175 results about "Derivatization" patented technology

The invention provides a method for measuring gamma-aminobutyric acid in tableted candies, which comprises the following steps: measuring gamma-aminobutyric acid in tableted candies by using HPLC-ELSD (High Performance Liquid Chromatography-Evaporative Light Scattering Detector) according to a volume ratio of acetonitrile to water of (50-70): (30-50) as a mobile phase; a chromatographic column is an amino column; a detector is ELSD, the temperature of a drift tube is 80-85 DEG C, and carrier gas is air. The detection method disclosed by the invention is strong in specificity, high in accuracy, strong in stability, good in repeatability and high in sensitivity, and compared with an existing derivation method, the method disclosed by the invention is simple, green and efficient, and can be used for effectively detecting the content of gamma-aminobutyric acid in the tabletted candies.

The invention relates to the field of detection, in particular to a method for simultaneously detecting multiple fat-soluble vitamins, which comprises the following steps: (S.1) carrying out protein precipitation and liquid-liquid extraction on a sample to be detected to obtain an extract containing fat-soluble vitamins; (S.2) carrying out derivatization reaction on the extract by using a PTAD derivatization reagent; and (S.3) analyzing the derivatized product by adopting a liquid chromatography-tandem mass spectrometry method, wherein the detected target fat-soluble vitamins comprise vitamin A, vitamin E, 25-hydroxy vitamin D2, 25-hydroxy vitamin D3, vitamin K1, vitamin K2 and vitamin K2. According to the application, PTAD is creatively adopted as a unified derivatization reagent, simultaneous and efficient derivatization of seven fat-soluble vitamins is successfully realized, the detection sensitivity of low-content targets, especially vitamin D, K2 and the like, is greatly improved, and the core problems of weak signal response and difficulty in accurate quantification are solved.

The application relates to the technical field of free radical detection, in particular to a high-sensitivity in-situ capture and detection method of organic free radicals based on a DIPPMPO probe and application, and the method comprises the following steps: adding a chemical probe DIPPMPO into a reaction system containing potential organic free radical precursors, so that the DIPPMPO and organic free radicals generated in a reaction process occur adduct reaction to form a DIPPMPO-free radical adduct which can be detected under liquid chromatography-mass spectrometry conditions; performing high performance liquid chromatography-quadrupole-time of flight mass spectrometry analysis on a mixed solution after the adduct reaction is completed, so that first mass spectrometry data and secondary mass spectrometry fragment information of the DIPPMPO-free radical adduct are obtained; and automatically processing the secondary mass spectrometry data, screening out parent ions with continuous neutral loss as potential DIPPMPO-free radical adduct candidate signals. The application does not need derivatization, is simple to operate, is broad-spectrum and high-efficiency, and can be applied to environmental water samples, biological fluids, chemical reaction liquids or drug metabolism systems.

The invention discloses a detection method of vitamin K1, and belongs to the technical field of biological detection. The problems that a vitamin K1 detection method is tedious in operation, prone to being influenced by a matrix, low in sensitivity and the like are solved. The detection method comprises the following steps: (1) preparing a standard substance intermediate working solution, an isotope internal standard substance solution and a standard curve working solution of the vitamin K1; (2) treating a serum sample and a standard curve working solution: adding a 2-nitroso pyridine solution to carry out derivatization reaction; and (3) detecting the vitamin K1 by using a high performance liquid chromatography-tandem mass spectrometry method. According to the method, the 2-nitroso pyridine is used as a derivatization reagent, the vitamin K1 and the 2-nitroso pyridine are subjected to a Diels-Alder reaction to generate a new six-membered heterocycle containing N and O, the 2-nitroso pyridine can efficiently and completely react with the vitamin K1 in only 10 minutes at room temperature, the detection steps are simplified, the sample pretreatment time is shortened, and the detection efficiency is improved.

This application provides a method for simultaneously detecting hydroxy acids and keto acids in a sample. The method includes the following steps: preparing a standard solution; performing ketone and carboxyl derivatization on the sample to be tested containing hydroxy acids and keto acids to obtain the sample to be tested; performing ketone and carboxyl derivatization on the standard solution to obtain a derivatized standard solution; and sequentially adding a ketone derivatization reagent and... 13 The method involves derivatization with a C6-labeled carboxyl derivatization reagent to obtain an isotope internal standard solution. This solution is then added to both the sample to be tested and the derivatized standard solution for LC-MS / MS analysis. The method described in this application achieves unified detection of paired hydroxy acids and keto acids by selectively derivatizing the ketone group followed by the carboxyl group. A sequential derivatization strategy is constructed based on the functional group differences between keto and hydroxy acids, significantly improving the stability, repeatability, and quantitative reliability of keto acid detection while enhancing overall detection sensitivity.

The invention discloses a high performance liquid chromatography analysis method for trace impurity content in an organic amine catalyst, and relates to the field of organic catalyst content analysis. Comprising the following steps: pretreating an organic amine catalyst sample, preparing a urea standard solution, performing HPLC (High Performance Liquid Chromatography) analysis and performing quantitative analysis by an external standard method, namely performing derivatization reaction on urea and benzaldehyde under an acidic condition, and successfully converting urea without ultraviolet absorption into dibenzylidene urea (DBU) with strong ultraviolet absorption, the technical blank of direct detection of urea is effectively filled, and the method is adaptive to a conventional ultraviolet / visible light detector to realize accurate detection. And the method has relatively high practical popularization and application values. The method has the advantages of being good in separation effect, high in sensitivity, easy and convenient to operate, high in reproducibility and the like, and can be widely applied to qualitative and quantitative analysis of various trace impurities in the organic amine catalyst.

The invention discloses a chiral 1, 4-diazabicyclo [3.1. 1] heptane derivative as well as a synthesis method and application of the chiral 1, 4-diazabicyclo [3.1. 1] heptane derivative. According to the invention, a 1-azabicyclo [1.1. 0] butane derivative is taken as a raw material, under the catalytic action of a chiral iridium complex, the 1-azabicyclo [1.1. 1] butane derivative and an N-allyl carbonate derivative are subjected to [3 + 2] cycloaddition reaction, a series of chiral 1, 4-diazabicyclo [3.1. 1] heptane skeletons with diversified structures are constructed with high stereoselectivity, and the obtained product has the potential of further derivatization. The method has the advantages of easily available raw materials, mild reaction conditions, simplicity and convenience in operation, good functional group compatibility and the like.

The application discloses a hydroxylamine hydrochloride detection method in azithromycin dry suspension, and relates to the trace detection field. The method uses isoamyl aldehyde as a derivatizing agent, generates isoamyl aldoxime by performing derivatization treatment on a sample to be measured, and then uses N-nitrosodiisopropylamine as an internal standard substance to quantitatively determine the isoamyl aldoxime by using liquid chromatography-tandem mass spectrometry. The detection method adopts an isoamyl aldehyde derivatizing agent-N-nitrosodiisopropylamine internal standard substance system, can correct detection errors caused by factors such as matrix effect, pretreatment loss and derivatization efficiency fluctuation, and improves the accuracy and sensitivity of the trace hydroxylamine hydrochloride detection result, thereby guaranteeing the safety of the medicine.

The application discloses a compound, a preparation method and a use for preparing a derivatization reagent, and belongs to the field of chemistry. The application claims a compound TMT-mAla-PP with a novel chemical structure and a preparation method and a use thereof. Compared with the same compound TMT-PP or TMT-Pro-PP in the prior art, the derivatization product obtained by using the TMT-mAla-PP provided by the application as a derivatization reagent for performing a derivatization reaction on a bile acid compound has a significantly better mass spectrometry response sensitivity. Therefore, the compound provided by the application can be used for preparing a derivatization reagent for a bile acid compound, and the derivatization reagent can perform derivatization modification on the bile acid compound before mass spectrometry detection of the bile acid compound, so that the detection performance of the mass spectrometry on the bile acid compound is significantly improved.

The application discloses a kind of 10 kinds of antioxidants in medical device leachable determination method.The present application, by ultra-high performance liquid chromatography time-of-flight mass spectrometry technology realizes the simultaneous determination of ten kinds of antioxidants in medical device leachable, covers different types of antioxidants such as phenolic and phosphite.The pretreatment process only needs to extract the measured product, and the extracted liquid is blown dry by nitrogen, methanol is added, vortexed and filtered through microporous filter to complete the preparation of test solution, and the operation steps are simple, without complex derivatization or purification process, greatly reducing the difficulty and time cost of sample processing.In the analysis process, the ultra-high performance liquid chromatography system is used in conjunction with specific chromatographic column and mobile phase gradient elution program, which can quickly realize the baseline separation of ten kinds of antioxidants, combined with the high sensitivity detection of time-of-flight mass spectrometry, significantly improves the analysis efficiency, and is suitable for rapid screening and quantitative analysis of large quantities of samples.

A method for measuring the content of hydrazine in a carbidopa-containing drug, comprising the following steps: (1) in a solvent, under the action of acid, mixing a sample under test with an aldehydes substance, said sample being a carbidopa-containing drug, and hydrazine in said sample and the aldehydes substance being derivatized to obtain a test solution; and (2) measuring the content of the hydrazine in the test solution. Compared with the prior art, the method for measuring the content of hydrazine in a carbidopa-containing drug does not require pretreatment to remove carbidopa, introduces negligible hydrazine during measurement, is easy to operate, does not need to accurately control derivatization time and sample introduction time, and exhibits good repeatability and accurate measurements.

The invention relates to a detection method, in particular to a method for detecting aldehyde impurities in polysorbate 20. According to the method, interference caused by the purity of 2, 4-dinitrophenylhydrazine is avoided, derivatization of a reference substance is performed by adopting a method synchronously operating with a test sample, eight aldehyde ketone substances can be detected at the same time, and compared with literature methods, the method is high in specificity, good in precision, high in accuracy, simple and easy to implement and high in operability.

The invention discloses a construction method and application of a polysaccharide mass spectrum fingerprint spectrum. The method comprises the following steps: mixing a polysaccharide standard substance with a methylation reagent, directly introducing the mixture into an in-situ ionization source for direct ionization, and carrying out tandem mass spectrometry to obtain a mass spectrum fingerprint spectrum of the polysaccharide; a sample to be tested is subjected to the same testing process to obtain a mass spectrum fingerprint spectrum of the sample to be tested, the monosaccharide unit type of the polysaccharide is rapidly judged by analyzing the mass difference of characteristic continuous neutral loss in the spectrum, and accurate identification of the polysaccharide type is achieved by utilizing characteristic precursor ions and diagnostic fragment ions thereof. The method realizes direct and rapid analysis of complete polysaccharides, does not need tedious hydrolysis, derivatization and chromatographic separation steps, can effectively distinguish isomeric polysaccharides with different structures, and provides a novel high-throughput and high-discriminability analysis method for polysaccharide components in food, plant and biological samples.

The application discloses a separation and detection method of methoxy PEG derivatives and methylsulfonyl PEG derivatives, which comprises the following steps: mixing a sample to be detected, ammonia and an ammonium salt catalyst, carrying out a derivatization reaction to obtain a derivative product, and detecting the derivative product by using a liquid chromatography method. The sample to be detected is a methoxy PEG derivative or a methylsulfonyl PEG derivative sample. In the method, the stationary phase of the chromatographic column is octadecylsilane bonded silica gel, the mobile phase A is a 0.01-5% formic acid aqueous solution in terms of volume percentage concentration, the mobile phase B is acetonitrile and methanol in a volume ratio of (1-5):1, a gradient elution program is adopted, and an electrospray detector is used. The method can effectively separate and quantitatively analyze the methoxy PEG derivatives and the methylsulfonyl PEG derivatives, and the method is completely in line with the standards and performs well in the quantitative limit, the linear range, the accuracy and the like, thereby providing an effective guarantee for subsequent product quality control or evaluation.

A method for processing a metabolite before analysis, the method comprising: a step for supplying a sample to be analyzed to a porous support and holding a metabolite contained in the sample to be analyzed on the porous support; and a step of supplying a vaporized derivatization reagent to the porous support holding the metabolite to derivatize the metabolite.

The invention provides a method for simultaneously detecting dichloroacetic acid and trichloroacetic acid in urine, and belongs to the technical field of analysis detection and occupational health / environmental health. According to the method disclosed by the invention, a synergistic pretreatment strategy of acidic sample loading, WAX / reversed-phase mixed mode solid-phase extraction, water / low-proportion organic phase step-by-step leaching and ammonia-water-containing organic phase elution is adopted; a technical route of protein precipitation, acidification pH regulation, purification and enrichment by adopting WAX / reversed-phase mixed mode solid-phase extraction on a 96-well plate and stable isotope internal standard isotope dilution LC-MS / MS quantification is adopted, the method can effectively reduce the matrix effect and realize high-throughput analysis in a high-salinity urine matrix, the quantitation limits of DCEA and TCAA are not higher than 0.30 g / L and 0.20 g / L respectively, and the method has the advantages that the method is simple and convenient to operate, and the method is suitable for large-scale popularization and application. The method is suitable for biological monitoring and risk assessment of occupational and environmental low-level exposure crowds.

The invention discloses a high-efficiency separation method of breast milk oligosaccharide and application of the breast milk oligosaccharide in specific recognition of influenza A virus hemagglutinin protein.The method comprises the steps that a DE-52 weak anion exchange column, a graphite carbon column and Bio-GelP10 column chromatography are combined for use, breast milk oligosaccharide components with low abundance and high molecular weight are efficiently enriched, and the specific recognition of influenza A virus hemagglutinin protein is achieved; after derivatization labeling of a bifunctional reagent 2-amino-N-(2-aminoethyl) benzamide (AEAB), 56 breast milk oligosaccharide monomers with the purity higher than 90% are separated from the isomer level through one-dimensional amide normal phase chromatography and two-dimensional C18 reverse phase circulation chromatography, and a monomer substance library is constructed. AEAB is used as a connecting arm to construct a breast milk oligosaccharide chip, an active monomer DSLNT II which is specifically combined with four subtype influenza A virus hemagglutinin proteins is screened out in a high-throughput manner, and fine structure analysis is completed in combination with electrospray tandem mass spectrometry. According to the method, the large-scale preparation of the low-abundance breast milk oligosaccharide monomer is realized, and a key material basis and theoretical guidance are provided for researching an antiviral mechanism and developing related functional foods and medicines.

The invention relates to the technical field of petrochemical engineering analysis, and provides a form analysis method and system for sulfides in a sulfuric acid alkylation working solution, and the analysis method comprises the following steps: S1, sample collection and pretreatment; s2, carrying out derivatization reaction; s3, separating and detecting; s4, data processing and analysis; the system comprises a sample pretreatment module, a derivatization reaction module, a separation detection module and a data processing and analysis module, and the analysis method provided by the invention can accurately and quickly analyze the forms and contents of various sulfides in the working solution, is high in sensitivity and accuracy, simple, convenient and quick to operate, has good universality and expansibility, and can be widely applied to industrial production. The method is suitable for qualitative and quantitative analysis of various sulfide forms in the field of petrochemical engineering, and has important industrial application value.

The invention discloses a C, N-FeNbO4 / NF microrod based on foamed nickel in-situ 001 crystal face derivation and a derivation method and application thereof, and the method comprises the following steps: in a hydrothermal reaction, hydrolyzing urea to release OH-to replace oxalate in niobium oxalate so as to form a Nb-OH monomer; meanwhile, Fe < 3 + > is hydrolyzed into Fe (OH) 3 colloid; the preparation method comprises the following steps: performing liquid phase nucleation on Nb-OH and Fe (OH) 3 under a hydrothermal condition to form a FeNbO4 precursor, and growing the FeNbO4 precursor on foamed nickel (NF) in situ; in this way, the 001 crystal face of FeNbO4 is accurately regulated and controlled through the strong coordination effect of F <-> to form a rod structure. Under high-temperature (900 DEG C) carbonization, the FeNbO4 is further crystallized into an acid-resistant and alkali-resistant monoclinic crystal type three-dimensional microrod (C, N-FeNbO4 / NF) with C and N co-doped (C, N-FeNbO4) composite NF. According to the method disclosed by the invention, the agglomeration phenomenon of FeNbO4 is relieved; the microrod structure exposes more catalytic active sites, so that the catalytic activity is improved. In addition, the catalyst shows high conductivity by co-doping C and N with synergistic high-conductivity NF. Based on the regulation and control, the C, N-FeNbO4 / NF shows good electrochemical performance in the oxygen evolution reaction.

The invention discloses a method for analyzing a polymeric lignin structural unit in watermelon peel, and belongs to the technical field of biological substance composition determination methods, the method comprises the following steps: S1, protective pretreatment: mixing a watermelon peel sample with a protective solution containing triphenylmethyl mercaptan; s2, thioacidolysis: adding a reaction solution containing boron trifluoride and ethanethiol, and heating for depolymerization; s3, in-situ neutralization and derivatization: adding a buffer solution, extracting and drying to obtain an organic phase, and then adding a silanization reagent for derivatization reaction; s4, qualitative and quantitative analysis; through the multi-level design of structure protection, efficient derivation and system integration, the established analysis method shows remarkable advantages in the aspects of inhibiting condensation reaction, improving operation safety, shortening analysis period and realizing quantification, effectively overcomes the technical bottlenecks of low recovery rate, high toxicity, long time consumption, incomplete detection and the like in the prior art, and has wide application prospects. And an excellent technical scheme is provided for composition analysis of the plant polymerized lignin.

The invention relates to a method for simultaneously detecting various steroid hormones in serum, which comprises the following steps: extracting hormones in serum by a liquid-liquid extraction method; a derivatization reagent is added into the extracted hormone, an oximation reaction is carried out, and the derivatization reagent comprises quaternary ammonium oxygen amine; the hormone after oximation reaction is injected into a two-dimensional liquid chromatography-tandem mass spectrometry system for detection, the hormone is enriched on a one-dimensional chromatographic column, and then the enriched hormone is subjected to back flushing and transferred to a two-dimensional chromatographic column for analysis. According to the method, the backwashing transfer two-dimensional liquid chromatography-tandem mass spectrometry and the derivatization reaction are combined, various steroid hormones including progestational hormone and androgen can be detected at the same time, and the method has the advantage of being high in detection sensitivity.

The invention relates to a method for detecting various free androgens in serum, which comprises the following steps: carrying out ultrafiltration treatment on a sample to obtain an ultrafiltration solution; magnetic beads are added into the ultrafiltration solution, and androgen is extracted through magnetic solid-phase extraction; adding a derivatization reagent containing quaternary ammonium oxygen amine into the extracted androgen, and carrying out oximation reaction; and injecting the solution after oximation reaction into a high performance liquid chromatography-tandem mass spectrometry system for detection. The method provided by the invention has excellent specificity and sensitivity, the linear fitting correlation coefficient (r) is greater than 0.99, the recovery rate of the extract is higher than 95.1%, the precision and accuracy measured by relative errors and variable coefficients both meet the regulations of the clinical and laboratory standard association (CLSI), and a stability test proves that under typical clinical treatment conditions, the analyte loss is extremely small.

The present application relates to the technical field of nitrofurans metabolite content determination, and particularly relates to a method for determining the residual amount of nitrofurans metabolite in propolis. The method is that the pretreated propolis sample is detected by liquid chromatography-tandem mass spectrometry after gradient elution of the mobile phase; the pretreatment is that the propolis sample is sequentially hydrolyzed by hydrochloric acid, purified by HLB solid phase extraction column, derivatized by o-nitrobenzaldehyde, and purified by ethyl acetate treatment. The present application purifies the propolis sample after hydrochloric acid hydrolysis before o-nitrobenzaldehyde derivatization, so that o-nitrobenzaldehyde fully reacts with the nitrofurans metabolite in propolis, and the residual amount of nitrofurans metabolite in propolis is accurately detected by combining the selection and gradient elution of the mobile phase.

The application discloses a method for detecting enantiomers in (S)-(1-hydroxypropan-2-yl) tert-butyl carbamate by high performance liquid chromatography. Specifically, the test product is dissolved in a diluent, and detection is performed by using a high performance liquid chromatograph, wherein a CHIRALPAK IG is used as the chromatographic column, the specification of the chromatographic column is an inner diameter of 4.6 mm, a length of 250 mm, and a filler particle size of 5 microns; a mobile phase is water-acetonitrile-tetrahydrofuran, and the volume ratio is 900:75:25; and isocratic elution is adopted. The method is simple and rapid, does not need derivatization treatment, has high sensitivity, good sample solubility, and accurate results, and is suitable for quality control of (S)-(1-hydroxypropan-2-yl) tert-butyl carbamate.

This invention provides a method for detecting free fatty acids in human serum. The method comprises: adding multiple fatty acid standards and a condensing agent to a solvent to obtain a fatty acid solution with activated carboxyl groups; adding an isotopic compound to the fatty acid solution, where the carboxyl groups of the fatty acids undergo a condensation reaction with the amino groups of the isotopic compound to obtain a derivatized isotopic internal standard solution; adding the condensing agent and a non-isotopic compound of the same type as the isotopic compound to a serum sample, where the carboxyl groups of the fatty acids in the serum sample undergo a condensation reaction with the amino groups of the non-isotopic compound to obtain a reacted solution; adding the isotopic internal standard solution and sending the sample to a mass spectrometer for detection to obtain the fatty acid content in the serum sample. This invention has the advantages of low detection difficulty and high accuracy.

The application discloses a kind of soybean oligosaccharide content detection methods in food, the food is soy milk, the soybean oligosaccharide is stachyose, raffinose and sucrose.Method includes the following steps: (1) preparation standard stock solution and standard working solution;(2) preparation sample solution to be measured;(3) high performance liquid chromatography analysis condition;(4) establish standard working curve;(5) result analysis.The application establishes the high performance liquid chromatography determination method of low content level soybean oligosaccharide in soy milk.The application innovatively uses derivatization method to the soybean oligosaccharide (stachyose, raffinose and sucrose) and is derived, thereby greatly improves detection sensitivity, so that simple and easy to operate, without needing to carry out multiple large volume extraction solvent extraction and rotary evaporation concentration processing, and fills the blank of soybean oligosaccharide content detection field in soy milk.The method is simple in operation, high in sensitivity, good in reproducibility and stability, can satisfy the daily detection requirement of low content level soybean oligosaccharide in soy milk for inspection organization and enterprise internal laboratory.

The application discloses an enzyme method for synthesizing unnatural sugar and application thereof, and belongs to the technical field of organic chemical synthesis. The unnatural sugar comprises an unnatural sugar obtained by introducing an acyl group into a hydroxyl group at the 6th position of a bare sugar through an acylation reaction; and the bare sugar is obtained by performing derivatization modification on an amide site of a natural sugar. The synthesis method uses a SubC enzyme as a catalyst to realize selective acylation of the hydroxyl group at the 6th position of the bare sugar, and synthesizes the unnatural sugar with an ideal yield. The unnatural sugar can be applied to glycomics metabolic labeling and mass spectrometry analysis as a marker, has excellent biological safety, specificity and labeling efficiency, can avoid non-specific labeling, and has no obvious cytotoxicity.

The present invention discloses a detection and analysis method for complexing agents in a complex iron desulfurization solution. The complexing agents are ethylenediaminetetraacetic acid and nitrilotriacetic acid. The detection and analysis method includes: adding a reducing agent to a sample to be tested to reduce the Fe 3+ complex in the complex iron desulfurization solution into Fe 2+ complex, obtaining a sample solution to be tested; adding a nickel salt derivatization reagent and an ion pair reagent to the mobile phase of a high performance liquid chromatography, and adjusting the pH value of the mobile phase to 5.8 - 6.2; using the high performance liquid chromatography to detect and analyze the sample solution to be tested. The detection and analysis method of the present invention simplifies the pretreatment process, and the analysis result is accurate and reliable.