbon monoxide and dimethylamine as raw materials to prepare dimethylformamide under the catalysis of methanol / sodium methoxide has the advantages of good product quality and low cost, but sodium methoxide dissolves in water and is prone to crystallization, and it will catalyze DMF in the evaporation process A reverse reaction occurs to form dimethylamine. The present invention provides a kind of DMF evaporation system and production process applicable to the above-mentioned production mode, and the described production process comprises the following steps: after the crude DMF of the DMF synthesis tower enters the separator for preliminary concentration, it is divided into two routes and the filter is forced Circulation, one way is to add water to the inlet of the second circulation pump to ensure the normal operation of the evaporation circulation pump by adding water, and the other is to inhibit the reverse reaction of DMF. The first circulating pump in the other path plays the role of filtering and discharging the salt mud in the system. The production process can effectively improve the DMF operation cycle and increase the output.

The invention belongs to the technical field of material synthesis, and specifically relates to a hollow iron oxide material and a preparation method thereof. An iron salt and an organic ligand are used as raw materials, methanol, a mixed solution of methanol and water, N,N-2-methylformamide, or a mixed solution of N,N-2-methylformamide and water is used as a reaction solvent, nitric acid is usedas an oxidant, hydrofluoric acid is used as an etching agent, a reaction is performed for 12-72 h, and petal-like hollow iron oxide is obtained. The preparation method provided by the invention has the advantages of controllable etching conditions, simple process, short flow, uniform control of the product morphology and the like, and provides a promising synthesis idea for exploring synthesis ofhollow etching iron oxide.

The invention relates to the field of organic synthesis, and discloses a method for synthesizing p-hydroxyphenethyl alcohol. Evaporate to dryness to obtain the 4-methoxyphenethyl alcohol crude product; 4) add the crude product to the solvent and stir; 5) dropwise add hydrobromic acid, heat up and reflux, and keep the temperature for the reaction until the reaction is complete; 6) be cooled to 55-65 ° C , slowly add alkaline solution, adjust the pH value to 6-7; 7) cool down to 8-12 ° C, stir for 0.5-1.5h, filter the material to obtain a wet filter cake, add a solvent, heat up to dissolve, separate water, and recrystallize , filtered, and spin-dried to obtain the final product. The purity of the product of the method of the invention can reach more than 99%, the yield can reach more than 90%, and the reaction conditions of the whole synthesis process are simple and mild, the post-processing is simple, and the cost is low.

A method for producing methyl acetate from synthesis gas by one-step method relates to a method for synthesizing the methyl acetate. The synthesis gas or the synthesis gas containing CO2 is used as areaction raw material, and the continuous relay reaction is carried out on a multifunctional catalyst to realize the preparation of methyl acetate by one-step method with high selectivity. In the process, the synthesis gas or the synthesis gas containing CO2 is first converted into methanol, then the methanol is dehydrated to form dimethyl ether, and further the dimethyl ether is carbonylated to obtain the methyl acetate. The one-step route significantly simplifies the reaction steps, improves catalytic efficiency, and significantly reduces costs. The used catalyst is a multifunctional composite catalyst, and the synthesis gas is converted into the methyl acetate in one step with high efficiency by designing and functionally coupling components. The target product has high selectivity, themethyl acetate selectivity is up to 90% or more, and the stability is high. By introducing a dehydration catalyst, the dehydration step and the dimethyl ether carbonylation step are separated to eliminate the interference of water to a reaction system. The preparation process is simple and controllable.

The invention discloses a method for producing antibacterial peptide through non-methanol induction. The invention relates to the technical field of the bioengineering and bio-pharmaceuticals, the bad expression effect of the antibacterial peptide in the pichia pastoris is solved, the most important is the methanol resides in the antibacterial peptide product expressed by use of the methanol induction, the toxicity of the methanol enables the antibacterial peptide product to be not applied in the fields of the food, the fodder and the medicines. The technical scheme provided by the invention is to add the inductor choline chloride into an inoculated culture medium so that the final concentration of the choline chloride in the culture medium is 1%-5%w / v. The method disclosed by the invention has the advantages that the PisL9K22WK expression level is high, the production cost is low, the product is safe and free from poisonous residue; the engineering saccharomycetes and the produced pisL9K22WK product can be applied to the antibacterial medicines or the animal or aquiculture fodder additives.

The invention provides a kind of production method that improves three monomer synthesis dimethyl isophthalate-5-sulfonic acid yield and purity, described production method, comprises N 2 Gas purging, adding sulfonated material, adding part of methanol, temperature rise and pressure reaction, adding remaining methanol and catalyst, step temperature rise reaction. The invention reduces the unit consumption of methanol and improves the economic benefits of the product; equivalent to 413-439Kg of methanol consumed per ton of three monomers; the feed amount of methanol is 20% less than that of the existing process; the unit consumption of methanol per ton of three monomers is lower than that of the existing process more than 30%; the purity of dimethyl isophthalate-5-sulfonic acid exceeds 96%, reaching 96.85-97.05%, and the yield exceeds 97%, reaching 97.18-97.42%; the subsequent production of the three-monomer product The rate exceeds 84%; the reaction time is shortened; the esterification reaction operation cycle is shortened by 2 hours compared with the existing production process.

The invention discloses an HPLC method for simultaneous determination of eight active components in Codonopsis pilosula. , Atractylodes Lactone III and 5-Hydroxymethylfurfural, its assay steps are as follows: (1) preparation of test solution; (2) chromatographic condition: C18 chromatographic column, mobile phase consists of methanol-0.01% phosphoric acid aqueous solution, gradient Elution program: 0‑10min, 10% methanol; 10‑25min, 10%‑65% methanol; 25‑40min, 65%‑80% methanol. Wavelength: 0‑5min, 260nm; 5‑6.5min, 210nm; 6.5‑36.5min, 260nm; 36.5‑38min, 220nm; 38‑40min, 260nm. Flow rate 1 mL / min. Column temperature: 30°C. The injection volume was 10 μL. (3) Establishment of standard curve for the determination of the content of eight active ingredients; (4) Determination of the content of active ingredients in the sample. The method is easy to operate, accurate, fast and efficient, can simultaneously measure the contents of eight active components in Codonopsis pilosula medicinal materials, and has great practical value.

The invention discloses a pure water-resistant chromatographic stationary phase as well as a preparation method thereof. According to the stationary phase, silica gel is taken as a matrix and is bonded with alkyl C1-C30, and the bonding density is 1.0-2.5 micromole / m < 2 >. The preparation method of the stationary phase comprises the following steps of: dispersing silica gel in an organic solvent; adding an inorganic weak base or an organic base as a catalyst; adding silane according to the feeding amount of 0.2-1.0 g per gram of silica gel; performing a reaction at 50-150 DEG C for 3-24 hours; filtering reaction liquid; cleaning a filter cake with a reaction solvent, methanol, 30-70% methanol / water (v / v) and methanol in sequence; and drying an obtained solid at 50-80 DEG C under a vacuum condition for 6-24 hours to obtain the stationary phase product. By optimizing the surface bonding density of the stationary phase, the state of the surface bonding phase of the stationary phase is improved, and the pure water-resistant chromatographic stationary phase is obtained. According to the stationary phase and the preparation method thereof, the reaction conditions are mild, the steps are simple and feasible, and repeated and large-scale preparation is easy.

The invention discloses a method for separating and purifying Epothilone D based on molecular imprinting. The EpoD molecular imprinting polymer is soaked in a small amount of pure methanol, loaded into a separation column, and methanol-acetic acid, methanol, and methanol-deionized water are sequentially used Rinse the column, vacuum compact the column; dissolve the EpoD crude product in 20-80% methanol aqueous solution, and add it to the installed column; after standing for 20-50min, rinse the column to remove the interference, and further reduce the interference of impurities; Use 10-90% methanol PBS solution as the eluent to elute the column, so that EpoD is completely dissolved in the eluent, collect the eluate and spin evaporate to dryness, and redissolve in pure methanol to obtain a purified EpoD methanol solution. Compared with the existing separation and purification methods, the method is simple, convenient and low in cost, and at the same time, it is specific adsorption in the epothilone D adsorption process, which can achieve better separation effect. It provides possibility for further separation and purification of epothilone D.