60 results about "Tert-butyl methyl ether" patented technology

Application of a reference mixture of natural products for systematic analysis and comparison of the properties of biphasic solvent systems in counter-current/partition chromatography. Because the reference mixture is comprised of compounds with varying polarities, functional groups, and structural features it provides a rational method for mapping the optimal resolution polarity range of a particular solvent system. The mapping of optimal resolution polarity ranges of solvent systems provided for the description of the overall optimal resolution polarity range of a solvent system family, comprised of the same solvents in different proportions. By comparing the reference mixture performance in the individual members of a solvent system family, the solvent system that best functions as the representative of, or portal to, the solvent system families is determined. Use of the reference mixture also afforded a method to compare the overall optimal resolution polarity ranges of solvent system families. Based on performance of reference mixture chromatograms, the CCC properties of solvent systems, can be compared and their CCC potential examined. The methods of the invention employing the reference mixture provides was used to identify a quaternary solvent system, hexane/t-butylmethylether/acetonitrile/water (HterAcWat), which was found to be useful for CCC of mixtures containing natural products.

The invention relates to a method for determining the content of astaxanthin in antarctic krill oil by chromatography, which comprises the steps of adopting a gel purification column with a BIO-3X packing, taking ethyl acetate and cyclohexane as eluant according to the proportion of 1:1, and collecting a fractions at 7.48-12.60min; carrying out low-temperature saponification in a solvent formed by methylene dichloride and methanol after purification, and completely converting astaxanthin esters to free astaxanthin; adopting a YMC-Carotenoid C30 chromatographic column; carrying out gradient elution by taking water solution of the methanol, methyl tert-butyl ether and 1% of phosphoric acid as a mobile phase; leading the flow rate to be 1.0mL/min, using an ultraviolet detector as the detector, and leading the detecting wavelength to be 474nm; and determining three isomers of the astaxanthin and adopting the sum of three peak areas for quantifying. The gel chromatographic column can better separate fat from the astaxanthin in the antarctic krill oil, and the adoption of the C30-reversed phase high performance liquid chromatography can accurately determine the content of the astaxanthin, thereby objectively and truly evaluating the quality of the antarctic krill oil.

This invention relates to anti thrombus medicine (+)-(S-)-chlorine pyrrole rayl bisulfate preparation method. (+)-(S-)-chlorine pyrrole rayl free alkali shown as formula (I) is added in organic solvent, and weight concentration 10-100 perent sulphuric acid solution is dropwised at 6-20 degree centigrade, then the reaction is kept for 10 minute to 1.5 hours at 50-65 degree centigrade and the temperature is protected, finally formula (II) compound is got after filtration. The sulphuric acid solution is made by sulfuric acid dissolved in organic solvent, the organic solvent is one or more of the following, ethyl formate, methyl acetate, ethyl acetate, butyl acetate, aether, isopropyl ether, tertiary butyl methyl ether or methylene chloride. Mol ratio of compound (I) and sulfuric acid is 1:0.95-1.05. The synthesis in this invention is safe and high efficiency, it is propitious to industrial manufacture, product purity is high, yield is high, and crystal form fluidity is good.

The invention belongs to the technical field of physiochemical detection of tea leaves and in particular relates to a method for determining alkaloids in tea leaves by using a GC-MS (Gas Chromatography-Mass Spectrometer) method. The method comprises the following step of determining nicotine and minor alkaloids (including nicotine, nornicotine, myosmine, neonicotine, neonicotine and cotinine) in tea leaf powder. The method is a method for extracting nicotine substances from the tea leaves by using a centrifugal tube filled with 0.01% triethylamine/tert-butyl methyl ether solution and analyzing the nicotine substances in the tea leaves by using a gas chromatography-mass spectrometer (GC-MS) method. When the method provided by the invention is used for detecting the content of the nicotine in the tea leaves, the method is rapid and effective, the pre-treatment is simple, an average relative standard deviation is smaller than 10 percent, and the average recycling rate of each index is 86.2 percent to 92.1 percent. The method has the advantages of rapidness and accuracy, high sensitivity and good repeatability.

The invention discloses a method for synthesizing phenetyl, which uses p-chlorophehol or p-bromophenol as starting reaction raw material. It first uses methyl, benzyl or tert-butyl to protect the phenolic hydroxyl, the parivis which is protected by the phenolic hydroxyl reacts with the magnesium in the ether, tetrahydrofuran, tert-butyl methyl ether, isopropyl ether and its mixing solution to obtain the Grignard reagent, the Grignard reagent directly reacted with the etox to obtain the tyrosol which is protected by the phenolic hydroxyl, the tyrosol reacts with the dimethyl sulfate, dimethyl carbonate, trimethyl orthoformate to obtain the tyrosol ether which is protected by phenolic hydroxyl, which obtains the product in acid or hydrogenation protection.

The invention relates to a method for simultaneously detecting five kinds of steroid hormones in serum. The five kinds of steroid hormones are respectively testosterone, androstenedione, 11-deoxycortisol, cortisol and cortisone. The method for simultaneously detecting the five kinds of steroid hormones in the serum comprises the following steps: sample pretreatment: adding an acetonitrile solution of an internal standard substance in a serum sample for carrying out protein precipitation, then adding tert-butyl methyl ether for extracting, blow-drying supernatant, adding a combination solution, and taking the supernatant, thus obtaining a to-be-detected sample; enrichment, separation and detection: carrying out enrichment, separation and detection on the to-be-detected sample by adopting a two-dimensional liquid chromatography-tandem quadrupole mass spectrometer. According to the method for simultaneously detecting the five kinds of steroid hormones in the serum, disclosed by the invention, the method is adopted for simultaneously detecting five kinds of compounds of which the concentration ranges are inconsistent in the serum, and the time for simultaneously detecting the five kinds of the compounds is about 8.5 to 12.0 minutes; the method for simultaneously detecting the five kinds of steroid hormones in the serum is low in cost, high in flux, high in precision degree and strong in specificity.

The invention discloses a method for simultaneously measuring the concentrations of six tyrosine kinase inhibitors in blood plasma. Imatinib is adopted as an internal standard, a medicament in the blood plasma is extracted at first by virtue of a mixed solution of ethyl acetate and tert-butyl methyl ether, then a sample is separated by virtue of high performance liquid chromatography, medicament targeting detection is performed in a high resolution mass spectrometry parallel reaction monitoring mode, and secondary fragment ions of the medicament are used for quantification, so as to realize simultaneous analysis and measurement of the concentrations of the six tyrosine kinase inhibitors in the blood plasma. The method is quick, has the advantages of extremely high targeting performance, high speed, high throughput, high sensitivity, high specificity, high precision and accuracy, high stability, high extraction recovery rate, no obvious substrate effect or dilution effect, and the like, and can be used for plasma concentration monitoring of clinically common antitumor medicaments, i.e. tyrosine kinase inhibitors, and a nanogram-level detection limit can be achieved.

The invention provides a method for detecting banned azo dyes in printing ink, coatings and paint. The method comprises the following steps: performing reduction and decomposition on a sample in a sodium citrate buffer solution medium in the presence of sodium hydrosulfite to generate possible banned aromatic amine, then extracting aromatic amine from an extracting solution by a liquid-liquid extraction method, and detecting by GCMS with a mass selection detector. According to the method, methyl alcohol is used to extract disperse dyes in the sample, so that the disperse dyes in the sample can be extracted as much as possible, and other impurities in the sample are prevented from being extracted overmuch. A sodium hydroxide solution is added into a test tube so as to neutralize to obtain proper pH, and a generated amine substance is relative stable under the pH condition. Five milliliters of tert-butyl methyl ether is added to facilitate liquid-liquid extraction. A moderate amount of sodium sulfate is added so as to absorb water, accelerate layering and facilitate removing of part of impurities in an organic phase.

The invention relates to natural gas metal cutting gas which is prepared from liquefied natural gas and an additive, wherein the additive is prepared from diphenylcarbinol, propylcyclohexanol, tert-butyl methyl ether, methanol, anhydrous ethanol and gasoline. The natural gas metal cutting gas is prepared from the following components in parts by weight: 98.4-98.7 parts of the liquefied natural gas and 1.3-1.6 parts of the additive. The additive is prepared from the following components in parts by weight: 7-30 parts of diphenylcarbinol, 10-20 parts of tert-butyl methyl ether, 40-60 parts of methanol, 2-10 parts of anhydrous ethanol and 3-6 parts of gasoline. According to the natural gas metal cutting gas provided by the invention, the additive and the natural gas jointly take part in combustion reaction in oxygen after the natural gas is liquefied and the natural gas metal cutting gas provides a chemical intermediate for combustion of the natural gas to improve the combustion speed of the natural gas in oxygen so as to improve the combustion temperature; the natural gas metal cutting gas is safe to use, free of tempering if being used for cuing and the like, and moreover, the cutting gas is lower than air in specific gravity, and can be used for indoor operation.

The invention provides a methanol gasoline efficient composite additive. The methanol gasoline efficient composite additive is prepared from, by weight, 8-10 parts of diethoxymethane, 5-7 parts of tert-butyl methyl ether, 1-1.5 parts of isooctyl phosphate, 1.5-2 parts of nanometer cobalt ferrite, 1.5-2 parts of n-heptane, 5-7 parts of propanediol butyl ether, 4-5 parts of coconut diethanolamide, 1-1.5 parts of isotridecyl stearate and 2-3 parts of sodium lauroyl sarcosine. The methanol gasoline efficient composite additive contains multiple cosolvents, a dispersant, a kinetic promoter and an anticorrosive agent, and is prepared through a special method by using a unique formula of all components, and all the components have protruding synergism; and the methanol gasoline efficient composite additive obviously improves the water resistance of methanol gasoline, reduces the discharge effects of combusted NOX, HC and CO, and also has kinetic lifting and certain gasoline consumption reduction effects by using a special formula.

The invention discloses a mobile phase formulation for measuring carotenoid through liquid chromatography and application of the mobile phase formulation and belongs to the field of methods for separating and metabolizing micromolecules through liquid chromatography. The mobile phase formulation comprises, by volume, A1 phase: 90-100% of methanol-water and B1 phase: 90-100% of tert-butyl methyl ether-methanol. By the mobile phase formulation, chromatograms and testing results of 7-10 carotenoids which are independent in components, good in peak pattern and linear relation, high in adding standard recovery rate and little in relative error can be acquired simply, accurately and quickly (the whole process can be completed within 40min).

The invention relates to an industrial production method of sitagliptin. The preparation method using 7-[3-amino-1-oxy-4(2,4,5-trifluorophenyl)-2-butenyl]-5,6,7,8-tetrahydro-3-(1-trifluoromethyl)-1,2,4-triazole[4,3,alpha] pyrazine as a starting material comprises the following steps of: (1), carrying out asymmetric catalytic hydrogenation reaction on the 7-[3-amino-1-oxy-4(2,4,5-trifluorophenyl)-2-butenyl]-5,6,7,8-tetrahydro-3-(1-trifluoromethyl)-1,2,4-triazole[4,3,alpha] pyrazine to generate sitagliptin free alkali with ee of more than 95% in the presence of catalytic amount of (1,5-cyclooctadiene) ruthenium dichloride and S-(-)-1,1-binaphthyl-2,2-diphenyl phosphine; (2) salifying the sitagliptin free alkali and phosphoric acid in methyl tert-butyl methyl ether to obtain the sitagliptin with ee of more than 99%, wherein the sitagliptin can completely achieve clinical medication requirements. The used catalyst is low in price and the used amount of the catalyst is only 0.2mol%, and therefore, the industrial production method of the sitagliptin is lower in cost and suitable for industrial production.

The invention provides a M60-M85 methanol gasoline additive for high cleaning vehicles and a methanol gasoline thereof. After the M60-M85 methanol gasoline additive for high cleaning vehicles is added into the M60-M85 methanol gasoline, the methanol gasoline has the advantages of favorable compatibility, high water resistance, no air resistance, high heat value, high combustion safety and the like, enables the automobile to perform cold starting easily, and inhibits the rubber plastic from swelling and cracking. The additive is free of any tert-butyl methyl ether component, or lead, aluminum, manganese or any other nonferrous metal ion, and is environment-friendly. The M60-M85 methanol gasoline additive can be directly used under the condition of not modifying the existing automobile engine.

The invention discloses a navigation alcohol fuel combustion-supporting additive for an automobile, which solves the technical problems that an engine is hard to start, the oil consumption is great and exhaust gas emission is great as the existing methanol gasoline is hard to combust fully. The combustion-supporting additive comprises more than two reagents in the following components in parts by weight: 20-40 parts of mixed C4-C6 alcohol, 10-30 parts of ethyl formate, 10-30 parts of fatty acid, 0.5-2 parts of diisopropyl ether, 2-8 parts of tert-butyl methyl ether, 0.5-3 parts of cerium nitrate, 8-16 parts of a low-carbon solvent and 5-15 parts of mixed benzene. By adding the combustion-supporting additive disclosed by the invention, the defect in the prior art that methanol gasoline is hard to combust fully is overcome.

The invention discloses a methanol gasoline efficient composite additive and a preparation method thereof. The methanol gasoline efficient composite additive is prepared from the following formula ingredients in parts by mass: 5 to 8 parts of diethoxymethane, 6 to 8 parts of [2.2]paracyclophan, 5 to 6 parts of tetraethylenepentamine, 2 to 4 parts of arachidic acid, 6 to 10 parts of tert-butyl methyl ether, 5 to 7 parts of n-heptane, 4 to 6 parts of propanediol butyl ether, 4 to 6 parts of 2,2,4-trimethylpentane, 6 to 8 parts of isooctyl phosphate, 2 to 4 parts of nanometer cobalt ferrite and 3 to 4 parts of coconut diethanolamide. The methanol gasoline efficient composite additive has the advantages that the effects of obviously improving the water resistance of methanol gasoline and obviously reducing the emission of NOX, HC and CO are achieved; meanwhile, the effects of improving the power and reducing oil consumption to a certain degree are also achieved through a special recipe.

The invention relates to a method for analyzing tert-butyl methyl ether in soil by purge-and-trap and GC-MS. The method for analyzing tert-butyl methyl ether in soil by purge-and-trap and GC-MS comprises the following steps: (1) purge-and-trap extraction is carried out for tert-butyl methyl ether in soil; (2) after trap extraction in the step (1), tert-butyl methyl ether is analyzed by GC-MS. Theinvention provides the method for analyzing tert-butyl methyl ether in soil with simplicity, high efficiency and accuracy, purge-and-trap pretreatment and standard quadrupole mass spectrum all scanning surface analysis are used for tert-butyl methyl ether in soil, the method is simple and rapid, content of methyl tert butyl ether in the soil can be accurately detected, and substance monitoring blank of soil can be filled.

The invention discloses a synthesis method for 4-bromo-o-phenylenediamine. The synthesis method comprises the following synthesis steps of: A, enabling o-phenylenediamine to react with a bromo reagent in acetic acid and acetic oxide to obtain 4-bromo-o-phenyl diacetyl amide; B, dissolving the 4-bromo-o-phenyl diacetyl amide in methyl alcohol, then, adding 5N sodium hydroxide aqueous solution, and hydrolyzing to obtain the 4-bromo-o-phenylenediamine, wherein the bromo reagent in the step A comprises sodium bromide and hydrogen peroxide. According to the synthesis method disclosed by the invention, the sodium bromide and the hydrogen peroxide are used as the bromo reagent instead of liquid bromine, and therefore, the reaction route is safe and environmentally friendly, the cost is low, the reaction condition is mild, the regioselectivity is high, and the bromine atom use ratio is high. A crude product generated by the invention is recrystallized by using tert-butyl methyl ether, and the obtained 4-bromo-o-phenylenediamine is high in purity.

A method for quantitative determination of 25-hydroxycholecalciferol in feed is described. The method includes the steps of adding a defined amount of an internal standard which has a mass different from 25-hydroxycholecalciferol and a polarity similar to that compound, e.g., 26,27-hexadeutero-25-hydroxycholecalciferol, to an aqueous dispersion of the feed, extracting the aqueous dispersion with tert.butyl methyl ether and further processing the extract by HPLC and mass spectrometry as described in the specification.

The invention relates to a device for detecting antioxidants in vegetable oil or animal fat and an operating method thereof, and belongs to the technical field of high performance liquid chromatography (HPLC). The method for detecting antioxidants in the vegetable oil or animal fat can quickly detect the objects with antioxidant activity in the oil and fat. The device for detecting antioxidants in vegetable oil or animal fat is composed of a high performance liquid chromatograph (HPLC includes a high-pressure pump, a silicone liquid chromatographic column, a visible ultraviolet detector, a sampler, a signal recorder), a high-pressure pump, a visible detector, a signal recorder, a T-joint for the HPLC, a buffer, and a reaction cycle, and utilizes a chemical radical Galvinoxyl to detect antioxidant in mixture. HPLC mobile phase utilizes n-hexane and tert-butyl methyl ether, and the radical solvent is n-hexane. Components in the oil and the fat are reacted with the radical after being separated by the high performance liquid chromatography (HPLC) one by one, wherein components with antioxidant activity enable the radical to fade and to be the negative peak. Chromatograms being compared with those reacted with the radical, the number of the antioxidants in the oil and fat, retention time and the antioxidant activity of the components can be acquired. The method for detecting the antioxidants in the vegetable oil or animal fat has the advantages of being quick and easy, and high in sensitivity.

The invention discloses a eugenol synergistic emamectin benzoate anti-mite suspending agent. The eugenol synergistic emamectin benzoate anti-mite suspending agent is characterized by being prepared from the following raw materials: emamectin, methanol, a phosphoric acid solution, methylbenzene, isopropyl acetate, tert-butyl methyl ether, benzoic acid, n-hexane, oil of leaves of flos caryophylli, a sodium hydroxide solution, cyclohexane, sodium citrate, dimetyl carbonate, potassium carbonate, petroleum ether, acetone, chitosan, acetic acid, fatty alcohol polyoxyethylene ether, liquid paraffin, vinyl acetate, an ammonium persulfate solution, hexamethyl phosphoryl triamide, dimethyl formamide, sodium lignin sulfonate, ethylene glycol and an appropriate amount of deionized water. The eugenol synergistic emamectin benzoate anti-mite suspending agent disclosed by the invention is capable of efficiently inducing mites and effectively killing the mites and has a good synergistic function, the dosage of the eugenol synergistic emamectin benzoate anti-mite suspending agent in a field is reduced, and pesticide residue and damage to beneficial organisms can be effectively reduced; meanwhile, the prevention and treatment cost is reduced, and the pollution to the environment is relieved.

The invention discloses a method for preparing 3-ester group catechin. The method comprises the following steps: (1) carrying out a phenolic hydroxyl selective esterification reaction on catechin and acid anhydride under a condition that tertiary amine serves as alkali and tert-butyl methyl ether serves as a solvent, and carrying out posttreatment after the reaction is completed to obtain 3,4',5,7-tetraester group catechin; (2) reacting the 3',4',5,7-tetraester group catechin with an acylating reagent to generate 3-ester group-3',4',5,7-tetraester group catechin; (3) treating the 3-ester group-3',4',5,7-tetra-ester group catechin with a selective deprotection reagent to obtain the 3-ester group catechin (I). The preparation method has a relatively good selectivity, and the selectivity and yield of intermediate and target products are relatively high; the preparation method is simple to operate, adoption of toxic or corrosive reagent is avoided, the reaction condition is mild, and thus the preparation method is suitable for industrial production application.

The invention provides a method for detecting four progestational hormones in serum. The four progestational hormones are 17alpha-hydroxypregnenolone, 17alpha-hydroxyl progesterone, progesterone and pregnenolone; and the method comprises the following steps: adding a methanol solution containing an internal standard substance in a serum sample, performing protein precipitation, centrifuging and taking supernatant, adding derivatization reagent to perform derivatization reaction, cooling to room temperature and then adding tert-butyl methyl ether, centrifuging and taking the supernatant, thereby obtaining a to-be-detected sample, wherein the internal standard substance is 17alpha-hydroxypregnenolone internal standard substance, the 17alpha-hydroxyl progesterone internal standard substance, the progesterone internal standard substance and pregnenolone internal standard substance; enriching, separating and detecting: performing enriching, separation and detection on the to-be-detected sample by adopting a two-dimensional liquid chromatography tandem quadrupole mass spectrometer. Through the method provided by the invention, the matrix interference can be effectively removed, and the method has the features of being strong in specificity and matrix interference resistance, low in quantitation and high in sensitivity.