101 results about "Ammonium formate" patented technology

The invention discloses an enzyme catalytic synthesis method of a luliconazole chiral intermediate, which comprises the following steps: adding a recombinant escherichia coli wet cell for expressing alcohol dehydrogenase, a recombinant escherichia coli wet cell for expressing formate dehydrogenase, a buffer solution, a substrate, a cosolvent, ammonium formate and a coenzyme into a reaction container, reacting at 25-35 DEG C for 2-24 hours, extracting, separating, and carrying out rotary evaporation, thereby obtaining the luliconazole chiral intermediate. The luliconazole chiral intermediate is obtained; the substrate is 2, 2 ', 4'-trichloroacetophenone; the alcohol dehydrogenase is a mutant of AKR3. The method is mild in reaction condition, environmentally friendly, high in regioselectivity and stereoselectivity, high in conversion rate, high in chiral purity, small in enzyme dosage, low in preparation cost and suitable for industrial production.

The invention discloses a CAD detection method for phosphoric acid and phosphorous acid in an alendronate sodium oral solution, and belongs to the technical field of pharmaceutical analysis. The method comprises the following steps: preparing a reference stock solution and a test solution; then setting high performance liquid chromatography detection conditions; a Shodex VN-504D chromatographic column is adopted, a CAD detector is adopted as a detector, a mixed solution of a mobile phase A and a mobile phase B is adopted as a mobile phase, the mobile phase A is ammonium formate, the mobile phase B is an acetonitrile solution, and gradient elution is performed by adopting the mobile phase; and respectively measuring the reference stock solution and the test solution, injecting into a liquid chromatograph, and recording a chromatogram. A CAD detector is adopted, the detection sensitivity is obviously improved, the quantitative concentration can reach 0.24 mu g / mL, and the detection concentration can reach 0.10 mu g / mL. The method is high in specificity, high in sensitivity, good in durability, rapid, simple, effective and reliable.

The invention discloses a high-performance thermosetting resin plugging material, a preparation method and a water-based drilling fluid, and relates to the technical field of oilfield chemistry, and the preparation method of the plugging material comprises the following steps: stirring an aromatic compound containing two double bonds with sodium tungstate, a transfer catalyst and a hydrogen peroxide solution at room temperature for reaction, and purifying to obtain an epoxy compound; the preparation method comprises the following steps: heating an aromatic compound containing an aldehyde group, ammonium formate and a palladium-carbon catalyst with nitrogen to react to obtain an amine compound, transferring the epoxy compound and the amine compound into a size-adjustable mold, carrying out heating curing treatment, carrying out low-temperature ball milling on a crude product to obtain plugging material particles, and preparing the water-based drilling fluid by using the plugging material particles. The specific aromatic rigid framework monomer is selected, and the molar ratio of epoxy to the curing agent is accurately controlled, so that the mechanical strength and thermal stability of the material are remarkably optimized, and the plugging material has a good treatment effect on cracks and pores in complex stratums.

The invention provides a method for detecting related substances of sucrose octasulfate salt auxiliary materials, and particularly relates to the field of medicines. An SCX cation exchange chromatography filler and a C18 filler are mixed according to the ratio of (0.8-1.2): (3-5) to serve as a filling agent; the specification of a chromatographic column is CAPCELLPAK CR C18 + SCX 5 [mu] m, 250 * 4.6 mml.D.; 18-22 mM / L ammonium formate and 0.08-0.12% formic acid are used as a mobile phase A, and acetonitrile is used as a mobile phase B; a detector is CAD, the spray temperature is High, the collection frequency half-peak width is 0.1-0.2 min, the column temperature is 28-32 DEG C, the flow rate is 0.8-1.2 ml / min, and the sample injection volume is 4-6 [mu] l; wherein acetonitrile and water in a ratio of (3-5): (5-7) are used as diluents, and gradient elution is carried out; the method provided by the invention can effectively separate and accurately analyze each impurity, has strong specificity and good separation degree, and can effectively control the product quality.

The invention relates to the technical field of breast milk oligosaccharide detection, and provides a breast milk oligosaccharide high-coverage analysis method based on liquid chromatography-high resolution mass spectrometry, which comprises the following steps: detecting breast milk oligosaccharide in a to-be-detected sample solution by using a UPLC-HRMS method, comparing fragment ions, retention time, primary parent ion accurate mass number and isotope distribution, and determining the breast milk oligosaccharide coverage degree of the to-be-detected sample solution according to the fragment ions, the retention time, the primary parent ion accurate mass number and the isotope distribution. The structure identification of the breast milk oligosaccharide in the breast milk sample is realized; chromatographic conditions in the UPLC-HRMS method are as follows: a 50mmol / L ammonium formate aqueous solution is taken as a mobile phase A, pure acetonitrile is taken as a mobile phase B, the elution mode is gradient elution, and the content of the mobile phase B is calculated by volume percent. According to the technical scheme, the problems of low coverage and low sensitivity during breast milk oligosaccharide detection and analysis in related technologies are solved.

The utility model discloses a urea hydrolysis product gas treatment system, which belongs to the technical field of flue gas denitration reducing agent preparation, and comprises a first water vapor adsorption device, a second water vapor adsorption device and a third water vapor adsorption device, two ends of the first product gas branch pipeline are respectively connected with the first water vapor adsorption device and the product gas pipeline; two ends of the first dry product gas output pipeline are respectively connected with the first water vapor adsorption device and the metering distribution module; a second molecular sieve assembly is arranged in the second water vapor adsorption device; two ends of the second product gas branch pipeline are respectively connected with the second water vapor adsorption device and the product gas pipeline; two ends of the second dry product gas output pipeline are respectively connected with the second water vapor adsorption device and the first dry product gas output pipeline; according to the system provided by the invention, the temperature of the product gas can be always kept above the dew point temperature in the conveying process, so that the situation that the pipeline is blocked by ammonium carbamate crystals generated in the pipeline due to water vapor recondensation is avoided.

The invention belongs to an amide intermediate treatment device and method for hydrazine hydrate production. Comprising a concentration tank, the concentration tank is provided with a water-phase reaction liquid inlet pipeline and a catalyst inlet, the catalyst inlet is connected with a quartz sand catalyst preparation unit, an outlet of the concentration tank is connected with a concentrated material inlet of an intermediate recovery kettle, and the intermediate recovery kettle is further connected with an ammonia feeding pipeline. An ammoniation liquid outlet of the intermediate recovery kettle is connected with a separation and recovery unit, and a liquid phase outlet of the separation and recovery unit is connected with a hydrazine compound synthesis section; a steam discharge pipeline is arranged at the top of the concentration tank; the method has the advantages that moisture in the water-phase reaction liquid can be removed, ammonium formate is converted into formamide and recycled, meanwhile, metal ions are prevented from being contained in ammoniation liquid, and further, the treatment cost is reduced and continuous treatment is achieved on the basis of energy conservation and consumption reduction.

The invention belongs to the technical field of biosynthesis, and particularly relates to a method for preparing chiral alcohol through asymmetric reduction of large steric hindrance rigid ketone based on aldehyde ketoreductase and a mutant thereof. Comprising the following steps: adding a recombinant Escherichia coli wet cell for expressing aldehyde ketoreductase, a recombinant Escherichia coli wet cell for expressing formate dehydrogenase, a buffer solution, a substrate, a cosolvent, ammonium formate and coenzyme into a reaction container, reacting at a certain temperature, and after the reaction is completed, extracting, separating and carrying out rotary evaporation to obtain a product alcohol. The biological catalysis method is mild in reaction condition, environmentally friendly and high in regioselectivity and stereoselectivity, chiral resolution and heavy metal residues in products are avoided, and the defects of a chemical method are exactly overcome.

The invention belongs to the technical field of medicine detection, and particularly relates to an LCMS (Liquid Chromatography Mass Spectrometry) detection method for histamine in prednisolone. Respectively injecting the reference solution, the test solution and the blank solution into an LCMS (Liquid Chromatography Mass Spectrometer), recording a spectrogram, and calculating the content of histamine in prednisolone by adopting an external standard method; wherein the detection condition of the LCMS comprises a mobile phase, and the mobile phase adopts acetonitrile as a mobile phase A and a 10mM ammonium formate aqueous solution containing 0.1 vol% of formic acid as a mobile phase B. The method is good in reproducibility and stability and high in precision.

The invention relates to a method for performing MALDI mass spectrum imaging detection and HE staining on a medical tissue slice. The method comprises the following steps: S1, performing matrix spraying on the medical tissue slice, and performing MALDI mass spectrum imaging detection; s2, cleaning the medical tissue slice subjected to MALDI mass spectrum imaging detection by using a cleaning agent; s3, carrying out HE staining on the cleaned medical tissue slice; the cleaning agent in the step S2 comprises ethanol gel and a mixed solvent composed of acetone and tetrahydrofurfuryl alcohol diethyl ether; the volume ratio of acetone to tetrahydrofurfuryl alcohol ether in the mixed solvent is (1.85-4): 1; the ethanol gel is prepared from the following raw materials: ethanol, acetonitrile, PEG-400 and an ammonium formate aqueous solution. The method for performing MALDI mass spectrum imaging detection and HE staining on the medical tissue slice can ensure that the tissue is complete and free of matrix interference during HE staining.

This invention discloses a method for determining the content of multiple indicators of Jinrong granules absorbed into the bloodstream. The ion chromatogram is obtained using UPLC-Q-TOF-MS / MS analysis. The chromatographic conditions include: flow rate: 0.3–0.5 mL / min; column temperature: 20–30℃; mobile phase: phase A is acetonitrile, and phase B is a 0.04–0.08 mmol / L ammonium formate aqueous solution. The mobile phase comprises acetonitrile and a 0.04–0.08 mmol / L ammonium formate aqueous solution. This invention can simultaneously determine the content of multiple major components of Jinrong granules after absorption into the bloodstream, enabling more comprehensive control of the quality of Jinrong granules. It provides a convenient and efficient method for determining the content of components both in vivo and in vitro, laying a scientific foundation for improving the overall quality standards of Jinrong granules.

The invention belongs to the technical field of vitamin content detection, and particularly relates to a method for measuring the content of various water-soluble vitamins B. The water-soluble vitamins B comprise vitamin B1, vitamin B2, vitamin B3, vitamin B6, vitamin B7, vitamin B12 and nicotinamide. A high performance liquid chromatograph and an electrospray detector are used as detection instruments, and chromatographic conditions are as follows: a mobile phase A is ammonium formate or ammonium acetate, a mobile phase B is methanol, and gradient elution is performed; the gradient elution procedure is as follows: a solvent of a test sample is a mixed solution of acetonitrile, water and glacial acetic acid, and the volume ratio of the acetonitrile to the water to the glacial acetic acid is 5: 95: 0.5; the atomization temperature of the electrospray detector is 35 DEG C; the method is better in separation degree and higher in specificity and sensitivity.

The application provides an alpha-carboxyl-beta-diimine nickel complex and a preparation method and application thereof and a preparation method of ethylene-methyl acrylate copolymer. The alpha-carboxyl-beta-diimine nickel complex has a structure shown in general formula (I): in the general formula (I), Ar is selected from 2,6-dialkylphenyl; X is chlorine or bromine; and L is acetonitrile or benzonitrile. The preparation method of the alpha-carboxyl-beta-diimine nickel complex is that acetylacetone is reacted with 2,6-dialkylaniline, then reacted with ammonium formate under the action of alkyl lithium, and then reacted with a halogenated nickel salt in an acetonitrile or benzonitrile solvent to obtain the alpha-carboxyl-beta-diimine nickel complex. The application further provides a preparation method of ethylene-methyl acrylate copolymer, which uses the alpha-carboxyl-beta-diimine nickel complex as a main catalyst. The application improves the copolymer molecular weight and the methyl acrylate insertion rate, and makes the prepared EMA similar to the branched structure of a commercial product prepared by a free radical process.

The invention belongs to the technical field of metallurgical binders, and particularly relates to a Bayer process red mud-based composite pellet binder, a preparation method thereof and iron ore pellets. The invention relates to a water-based adsorbent, which is prepared from the following components in percentage by mass: 60 to 80 percent of Bayer process red mud subjected to microwave-ultrasonic wave synergistic activation treatment, 10 to 25 percent of superfine slag powder, 2 to 8 percent of nano SiO2 and 1 to 5 percent of mixture of sodium lignin sulfonate and ammonium formate, the parameters of the microwave-ultrasonic wave synergistic activating treatment are as follows: the microwave power is 600 to 1000W, the ultrasonic wave frequency is 30 to 50kHz, and the treatment time is 20 to 40min. Compared with an existing technology of only microwave single activation or red mud-bentonite compounding, in the embodiment of the invention, microwave-ultrasonic wave synergistic activation and a mixture of superfine slag powder-nano SiO2-sodium lignin sulfonate and ammonium formate are introduced into the red mud-based binder in a ternary synergistic manner for the first time; and the problems of activity, strength and grade loss are synchronously solved on the premise of not introducing bentonite.

The invention relates to the field of quality detection of traditional Chinese medicine preparations, and particularly provides a sophora flower bud and sophora flower bud preparation characteristic chromatogram construction method and a quality detection method. In the characteristic chromatogram construction method, a test solution is purified by adopting a macroporous adsorption resin method during preparation; chromatographic conditions are as follows: octadecylsilane chemically bonded silica is used as a filler, acetonitrile is used as a mobile phase A, an ammonium formate aqueous solution with the concentration of 0.01-0.02 mol / L is used as a mobile phase B, the pH value of the ammonium formate aqueous solution is 4-5, 16 common characteristic peaks are obtained under a specific elution procedure, good separation of the common characteristic peaks is realized, the obtained characteristic chromatogram has a stable base line, and the detection sensitivity is high. The method has the advantages of large number of characteristic peaks, symmetrical peak shapes, good separation effect and strong specificity of characteristic components, provides a basis for quality detection and control of sophora flower buds and preparations thereof, realizes characterization of the whole components of sophora flower buds and preparations thereof, and has stable reproducibility.

The invention belongs to the technical field of carbon fiber material modification, and relates to an activated carbon fiber modification method, a modified activated carbon fiber and application thereof. The preparation method comprises the following specific steps: (1) mixing activated carbon fibers, a maleic acid solution and an ammonium formate solution according to a mass fraction ratio of (0.1-1): (2-10): (2-10), and reacting at 50-70 DEG C; and (2) after the reaction is finished, taking out a reaction product, cleaning and drying to obtain the modified activated carbon fiber. Results show that under the compound modification condition of 6% of ammonium formate and 4% of maleic acid, the SO2 adsorption capacity of the activated carbon fiber material after compound modification reaches 18.294 mg / g and is improved by 141.36% compared with that of an unmodified original sheet.

The invention relates to the technical field of inspection and detection, in particular to a method for detecting tadalafil analogues. According to the method disclosed by the invention, the tadalafil impurity O, the EP impurity 1 and the impurity 82 in the sample are rapidly screened and quantitatively detected by adopting UPLC-MS / MS (Ultra Performance Liquid Chromatography-Mass Spectrometry). Extracting and purifying the sample by adopting a four-salt dispersion solid-phase extraction method; a C18 chromatographic column is adopted, 5-20 mM ammonium formate-acetonitrile is used as a mobile phase for gradient elution, and an MRM mode is combined for detection. A verification result of the method shows that the linear relation of target impurities is good, the quantitation limit of oral liquid is 0.02 mg / kg, the detection limit is as low as 0.007 mg / kg, the quantitation limit of a semi-solid preparation and a solid preparation is 0.05 mg / kg, the detection limit is as low as 0.02 mg / kg, and the average recovery rate reaches 80%-116% (RSDlt; 5.3%).

The invention discloses 2-((4-aminopyridine-2-yl) amino)-4-methylphenol as well as a synthesis method and application thereof, 2-bromo-4-methylphenol and 4-nitropyridine-2-amine are taken as raw materials, and an intermediate 4-methyl-2-((4-nitropyridine-2-yl) amino) phenol is obtained through condensation reaction; and reducing the intermediate under the action of ammonium formate and a catalyst to obtain the 2-((4-aminopyridine-2-yl) amino)-4-methylphenol. The method is simple and convenient to operate, mild in operation condition and high in reaction rate, the obtained product is high in purity and yield, the dispersity and antistatic performance of the insoluble sulfur can be improved, and the method is suitable for industrial mass production.

The invention belongs to the technical field of organic synthesis, and particularly relates to a preparation method of a pyrrolopyrimidine-4-amine derivative, which selects methanol, ammonium formate and formic acid as a reaction system to carry out directional reaction, avoids the use of high-pressure hydrogen and a high-pressure kettle, avoids the safety risk caused by high-pressure operation, and improves the yield of the pyrrolopyrimidine-4-amine derivative. And the alcoholic solution solves the problems of low solubility and obvious amplification effect of a starting material when water is used as a solvent in the prior art, and realizes homogeneous reaction. By adopting the fixed bed reaction unit, the problem of pipeline blockage caused by sublimation of ammonium formate is solved, the potential safety hazard in large-scale production is eliminated, the fixed bed reaction unit is used for continuous catalytic reaction to replace the traditional staged reaction, the production period is remarkably shortened, the production efficiency is improved, and the method is suitable for large-scale industrial production.

The invention provides a method for separating and detecting components in butanedisulfonic acid ademetionine enteric-coated tablets, and belongs to the technical field of medicine quality analysis. According to the method, ammonium formate solution-water-acetonitrile and ammonium formate solution-acetonitrile-methyl tert-butyl ether are used as a mobile phase system, and the pH value of the ammonium formate solution is controlled to be 2.2-3.1, so that adenosine and adenine can be effectively separated; according to the method, the S-adenosyl-L-methionine glycine isomer 2, adenosine, adenine and S-adenosyl-L-homocysteine can be separated, the time consumption is short, the separation efficiency is high, the operation is simple, the separation cost is low, and the quality control of butanedisulfonic acid adenosyl methionine or related preparations can be improved. According to the method, the detection of the ademetionine and the related impurities is not influenced by auxiliary materials, the method is efficient and convenient, good in reproducibility, high in specificity, high in accuracy and high in sensitivity, and the quality control of the ademetionine sample can be realized.

Provided are: a separation solution for an aluminum foil laminate, which can reduce elution of an aluminum foil into the separation solution and reduce the amount of impurities when a recovered aluminum foil is melted and cast, and which has sufficient ability to separate an aluminum foil laminate into a resin and an aluminum foil; and a method for separation and recovery of an aluminum foil laminate using same. The present invention is capable of providing a separation solution for an aluminum foil laminate, which contains an ammonium salt comprising at least one of ammonium formate and ammonium acetate, one or more acids selected from the group consisting of nitric acid, sulfuric acid, phosphoric acid, formic acid and acetic acid, and water, the separation solution being characterized in that a content ratio obtained by dividing the content (mass%) of the ammonium salt in the separation solution by the content of the acid (mass%) in the separation solution is 0.1-40.0.

The invention provides a method for simultaneously determining the content of glycine methyl ester hydrochloride and the content of 2, 5-piperazine diketone, and belongs to the field of chemical detection and analysis. According to the method, acetonitrile and an ammonium formate aqueous solution with the volume ratio of 3: 97 are used as a mobile phase, the concentration of ammonium formate is 1.26 g / L, formic acid is used for adjusting the pH value of the solution to 3.95, meanwhile, an electric fog detector is selected, and a simertorin Accuore TM aQ C18 chromatographic column is used for detection, so that effective separation of glycine methyl ester hydrochloride and 2, 5-piperazine diketone is realized, and the method is suitable for large-scale production of glycine methyl ester hydrochloride and 2, 5-piperazine diketone. The method can be used for rapidly and accurately detecting the content of glycine methyl ester hydrochloride and 2, 5-piperazine diketone, and can be applied to the central control monitoring of the reaction for synthesizing 2, 5-piperazine diketone by glycine methyl ester hydrochloride.

This invention discloses a process and coating structure for rare earth modified trivalent chromium pearl chromium plating on zinc alloys. The process includes sequentially preparing a cyanide-free copper plating layer, a cyanide-free copper-zinc alloy plating layer, a high-corrosion-resistant nickel-phosphorus alloy plating layer, a bright nickel-cobalt alloy plating layer, a pearl nickel plating layer, a rare earth modified trivalent chromium pearl chromium plating layer, and an anti-discoloration protective film on a zinc alloy substrate. The rare earth modified trivalent chromium pearl chromium plating process is as follows: chromium chloride hexahydrate 90-130 g / L, potassium chloride 90-160 g / L, ammonium chloride 90-160 g / L, ammonium bromide 18-28 g / L, ammonium formate 40-60 g / L, boric acid 45-65 g / L, rare earth additives 8-12 mL / L, leveling agent 2-4 mL / L, accelerator 1-3 mL / L, plating bath pH 2.5-3.2, plating bath temperature 25-35℃, and cathode current density 8-16 A / dm². The rare earth additives have a synergistic effect on improving the performance of trivalent chromium plating solution. No rust was observed on the surface of the plated parts after undergoing a neutral salt spray test for 132 hours according to GB / T 10125–2021 standard.

The present application relates to a kind of HPLC-MS / MS detection method of detecting in human plasma, desloratadine and 3-hydroxydesloratadine in human plasma, it includes the following steps: (1) human plasma sample pretreatment;(2) liquid chromatography-mass spectrometry detection, using mobile phase A and mobile phase B as mixed mobile phase is carried out gradient elution, wherein: mobile phase A is methanol-acetonitrile mixed solution, in mixed solution methanol and acetonitrile volume ratio is 4-6:6-4;Mobile phase B is 2-20mM ammonium formate aqueous solution;(3) the determination of the concentration of human plasma in lopatadine, desloratadine and 3-hydroxydesloratadine.The present application uses lopatadine-d4, desloratadine-d5, 3-hydroxydesloratadine-d4 as deuterium internal standard, using Agilent, ZORBAX Eclipse XDB-Phenyl is carried out gradient elution, deuterium internal standard and the measured substance has the same retention time, chemical property and matrix effect, the reproducibility, accuracy of determining the concentration of lopatadine, desloratadine and 3-hydroxydesloratadine in plasma are good.The method of the present application can be used to evaluate the bioequivalence of lopatadine.

This invention discloses a catalyst and method for the continuous synthesis of formamide from ammonium carbonate or ammonium bicarbonate, belonging to the field of chemical technology. The catalyst is a boron-nitrogen co-doped activated carbon supported palladium catalyst prepared by using a palladium precursor, boric acid, and nitrogen-doped activated carbon. The method uses ammonium carbonate solution or ammonium bicarbonate solution as raw material, and in a continuous flow reactor, the above-mentioned catalyst catalyzes the hydrogenation of ammonium carbonate or ammonium bicarbonate to synthesize formate. The formate is then dehydrated to obtain formamide. The catalyst of this invention has advantages such as high activity and high stability, and can efficiently and stably produce ammonium formate in a continuous flow reactor, which can then be further dehydrated to obtain formamide, thus providing a green, low-carbon, and safe method for the synthesis of formamide.

The invention discloses an enzymatic synthesis method of a melogabalin intermediate and related alcohol dehydrogenase, racemic 3-ethyl bicyclo [3.2. 0] hept-3-ene-6-ketone is used as a substrate, a genetically engineered bacterium for producing alcohol dehydrogenase is used as an enzyme catalyst, a genetically engineered bacterium for producing formate dehydrogenase, ammonium formate and coenzyme are matched, an enzymatic reaction is carried out under a stirring condition, and the melogabalin intermediate is obtained. And carrying out purification and separation on a reaction product to obtain the melogabalin intermediate (1R, 5S)-3-ethyl bicyclo [3.2. 0] hept-3-ene-6-ketone. The method has the advantages of simple reaction, few steps, mild reaction, less pollution and the like, and has great industrial application potential and commercial value.

The invention discloses a method for detecting related substances of Velciguat, which comprises the following steps: detecting by adopting a high performance liquid chromatography under the chromatographic conditions that a stationary phase is an octyl silane bonded silica gel chromatographic column, a mobile phase A is an ammonium formate aqueous solution, a mobile phase B is acetonitrile, and gradient elution is carried out; the gradient elution procedure is as follows: within 0-30 minutes, the volume fraction of the mobile phase A is gradually changed from 78-82% to 28-32%; within 30-45 min, the volume fraction of the mobile phase A is gradually changed from 28-32% to 8-12%; within 45-50 min, the volume fraction of the mobile phase A is kept at 8-12%; within 50-50.1 min, the volume fraction of the mobile phase A is gradually changed from 8-12% to 78-82%; and within 50.1-60 minutes, the volume fraction of the mobile phase A is kept at 78-82%. According to the method provided by the invention, effective separation between the main peak of the Velciguat and each impurity can be realized.

The invention relates to the technical field of food science and analytical chemistry, in particular to a method for analyzing carbohydrates in sialic acid lactose and application of the method. The analysis method disclosed by the invention comprises the following steps: separating carbohydrates through ultra-high performance liquid chromatography, wherein in the ultra-high performance liquid chromatography, a mobile phase A comprises acetonitrile; the mobile phase B comprises 10-30 mmol / L of an ammonium formate aqueous solution; the elution procedure is a specific gradient elution procedure. According to the analysis method, lactose, N-acetylneuraminic acid, 3 '-sialic acid lactose, 6'-sialic acid lactose, 3 '-sialic acid lactulose, 6'-sialic acid lactulose and other carbohydrates in sialic acid lactose can be completely separated, and the problem that the substances cannot be effectively separated in the prior art is solved.

The present invention belongs to the technical field of organic complex synthesis, and specifically relates to a metal complex and its preparation method and application. The general formula of the metal complex is L-M, wherein L is a ligand, M is a metal salt, and the ligand is diphenylmethylbenzylamine or diphenylmethylquinuclidine-3-amine. The diphenylmethylbenzylamine is prepared by reacting imine and sodium cyanoborohydride; the diphenylmethylquinuclidine-3-amine is prepared by reacting diphenylmethylbenzylamine and ammonium formate. The preparation method of the metal complex is to dropwise add a metal salt solution to a methanol solution containing the ligand, carry out a coordination reaction, and filter to obtain a target product. The preparation method has the advantages of simple process, mild conditions, low cost, and easy industrialization. The metal complex provided by the present invention can be used to prepare an antibacterial agent, which has the advantages of high efficiency, low toxicity, and environmental protection.

The invention belongs to the technical field of chemical component detection, and particularly relates to a method for detecting residues of NDMA, NMBA, NDEA, NDIPA and NDBA in tea diphenhydramine, which comprises the following steps: (1) preparing a tea diphenhydramine test solution; and (2) determining the tea diphenhydramine test solution by using a liquid chromatography-mass spectrometry method, and liquid chromatography conditions are as follows: a chromatographic column takes phenyl-hexyl bonded silica gel as a filler, an aqueous solution containing trifluoroacetic acid and ammonium formate as a mobile phase A, and a methanol-acetonitrile mixed solution containing trifluoroacetic acid as a mobile phase B, gradient elution is performed, and the content of the tea diphenhydramine is determined. The residual contents of NDMA, NMBA, NDEA, NDIPA and NDBA in a tea diphenhydramine test sample are calculated by adopting an external standard method. The method provided by the invention plays an important role in formulating and improving quality standards of tea diphenhydramine bulk drugs and preparations.