4849 results about "Acetonitrile" patented technology

The invention discloses hot pepper and a determining method for 96 pesticide residues in a product of the hot pepper. The determining method comprises the following steps: homogenously extracting residual pesticide in a sample with 1% acetic acid-acetonitrile solution, purifying the extracting solution with a Florisil solid phase extraction column, dispersing and purifying the extracting solution with ethylenediamine-N-propyl silane (PSA) and octadecyl silane bonded phase (C18) substrate, detecting 69 pesticide residuals in the purified concentrated liquid of the Florisil column by GC-MS (gaschromatographic mass spectrometry), detecting 27 pesticide residuals in the substrate dispersed purified liquid by liquid chromatography-tandem mass spectrometry (LC-MS / MS), using the black substrate solution dilution standard to construct the updated calibration curves, adopting an internal standard method to quantify when using GC / MS to detect the residuals, and adopting an external standard method to quantify when using LC-MS / MS to detect the residuals. The average recovery rate of the method is 70.7-118.6%; the average relative standard deviation (RSD) is 3.2-11.4%; the detection limit is 0.13-28.2 ug / kg. The determining method has the advantages of simplicity and convenience in operation, high speed, accuracy, high sensitivity and good repeatability.

The invention belongs to the technical field of food detection methods, and particularly relates to a method for determining multiresidue of veterinary drugs in animal-derived foods. The method comprises the following steps of weighing a sample, adding an acetic acid-acetonitrile solution, carrying out vibrating extraction, centrifuging to obtain acetonitrile extracting solution, loading the extracting solution obtained by centrifuging into a centrifuge tube with a mixed filler, carrying out vibrating centrifugation, sucking purified liquid, concentrating by blowing nitrogen, diluting to constant volume and detecting by UPLC / MS / MS (ultra performance liquid chromatography-tandem mass spectrometry). The method disclosed by the invention is firstly applied in detecting animal-derived foods and 107 kinds of veterinary drugs such as sulfonamides, quinolones, beta agonists in animal products are subjected to fast qualitative and quantitative detection, the detection limit is completely capable of meeting the detection requirements and the detection efficiency is greatly promoted.

The invention discloses a method for preparing bisphenol A molecular imprinting polymer, comprising the following procedures: dissolving template molecule bisphenol A and functional monomer according to the mol ratio of 1.5:1 to 2:1 into acetonitrile solution which is no less than 10ml with 10 to 15 crosslinking agent and initiator of catalytic amount to prepare mixed liquor; the mixture liquor is churned up at 55 to 70 DEG C to polymerize for 12 to 24 hours and then white powdery polymer is generated; synthesizing fine white powdery polymer using mixed solution of methanol and acetic acid as extracting solution, removing the template molecules and then extracting acetic acid molecules using pure methanol; after extracting, the polymer is arranged in vacuum drying chamber to dry until reaching balancing weight and then bisphenol A molecular imprinting polymer is obtained. The invention has advantages that the prepared bisphenol A molecular imprinting polymer has special adsorption for bisphenol A molecular in cosmetic samples which can rapidly, delicately and accurately concentrate and purify the cosmetic samples in an efficient way; the rate of recovery is high, the reproducibility is good and the sensitivity is high.

The invention provides a high-sensitivity and high-throughput kit for simultaneous quantitative detection of 30 amino acids and a preparation method thereof. According to the kit, after extraction treatment of amino acids in a complex sample by using organic solvents, precipitating by using methanol, adding stable isotope-labeled amino acid internal labels, performing derivatization treatment by using hydrochloric acid and n-butanol, drying and redissolving, carrying out reversed-phase chromatography gradient separation by adopting C18 bonded phase silica gel as a stationary phase and acetonitrile-water containing heptafluorobutyric acid and formic acid as a mobile phase, and carrying out quantitative detection by adopting a mass spectrometer. The kit of the invention has the advantages that detection sensitivity can reach 10ng / ml, and all methodological indexes can meet the requirements of quantitative detections of amino acids in clinical examinations, industrial productions and scientific researches.

The invention relates to a synthesis method and application of a ratiometric fluorescent molecular probe for simultaneously detecting a fluorine ion and a sulfite radical. The ratiometric fluorescent molecular probe adopts a 2-(2-hydroxyphenyl)benzothiazole derivative as a matrix structure, and detects the fluorine ion and the sulfite radical based on excited-state intramolecular proton transfer (ESIPT) and intramolecular charge transfer (ICT) mechanisms, respectively. The probe has a maximum emission wavelength of 498 nm in an acetonitrile solution with a concentration of 80%, when the fluorine ion is added, the fluorescence spectrum of the probe has a red shift of 136 nm; and when the sulfite radical is added, the fluorescence spectrum of the probe has a blue shift of 127 nm. The differentiated detection of the two ions can be realized by the fact that the fluorescence spectrum of the probe has an obvious red shift or blue shift after the fluorine ion or sulfite radical is added, respectively, showing different fluorescence response signals. The inventive fluorescent probe has the advantages of simple operation, mild reaction conditions, easy purification, high synthesis yield, good selectivity, high sensitivity and stable optical performances. At the same time, the design and synthesis of the fluorescent probe provide an important foundation for development of multi-functional fluorescent probes in the future.

The object of the present invention is a fluoropolymer aqueous dispersion showing only a moderate viscosity increase upon temperature rise and having a low fluorine-containing anionic surfactant concentration as well as a method of producing such fluoropolymer aqueous dispersion. The present invention provides a fluoropolymer aqueous dispersion comprising a particle comprising a fluoropolymer dispersed in an aqueous medium in the presence of a nonionic surfactant, wherein a supernatant for assaying as obtained by subjecting the fluoropolymer aqueous dispersion to 30 minutes of centrifugation at 25° C. and at a gravitational acceleration of 1677 G, when subjected to high-performance liquid chromatography [HPLC] under the conditions of a flow rate of 1.0 ml / minute and a column temperature of 40° C. using an acetonitrile / 0.05 M aqueous solution of phosphoric acid (60 / 40% by volume) mixture as a developing solution, followed by detection at an absorption wavelength at which the nonionic surfactant can be identified, shows a ratio (A1 / A0), which is the ratio between the total area (A0) under the detected line and the area (A1) under the detected line over a retention time period shorter than 16 minutes, of not lower than 0.4 and the supernatant for assaying has a fluorine-containing anionic surfactant content of not higher than 100 ppm.

The invention discloses a triazine weedicide, and metabolite molecular engram polymer microspheres, a preparation method and an application thereof, which relate to molecular engram polymer microspheres and a preparation method and an application thereof and are used for solving the problem that the conventional molecular engram polymer can only specially absorb one kind of substance and realizing the effect of separating and enriching a plurality of triazine pesticide residues in a sample respectively. The molecular engram polymer microspheres are prepared by the following steps of: dissolving double template molecules and methacrylic acid into acetonitrile; oscillating; adding trimethylolpropane trimethylacrylate and azobisisobutyronitrile; performing ultrasonic treatment, charging nitrogen, removing oxygen and sealing; and heating in a constant-temperature water bath, cooling, grinding, sieving, eluting and drying. The molecular engram polymer microspheres are applied to a filling material of a solid phase extraction column. A product obtained in the invention has the advantages of high specificity, large absorption amount, wide application range, simple method and low cost. High specific separating and enriching characteristics on the triazine weedicide are achieved, the recovery rate is 65-110 percent, and the requirement of multiple residues can be met.

An apparatus for separating propane from propene by extracting-rectifying in a divided wall column (DWC) in which the water contained acetonitrile is used as the extractant is disclosed. Said DWC has a vertical bulkhead to divide it into three regions: the region A for extracting rectifying of propene and propane, the region B for separating propane from propene, and the region C as common desorption region. Its separation method is also disclosed.

The invention discloses an analysis method for simultaneously measuring residues of 12 sulfonamide medicaments, 19 quinolone medicaments and 8 benzimidazole medicaments and metabolites thereof in chicken liver by quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction and purification-ultrahigh performance liquid chromatography-tandem mass spectrometry (QuEChERS-UPLC-MS / MS). The method comprises the following steps of: extracting a sample by using 1 percent acetic acid-acetonitrile solution, purifying the sample by using NH2 adsorbent, and degreasing the sample by using n-hexane;and then performing separation by using a Kromasil Eternity C18 chromatographic column (100mm*2.1mm, 2.5mum), performing gradient elution by using 0.1 percent formic acid and methanol as mobile phases, performing ionization in an electron spray positive ion (ESI<+>) mode, performing detection in a multi-reaction monitoring (MRM) mode, and performing quantification by an internal standard method. The 39 medicaments have good linearity (r is more than 0.98) in a blank adding concentration range of 5 to 100mug / kg, the average recovery rate of the medicaments in the adding level range of 10 to 50mug / kg, the relative standard deviation (RSD) is 1.5 to 23.4 percent, the limit of detection (LOD) of the 39 medicaments is 5mug / kg, and the low limit of quantification (LOQ) is 10mug / kg. The method is simple, convenient, quick, sensitive, accurate and rugged, and is suitable for confirmation and quantitative determination of the residues of the residues of the sulfonamide, quinolone and benzimidazole medicaments in the chicken liver.

The invention relates to a method for preparing 2-bromine-4, 5-dimethoxy benzene propane nitrile, which consists of steps: 3-4-dimethoxy benzaldehyde and bromine are dissolved in acetic acid to be reacted; when solid is precipitated, 2-bromine-4, 5-dimethoxy benzaldehyde crystal is obtained through suction filtration; the crystal and acetonitrile are dissolved in organic solvent; after a catalytic reaction, yellow solid is precipitated, cooled, extracted and dried to get 2-bromine-4, 5-dimethoxy cinnamonitrile solid which is then dissolved in methanol with reducing agent and is reduced to obtain 2-bromine-4, 5-dimethoxy benzene propane nitrile after a reflux reaction; or the obtained 2-bromine-4, 5-dimethoxy cinnamonitrile is reduced with hydrogen under the catalysis of palladium-charcoal to get 2-bromine-4, 5-dimethoxy benzene propane nitrile. The 2-bromine-4, 5-dimethoxy benzene propane nitrile prepared by the invention has high yield coefficient; original raw materials of the preparation method are easy to get; the price is low; the reaction operation is simple; the reaction route is short; and the method is easy for industrialization production.

The invention discloses a fast detection method for the surface enhanced Raman scattering of trace pesticide residues in oranges, and belongs to the technical field of fast pesticide detection. The fast detection method comprises the following steps: adopting acetonitrile, anhydrous magnesium sulfate and sodium chloride for mixing in a certain ratio so as to extract pesticide ingredients from the oranges as many as possible; mixing anhydrous magnesium sulfate, N-propyl ethylenediamine, C18 and graphitized carbon in a certain ratio; eliminating influences of fluorescent substances, such as organic acids, pigments, pectin and cellulose, in an extraction liquid. According to the fast detection method, the detection accuracy for the surface enhanced Raman scattering of the pesticide residues in the oranges is greatly increased, the aim of the fast detection of the trace pesticide residues is achieved, and the fast detection method basically meets the requirements of detection limit specified by the state; the fast detection method is adopted to detect the trace pesticide residues in the oranges, is simple in pre-processing of samples to be detected, fast in detection speed, low in detection cost and high in accuracy and precision, can fast and accurately analyze the trace pesticide residues in the oranges in a qualitative and quantitative manner, and can be used for on-site sample detection on a large scale.

A wet recycling method for impregnated active carbon used to remove radioactive organic iodide in a nuclear power plant by extracting impregnated substance and radioactive organic iodide from the used impregnated active carbon with an acetonitrile solution and reproducing active carbon to be used in preparing impregnated active carbon, the filtered extractive solution being distilled to obtain pure acetonitrile for the use purpose as an extractive solution, the impregnated substance and radioactive organic iodide extracted in a small amount of solid, thus reducing the volume of the waste impregnated active carbon greatly to decrease solid waste material and at the same time recycle materials.

The invention relates to three-layer core-shell-structure inorganic nanoparticle / silicon dioxide / high polymer composite microspheres and a preparation method thereof. The average particle size of the composite microspheres is 15-800nm, the particle size is uniform, the three-layer core-shell structure is obvious, and the inorganic nanoparticle is completely coated to enter the silicon dioxide and high polymer shell. By using the hydrophilic high polymer as the stabilizer, the inorganic nanoparticles can be uniformly dispersed in ethanol, acetonitrile or any other polar solvent, and can not generate the phenomenon of aggregation or precipitation; and thus, the invention can implement preparation of the silicon core and polymerization reaction of the high polymer shell in one reaction solvent, thereby saving the process of purifying and washing the silicon core and replacing the reaction system, simplifying the experimental process and greatly shortening the experimental time. Besides, a distillation precipitation polymerization method, which has the advantages of simple reaction and high polymerization efficiency, is adopted to prepare the high polymer shell.

Hydrolyzed nitrilotriacetonitrile compositions are disclosed prepared by a method characterized by a one-shot addition of an amount of nitrilotriacetonitrile to a solution containing an acid catalyst, where the reaction is complete in a time period of less than an hour. The method is also characterized by adjusting the pH of the reaction mixture to a pH of at least 8. The method is also characterized by oxidatively removing free cyanide to a desired low level through the addition of an oxidizing agent the produces environmentally benign by-products to the crude hydrolyzed NTAN to form hydrolyzed NTAN compositions having minimized, negligible, or substantially no free cyanide levels.

The invention discloses a probe reagent for concurrent selection and determination of multiple metal ions, and preparation and appliance, and belongs to the field of organic synthesis and analytical chemistry. Tri (2-aminoethyl) amine serves as a parent, wherein rhodamine B is connected to an amino chain, 2-hydroxy-1-naphthaldehyde groups are connected to other two amino chains respectively, and thus a tripod structured rhodamine-hydroxyl naphthalene derivative probe is prepared. In 1,4-dioxane / water (19 / 1, v / v, pH=7) solution, the probe respectively detects Cu2+, Co2+ and Fe3+ by utilizing rate absorption of different wavelengths, and the detection does not interfere with each other; in acetonitrile / water (19 / 1, v / v) solution, fluorescence emission of different wavelengths under different pHs is utilized, the probe respectively detects Zn2+, Al3+, Hg2+ and Cu2+, and the detection does not interfere with each other; under an ultraviolet lamp of 365 nm, Zn2+, Al3+ and Hg2+ are detected to show blue, pink and orange red fluorescence respectively, and through -Zn2+ mixture detection by the probe, Cu2+ shows blue fluorescence vanishing. The probe structure is as follows.

The embodiment of the invention provides a method for detecting 25(hydroxyl)vitamin D by using a high-pass liquid chromatography-tandem mass spectrometry. The method comprises the following steps of: adding an acetonitrile solution containing an internal standard substance of the 25(hydroxyl)vitamin D into a human serum sample to carry out protein precipitation; sufficiently and uniformly mixing the solution, and then, adding an n-hexane extracting solvent; sufficiently and uniformly mixing the solution, then centrifuging the solution, movably taking a supernatant and drying the supernatant, and adding a complex solution to obtain a sample to be detected; detecting the sample to be detected by using a high-pass liquid chromatography-tandem quadrupole mass spectrometer; and quantifying according to the relative retention time of 25(hydroxyl)vitamin D2 and / or 25(hydroxyl)vitamin D3 and the detected abundance ratio of quantitative ion pairs by using an internal standard curve method. According to the embodiment of the invention, the method has the advantages of simplicity in pretreatment, strong specificity and matrix interference resistance, short detection time, high pass, high detection precision and low cost.

The invention relates to alkyl imidazole perrhenate ionic liquid and a method for preparing the same. The adopted technical proposal is follows: the preparation method comprises the following steps: taking certain volume of alkyl imidazole chloride compounds or alky imidazole bromide compounds, adding deionized water the volume of which is 2 to 4 times of that of the alkyl imidazole chloride compounds or the alky imidazole bromide compounds to dissolve the alkyl imidazole chloride compounds or the alky imidazole bromide compounds, adding the mixture to OH-type anion exchange resin to perform ion exchange, and collecting outflow solution which is alkyl imidazole hydroxide; then adding the alkyl imidazole hydroxide to ammonium perrhenate aqueous solution, wherein the molar ratio of the alkyl imidazole hydroxide to the high ammonium perrhenate is between 1 to 1 and 1 to 2, then stirring the mixture for 3 to 5 hours at a temperature of between 70 and 90 DEG C, reducing the pressure and distilling the mixture to remove water, adding the mixed solution of anhydrous methanol and acetonitrile to the mixture after cooling the mixture, sealing and stirring the mixture intensely, keeping stand the mixture for 10 to 15 hours at a temperature of between 30 DEG C below zero and 40 DEG C below zero, reducing the pressure and distilling the mixture to remove the methanol and the acetonitrile, and performing vacuum drying on the treated mixture. The ionic liquid prepared by the method has the advantages of high yield and high stabilities of air and water.

The invention discloses a recombinant nitrilase, a coding gene, a mutant and engineering bacteria from Acidovorax facilis ZJB09122, and the application thereof to preparation of 1-cyano cyclohexyl acetate. The invention provides a nitrilase and its mutant for hydrolysis of 1-cyano cyclohexyl acetonitrile, the enzyme and its mutant have good regional selectivity and catalytic activity in catalysis of the above reaction, and the production process is environmentally friendly. The invention solves the problems in a traditional chemical hydrolysis of 1-cyano cyclohexyl acetonitrile into 1-cyano cyclohexyl acetate, such as harsh reaction conditions, a large amount of organic solvent required in the reaction, high cost, low yield and serious environmental pollution.

The present invention discloses a compounded full-solid polymer electrolyte for secondary lithium cell and its preparation method. The described polymer electrolyte contains 2%-30% of inorganic oxide, and the matching ratio of polyethylene glycol and alkali metal salt O / Li is 8-16. Its preparation method includes: dissolving polyethylene glycol and LiClO4 in acetionitrile, adding inorganic oxide,pouring the mixed solution onto teflon plate, evaporating solvent and drying at 50-100 deg.C in vacuum drying box. The described inorganic oxide also can be modified inorganic oxide. Said prepared material can be extensively used in the fields of handset, domestic appliances and electric car.

The invention discloses a method for synthesizing acetonitrile through a one-step ammoniating method with acetic acid. The method comprises the following steps of: (1) reacting acetic acid with liquid ammonia in a fixed-bed reactor provided with a catalyst of aluminum oxide to generate a mixed gas containing the acetonitrile; and (2) continuously refining the gas mixture to obtain an acetonitrileproduct. By adopting the method, the acetonitrile product is relatively pure, the purity can reach more than 99.9%, the separation process is relatively simple, the process is short, the energy consumption in the production process is low, the energy consumption of a unit product is about 40% of the energy consumption with a by-product method, and the cost is lower. The separation process adopts a physical separation method, and avoids the problem of generating a great deal of wastewater and waste gas in the chemical process in the by-product method. Meanwhile, because the synthesis method isadopted, the limitation that the yield is restricted by the main product can be thoroughly avoided.

The invention discloses a method for preparing high-purity acetonitrile from acetic acid and ammonia by two steps, which comprises the following steps of: (1) neutralizing acetic acid and ammonia to generate ammonium acetate; (2) mixing aqueous solution of ammonium acetate and gaseous ammonia, preheating, and making the mixture enter a fixed bed reactor filled with a catalyst aluminium oxide for reaction to generate acetonitrile-containing mixed gas; and (3) continuously refining the mixed gas to obtain the acetonitrile. The 70 to 80 weight percent acetic acid is taken as a raw material, and the produced acetonitrile product has the advantages of less varieties and low content of impurities, high purity of over 99.9 percent, simple separation process, shorter flow, low energy consumption only about 40 percent of that of a byproduct method in unit product, and lower cost. The separation process is a physical separation method, and avoids generating a great amount of wastewater and waste gas in the chemical treatment process of the byproduct method. Meanwhile, a synthesis method is adopted, so the limitation that the yield is limited by a main product can be radically eliminated.

The present invention belongs to preparation of aliphatic nitrile or carbocycle and heterocycle compound side chain nitrile, and is especially ethanol ammoxidizing process to synthesize high-purity acetonitrile. Fluidized bed catalytic reaction technology and continuous recovering and refining technology are adopted; and the process features the utilization of ethanol, ammonia and air as main material. Compared with available technology, the acetonitrile product has purity has high as 99.9% and less kinds of impurity, lower power consumption and less waste and waste gas prdouced. The product may be further processed into chromatographic product.

The invention relates to an organic matter and ammonia borane compounded hydrogen storage material. The hydrogen storage material is prepared by compounding the organic matter and the ammonia borane, wherein the organic matter is phthalic anhydride, polyethylene oxide, dextrose, mannitol or mannitol hexaacetic ester. The preparation method comprises the following steps: 1) adding the organic matter to the purified acetonitrile solvent, and stirring for dissolving; 2) dissolving the ammonia borane into the mixing solvent comprising acetonitrile and methanol, and stirring at the temperature of 20 to 70 DEG C to obtain a uniform solution; and 3) carrying out vacuum drying, and removing the solvent, thus obtaining the hydrogen storage material. The invention has the advantages that the ammonia borane and the organic matter are taken as raw materials to prepare the hydrogen storage material at the lower hydrogen discharge temperature; the thermal decomposition and hydrogen discharge temperature of the ammonia borane can be effectively reduced; the generation of harmful gas impurities of borazole, diborane, ammonia and the like is effectively inhibited; the hydrogen storage material has quicker hydrogen discharge kinetics; in addition, the heat discharge amount is less in the hydrogen discharge course; and the enthalpy change of a decomposition reaction approaches to thermal neutrality; and the hydrogen storage material is beneficial to realizing the regeneration of reaction products through a solid-gas reaction or a chemical process under the relatively mild condition.

A process for producing amidine derivatives represented by the following reaction scheme, characterized in that the reactions of steps 1 and 3 are conducted in acetonitrile and the reaction of step 2 is conducted in acetone. 1

The present invention discloses an acrylonitrile compound, a preparation method thereof, and a pest prevention and curing agent with the compound as an active constituent. The compound has structural characteristics as shown in Formula (I). In the preparation method, under the condition with alkaline, an organic solvent at the temperature between minus 10 DEG C and 150 DEG C is used for the reaction between benzofuran acyl chloride or pyrazole acyl chloride and substituted benzyl cyanide, so as to produce an intermediate, the produced intermediate reacts with acyl chloride, and the (I) can be separated. The compound can be used as an active constituent in a pest prevention and curing agent. The present invention has the advantages that the compound has excellent prevention and curing effects on harmful insects and acarus category, the activity of the compound is high, the consumption is low and the security is excellent.

The invention belongs to the field of Chinese medicine analysis and particularly relates to a content measurement method for Chinese patent medicine prepared from sweet wormwood, honeysuckle and gardenia jasminoides fruit. The method measures the content of nine ingredients including neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, caffeic acid, geniposide, secoxyloganin, isochlorogenic acid B, isochlorogenic acid A and isochlorogenic acid C in the Chinese patent medicine by reversed-phase high performance liquid chromatography, wherein the chromatographic conditions include: a chromatographic column is C18 column; methanol or acetonitrile is used as a flowing phase A; 0.05-to-1.0 percent phosphoric acid or 0.05-to-1.0 percent acetic acid is used a flowing phase B; the totalpercentage of flowing phases A and B is 100 percent; and gradient elute is performed. The content measurement method has high repeatability; and the method completely reflects the main ingredients and the change of the main ingredient content of the medicine from a qualitative prospect respectively and thus improves the level of the control over the quality of the medicine.

The non-aqueous electrolyte solution of the present invention is a non-aqueous electrolyte solution comprising acetonitrile and a lithium salt, wherein the anion of the lithium salt has a LUMO (lowest unoccupied molecular orbital) energy in the range of −2.00 to 4.35 eV, and a HOMO (highest occupied molecular orbital) energy in the range of −5.35 to −2.90 eV.

The invention discloses a making method of 3.4.3'.4'-biphenyl tetracarboxylic dianhydride, which comprises the following steps: adopting 4-chlorophthalandione anhydride as raw material; preparing 4-chlorophthalandione dimethyl ester, 3.3'.4.4'-biphenyl tetracarboxylic tetramethyl ester, 3.3'.4.4'-biphenyl tetracarboxylic acid and 3.3'.4.4'-biphenyl tetracarboxylic dianhydride; coupling; hydrolyzing; refining; (1) adopting p-toluenesulfonic acid as esterifying catalyst in the preparing procedure of 4-chlorophthalandione dimethyl ester; (2) adopting acetonitrile as solvent in the coupling procedure; (3) purifying hydrolytic 3.3'.4.4'-biphenyl tetracarboxylic acid through deionized water in the refining procedure; (4) washing and purifying 3.3'.4.4'-biphenyl tetracarboxylic dianhydride through acetone.