30results about How to "High derivatization efficiency" patented technology

The invention discloses a method for separating and determining 1,2-propylene glycol, bulk drugs containing 1,2-propylene glycol and 1,2-propylene glycol enantiomer impurities in preparations of the bulk drugs by using precolumn derivatization gas chromatography. The method employs an aldehyde ketone compound as a derivative reagent, carries out precolumn derivatization on the aldehyde ketone compound and 1,2-propylene glycol in the presence of a catalyst and a water reducer and determines trace enantiomer impurities by using gas chromatography. The method provided by the invention overcomes the defect of incapability of accurate quantification of 1,2-propylene glycol enantiomer impurities due to serious trailing of peaks during frequently-used chiral gas chromatographic column separation and guarantees that the quality of 1,2-propylene glycol, the bulk drugs containing 1,2-propylene glycol and the preparations thereof is controllable.

The present invention provides a derivatization method and the application thereof of a sample based on the needlepoint in a top empty bottle, and includes the following procedures: 1, using a minim injector to suck the derivatization reagent and insert the needlepoint into the empty top of a top empty battle in which the sample is preset. 2, making the derivatization reagent form a liquid drop hanging on the needlepoint of the injector and exposes in the empty top of the sample. 3, after a period of derivatization, sucking back the derivatization reagent, and the derivatization process is finished. 4, taking the injector out conducts analysis by instruments directly according to requirements. The derivatization method can be applied in top air of the tobacco sample, or acid ingredient in cigarette smoke and the derivatization of aldehyde ketone ingredient. The present invention has the advantages of simple operation, high efficient derivatization, and lower cost; a trace of derivatization reagent can meet the derivatization purpose of the analysis requirements without memory effect and discrimination effect of the analyzed object. Simultaneously, the present invention combines the liquid phase extraction technology and the derivatization means, improves the sensitivity by the enrichment function of the liquid phase extraction, reduces the dosage of the extraction solvent, and shortens the preparation time.

The invention relates to an flatoxin and sulfanilamide drug light derivatization device. An array ultraviolet LED is taken as an excitation light source, and an excitation wavelength is between 280 nmand 380 nm. A fine internal-diameter pipeline which allows ultraviolet light to pass is taken as a derivatization reaction tank, the derivatization reaction tubes are arranged in a linear mode, the internal diameter of the derivatization reaction tube is 0.15-0.5 millimeters, a length is 0.5-12 meters, and the volume of the derivatization reaction tank is 100-1000 [mu]L. The fluorescence intensity of flatoxin B1 is increased by 6.5 times by the light derivatization device, and the light derivatization device is suitable for requirements of derivatization after high performance liquid chromatography columns and flow injection analysis derivatization.

The invention belongs to the field of analytical chemistry and in particular relates to a detection and analysis method for the content of trace triptolide in a biological sample. The method specifically comprises the following steps: carrying out stable isotopic labeling derivatization reaction on the triptolide and a derivatization reagent d0- / d3-3-N-methyl-2'-carboxyrhodamine 6G; after filtering a derived product, which is obtained by specifically extracting through a magnetic molecularly imprinted polymer, through a filtering membrane, detecting by utilizing an ultra performance liquid chromatography triple quadrupole tandem mass spectrometry analysis system. According to the detection and analysis method, the trace triptolide is labeled and derived by utilizing a stable isotopic labeling derivatization reagent with permanent positive charge d0- / d3-MCR6G; reaction is moderate and rapid and the efficiency is high; the chromatographic separation degree and the mass spectrum ionization efficiency of an analyte are remarkably improved. The magnetic molecularly imprinted polymer provided by the invention is used for selectively identifying and enriching a target object in a complicated sample and reducing matrix interference; the magnetic molecularly imprinted polymer has the advantages of simplicity in preparation, good stability and high selectivity and recycling rate.

The invention discloses a fatty acid LC-MS / MS analysis method based on double derivatization technology, comprising the following steps: 1. preparing a fatty acid mixed standard solution; 2. preparing a 2-hydrazinopyrimidine derivatization solution; 3. preparing a derivative 4. Prepare 2-hydrazino-4,6-dimethylpyrimidine derivatization solution; 5. Prepare each standard curve solution to be tested; 6. Use LC-MS / MS method to detect each standard curve to be tested solution, to establish a standard curve for various fatty acids; 7. Take the sample to be tested, add DMP derivatization solution and mix until the fatty acids are derivatized, then add the derivatization internal standard solution, mix well, take the supernatant after centrifugation, and use LC-MS / MS method to measure the type and content of fatty acids. The invention can effectively improve the sensitivity and specificity of mass spectrometry detection of fatty acids, and can realize simultaneous quantitative analysis of short-chain, medium-chain, long-chain and ultra-long-chain fatty acids.

The invention discloses a chemical derivatization method and an application thereof to nucleic acid modification detection by a liquid chromatogram-mass spectrometer (LC-MS) method. A derivatization strategy is performed on 5-methylcystein, 5-hydroxymethylcytosine, 5-aldehyde cytosine and 5-carboxylcytosine in deoxyribonucleic acid (DNA) by means of 2-bromo-1-(4-dimethylamino-phenyl)-ethyl ketone (BDAPE). Retention behaviors of modified nucleosides in reversed phase liquid chromatography are remarkably improved, and meanwhile, the detection sensitivity of the modified nucleosides in mass spectra is greatly improved. The chemical derivatization method has the advantages that the sensitivity and the selectivity are high, the operation is simple and convenient, quantitative detection of cytosine modification with extremely low abundance in the DNA can be achieved without complicated sample pretreatment, and the method can be applied to analysis of diseases and study on mutual relation among the 5-methylcystein, the 5-hydroxymethylcytosine, the 5-aldehyde cytosine and the 5-carboxylcytosine.

The invention belongs to the field of mass spectrometry detection, and specifically discloses application of reactive matrix3-hydrazino-benzoic acid derivatized glucan to MALDI-TOF-MS mass calibration. 3-hydrazine-benzoic acid reacts with hemiacetal at the tail end of reducing sugar in a hydrazone mode, reaction is high in derivatized efficiency, a target board is used for online derivation, and operation is simple and convenient; the derivative strategy is used, and derivatized products can be detected in a positive ion mode and a negative ion mode; and carboxylate radical in the 3-hydrazine-benzoic acid significantly improves the ionization efficiency of the reducing sugar in the negative ion mode. According to the application, the 3-hydrazino-benzoic acid derivatized glucan is used as amass calibration object of MALDI mass spectrometry, mass difference between adjacent signal peaks is 162Da, and the accurate calibration is realized simultaneously in the positive ion mode and the negative ion mode corresponding to a glucose residue.

The present invention discloses a method for simultaneously detecting 14 sour components in main stream smoke obtained by heating noncombustible cigarettes. The method comprises following steps: 1) gathering main stream smoke particulate substances obtained by heating the noncombustible cigarettes by using a Cambridge filter piece, installing the Cambridge filter piece in an extraction device, adding an acetone solution, adding an inner standard solution, performing vibration extraction, adding a derivatization reagent into supernate, and heating to obtain smoke samples; 2) detecting the smoke samples by GC-MS, and detecting the contents of the 14 sour components in the main stream smoke obtained by heating the noncombustible cigarettes by using an inter-standard quantitative method. The method adopts a solvent extraction-gas chromatographic mass spectrometry and can be used for simultaneously detecting the contents of the 14 sour components in the main stream smoke obtained by heating the noncombustible cigarettes. The method has the advantages of being fast in detection, good in selectivity, and high in precision, and is particularly suitable for detecting the contents of the sour components in the smoke obtained by heating the noncombustible cigarettes.

The invention relates to a method for homogeneously derivatizing a plant fiber raw material by taking an ionic liquid as a medium. The method comprises the following steps of: (1) adding the plant fiber raw material into the ionic liquid; (2) dissolving at the temperature of 80-140 DEG C for 0.5-48 hours to obtain a reaction mixed solution; (3) leaching and separating the reaction mixed solution with a stainless steel filer screen; (4) adding a derivatization reagent into a filtrate, and undergoing an acylation reaction at the temperature of 70-130 DEG C for 1-10 hours; (5) after reacting, adding a precipitant into the mixed solution to separate a product out, filtering and drying to obtain a plant fiber derivatized product; and (6) distilling the filtrate under reducing pressure and recovering to obtain the ionic liquid. The method disclosed by the invention is simple and practicable, and the obtained plant fiber has a high derivatization degree.

The invention relates to a method for detecting the content of an etimicin sulfate raw material and preparation of the etimicin sulfate raw material and relevant substances. The method adopts precolumn derivatization, the derivatization condition comprises taking 4ml sample with appropriate concentration, adding 1ml O phthalic aldehyde (OPA) solution into the sample, diluting the mixed solution with isopropyl alcohol to 10ml, heating the mixed solution at 30-60 DEG C in water bath away from light, and obtaining derivatization solution. The novel method for detecting etimicin sulfate adopts a high efficiency liquid chromatograph, the chromatographic condition is that an octadecylsilane chemically bonded silica filler chromatographic column has particle size ranging from 4-10mum, column specification is 150-250mmX4.6-8.0mm; flowing phase is divided into organic phase and aqueous phase, wherein the volume rate of the organic phase to the aqueous phase is 55-75:45-25, the organic phase is methyl alcohol or acetonitrile, the aqueous phase is glacial acetic acid containing 0.01M-0.03M ion pair reagent sodium heptanesulfonate, potential of hydrogen (PH) range is adjusted by ammonia water or ammonium acetate; flow speed is 0.5-1.0ml / min; sample feeding amount is 10-20mul; a detector is a conventional ultraviolet-visible light detector, and detection wavelength is from 330-350nm. The novel method for detecting etimicin sulfate adopts the conventional detector and the high efficiency liquid chromatograph, can achieve on-line detection of the content of the etimicin sulfate, the preparation of the etimicin sulfate and the relevant substances, and is simple, convenient, feasible, accurate and reliable.

The invention belongs to the technical field of drug detection, and specifically discloses a method for detecting hydrazine hydrate in drugs. The detection method provided by the invention has excellent linearity, detection limit, specificity and accuracy, good applicability and reliability of the method, and meets the regulations for drug detection; and the appropriate amount and reaction conditions of the derivatization reagent have been tested, which improves the derivatization The conversion efficiency and the stability of derivative products were determined; the parameters of liquid phase and mass spectrometry conditions were determined, and the detection sensitivity of derivative products and the resolution of interference peaks were improved.

The invention relates to the field of analytical chemistry, and particularly relates to a detection and analysis method for hydroxy-containing cholesterol and metabolites thereof. The method includessubjecting hydroxy-containing cholesterol and metabolites thereof to stable isotope labeling derivatization with a derivatization agent that is d<0>- / d<3>-3-N-methyl-2'-carboxyrhodamine 6G; and aftera derivatization product obtained by magnetic dispersive solid-phase extraction is filtered by a filter membrane, detecting with an ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry analysis system. The stable isotope labeling derivatization agent that is the d<0>- / d<3>-MCR6G with permanent positive charges is utilized to label the hydroxy-containing cholesterol and metabolites thereof in a biological sample, and derivatization is mild in condition, rapid and high in efficiency. A magnetic dispersive solid-phase extraction technique is utilized, thus increasing the extraction efficiency, reducing sample pretreatment time, significantly increasing the degree of chromatographic separation and the mass spectrum ionization efficiency of analytes and reducing matrix interferences.

The invention provides a miniature light derivatizer for aflatoxin and sulfa drugs. It includes a UV LED light source, the excitation wavelength of which is between 280 and 370nm, and uses a thin inner diameter tube transparent to ultraviolet light as the derivation reaction pool. The diameter is 0.10-0.35 mm, the length is 17-30 cm, and the volume of the derivation pool is 7-15 μL. The optical derivatizer of the present invention increases the fluorescence intensity of aflatoxin B1 by 5 times; the derivatizer is used for liquid chromatography post-column derivatization and flow injection analysis derivatization needs, including high performance liquid chromatography (HPLC) and ultra-high pressure liquid Trace aflatoxins and sulfonamides in samples were analyzed by UPLC.

The invention discloses an aflatoxin fluorescence detector integrated with a chip-type light derivatizer, which integrates the light derivatizer and the fluorescence detector, and the chip-type derivatization reaction pool is also a fluorescence detection pool. The light derivation cell and the fluorescence detection cell are implemented on a chip of UV-transparent material. The high-power ultraviolet LED used is used as a light derivative light source and a fluorescence excitation light source at the same time. The LED is perpendicular to the light derivation cell / detection cell, and the included angle between the photoelectric detection device and the LED is 20-70°. When the invented chip light derivatizer has a cell volume of 7.5 μL, its derivatization efficiency is close to that of the traditional light derivatizer with a cell volume of 1000 μL. The invention not only greatly reduces the post-column volume after chromatographic column separation, significantly reduces peak broadening, improves resolution, and lowers the lower limit of detection, but also improves the overall performance and reliability of the instrument, and at the same time greatly reduces the volume and cost of the instrument.

The invention discloses a method for rapid quantitative analysis of 48 kinds of amino acids. The invention provides a derivatization reagent combination for quantitative analysis and detection of amino acid content by a derivatization HPLC-MS / MS method, including a derivatization reagent A and a derivatization reagent B; wherein, the derivatization reagent A is n-propanol and 3-methanol The mixed solution of base pyridine, the mixed solution of dichloromethane, chloroformyl propyl ester and isooctane as the derivatization reagent B. And further established the stable isotope internal standard combination, sample pretreatment method and liquid chromatography-tandem mass spectrometry method based on the derivatization method. The derivatization reagent proposed by the present invention has high derivatization efficiency and low reagent toxicity; the method requires less sample volume, simple, fast, good repeatability, and low detection cost; and the absolute quantitative analysis of 48 amino acids is realized in only 22 minutes , which greatly shortens the analysis time and improves the detection throughput; it has great popularization and application value.