34 results about "Deuterated chloroform" patented technology

The invention discloses deuterated diazepam and a preparation method thereof. The preparation method of deuterated diazepam comprises the following steps of: (1) mixing 7-chlorine-1-methyl-5-phenyl-1,3-dihydro-1,4-benzodiazepine-2-ketone and N,N-dimethyl formamide, and stirring; (2) adding potassium carbonate and deuterated chloroform, heating the mixture to more than 40 DEG C and stirring; and (3) carrying out separation to obtain the deuterated diazepam. The preparation method provided by the invention is short, simple and convenient to operate, low in cost and easy to purify. The commercially available non-deuterated diazepam uses a small amount of deuterated reagents as deuterium sources in a non-deuterated solvent atmosphere, so that deuterated diazepam is obtained in a relatively short period of time, and through simple column chromatography purification, a purified product is purified. The deuterated diazepam standard product prepared according to the invention is high in purity and stable in chemical property; and the preparation of the standard product for analysis is convenient. The preparation method provided by the invention can be used for producing deuterated internal standard substance used for analyzing and detecting diazepam.

The invention discloses deuterated estazolam and a preparation method thereof. The preparation method comprises following steps of (1) adding 6-phenyl-8-chlorine-4H-[1,2,4] triazole-[4,3-a][1,4] benzo-diazepine into dimethyl sulfoxide or N,N-dimethylformamide, mixing and stirring; (2) adding a catalyst cesium carbonate or potassium carbonate as well as deuterated chloroform, stirring and heating up to over 40DEG C; and (3) separating so as to obtain deuterated estazolam. The preparation method is concise, is simple and convenient to operate, has low cost, and is easy for purification. Commercially available non-deuterated estazolam can be converted into deuterated estazolam by a little deuterated reagent used as a deuterium source in the non-deuterated solvent atmosphere in shorter time, and a pure product can be obtained through simple purification by column chromatography. The standard deuterated estazolam prepared by the method has high purity and stable chemical property, and is convenient for preparing standard substances for analysis. The preparation method can be used for producing, analyzing and detecting the deuterated internal standard substance used by estazolam.

The invention provides a method for preparing deuterochloroform. The method comprises the following steps: (1) enabling sodium trichloroacetate, calcium oxide and heavy water to react at 80-95 DEG C,and terminating the reaction after the heavy water completely react so as to obtain a crude product; (2) drying and separating the crude product obtained in the step (1), thereby obtaining deuterochloroform. As reagents are cheap chemicals which are common and easy to use, the method is small in side reaction, easy in reaction product separation, simple in process, high in yield, low in cost and great in social and economic benefit.

The invention discloses polycarbonate polyols, and a preparation method and applications thereof. The polycarbonate polyols comprise repetitive units disclosed as Formula (A) and terminal groups, wherein R is C3-C15 bivalent aliphatic hydrocarbons; and 92-99.9% of the terminal groups are hydroxyls. In 1H-NMR of the polycarbonate polyols, when deuterated chloroform is used as a solvent and primary standard substance, the chemical shift of the deuterated chloroform signal is set at 7.26ppm; and when the 3.90-4.45ppm signal integral value is set at 1000, the 3.70-3.85ppm signal integral quantity is 0.1-10.

The invention discloses an H-NMR method for identifying beef, pork or duck meat doped in mutton. The method comprises the following steps: weighing a proper sample by a nuclear magnetic resonance hydrogen spectrum method of pork or duck meat, extracting by adopting an organic solvent, adding a proper amount of ultrapure water, carrying out vortex centrifugation, carrying out nitrogen blowing on anupper organic phase, dissolving a small amount of treated sample by using TMS-containing deuterated chloroform, and analyzing by adopting a 400MHz nuclear magnetic resonance spectrometer; and judgingwhether the sample mutton is true mutton or not according to the obtained nuclear magnetic resonance hydrogen spectrum fingerprint. The identification method disclosed by the invention is simple, efficient in detection, high in result accuracy and good in reproducibility, and in addition, the identification method has reference significance for researching the authenticity of mutton doped with other meat or other meat and meat products.

The invention relates to the technical field of food detection, in particular to a method for identifying and quantitatively analyzing adulteration in zanthoxylum bungeanum by using nuclear magnetic resonance hydrogen spectrum.The method comprises the steps that after a zanthoxylum bungeanum sample is subjected to deuterated chloroform extraction, a hydrogen spectrum signal is tested; the obtained hydrogen spectrum data is subjected to peak displacement correction, data binning and normalization processing, a random forest model is established, and a test standard for judging oil doping or pepper doping is formed. And according to a random forest model discrimination result, respectively finding oil-doped and Shandong pepper-doped difference marker signals. Linear fitting is carried out on the pepper difference marker signals of different oil doping amounts or pepper doping amounts and the oil doping amounts or the pepper doping amounts to obtain the relation between the peak area and the oil doping amounts or the pepper doping amounts, and the relation can be used for quantitatively analyzing the oil doping amounts or the pepper doping amounts in the peppers; the problems that an existing sensory evaluation method adopted for pepper adulteration identification has high professional requirements for reviews, the evaluation result is easily interfered by external factors, and adulteration cannot be accurately quantified are solved.

The invention belongs to the technical field of detection and analysis, and particularly discloses a nuclear magnetic resonance spectrum analysis method for biodegradable plastics, which comprises the following steps: S1, extracting the biodegradable plastics by trichloromethane to obtain an extraction solution; S2, evaporating the extraction solution to dryness to obtain an extract for later use; S3, adding deuterated chloroform into the extract in the step S2, and dissolving to obtain a solute; and S4, detecting the dissolved matter in the step S3 by a nuclear magnetic resonance spectrum. The method at least has one of the following beneficial effects: trichloromethane is adopted to separate and extract the biodegradable plastic product, a nuclear magnetic resonance (NMR) spectrum method is adopted to qualitatively and quantitatively analyze the extract, and 1, 2, 4, 5-tetrachlorobenzene is taken as a quantitative internal standard to calculate the content of the degradable polymer in the to-be-detected sample. Therefore, rapid detection of the degradable components in the biodegradable product is realized.

The invention relates to a method for detecting the content of polycyclic aromatic hydrocarbon in a resin material, and belongs to the field of testing of raw materials for tire production. The method comprises the following steps of: 1) performing sample treatment, specifically, dissolving hydrocarbon resin in an alkane solvent, quantitatively transferring an alkane solution into an SPE column, performing eluting with alkane, and collecting a purified part; 2) dissolving dried residues with deuterated chloroform, then carrying out nuclear magnetic resonance test, and carrying out a deuterated chloroform blank experiment. and 3) carrying out integration on nuclear magnetic hydrogen spectra and calculating the HBay content according to a formula. The method has the advantages of high accuracy and rapidness, and better repeatability and reproducibility. The method can monitor the content of hydrocarbon resin polycyclic aromatic hydrocarbon HBay in raw materials for tires, so that the purpose of monitoring the content of the polycyclic aromatic hydrocarbon HBay in the tires from the production source is achieved, and the generation of environment-unfriendly tires is prevented.

The invention relates to a method for detecting overheating treatment of vegetable oil, and use of the method in the field of edible oil. The method is specifically characterized by comprising the steps of taking 100mu L of an oil sample, adding 400mu L of deuterated chloroform into the oil sample, taking tetramethylsilane (TMS) as internal standard, wherein d is equal to 0, testing 1 <1>H-nuclear magnetic resonance (1H-NMR) spectrum, and taking an aldehyde-group hydrogen characteristic signal (the characteristics of which are as shown in E and F in figure 1) as the proof of the detected vegetable oil being subjected to the overheating treatment, wherein the signal appears when delta H in the 1H-NMR spectrum is equal to 9.0-10.0. After the method is adopted, gutter oil can be simply and rapidly detected.

The invention discloses a polymer type lyotropic liquid crystal material as well as a preparation method thereof and application thereof in chiral drug resolution. Firstly, pseudo-dipeptide polyisocyanide adopting chiral naphthylethylamine as a side chain is synthesized, and then a low-concentration polymer lyotropic liquid crystal material is successfully assembled in deuterated chloroform. Afteran aryl propionic acid anti-inflammatory drug to be detected is mixed with the lyotropic liquid crystal material, a nuclear magnetic resonance hydrogen spectrum signal with separated spectral lines is determined, and the optical purity of the chiral drug can be rapidly detected. The preparation method is efficient, the detection process is simple, the chemical displacement difference value is large, and high-throughput chiral analysis is achieved.

The invention belongs to the technical field of medicine synthesis, and particularly relates to a method for preparing a compound pyrrolo [2, 1-a] isoquinoline alkaloid with a lamelline structure through a one-pot method. According to the invention, a tetrahydroisoquinoline derivative and a (Z)-5-phenylpent-2-ene-4-alkyne aldehyde derivative are used as raw materials, are heated to 100-130 DEG C under the catalysis of trifluoroacetic acid, and reacted for 5 hours, so that the 1-phenyl-5, 6-dihydropyrrolo [2, 1-a] isoquinoline alkaloid is obtained by a one-step method. The method has the advantages that the reaction condition is simple, the substrate has high universality and can be well converted into the target compound, an oxidizing agent does not need to be additionally used, and the compound needs to be stored in a dark place under the condition of deuterated chloroform. The compounds provide a relatively simple method for synthesizing medicines for treating sterility, and the skeleton has effective cytotoxic activity on in-vitro tumor cells.