330 results about "Derivatization" patented technology

The invention relates to the technical field of medicine analysis and detection, and particularly discloses a method for detecting the content of protein in a 3D-MLA adjuvant, which comprises the following steps: (1) preparing a test solution: firstly dissolving the 3D-MLA adjuvant by using a hydrochloric acid solution, performing 300-600W ultrasonic treatment for 2-5min, centrifuging 10000-13000g for 4-7min, and taking supernate; adding a compound enzyme into the supernate for enzymolysis; then adding concentrated hydrochloric acid, uniformly mixing, hydrolyzing for 20 + / -2 hours in a nitrogen atmosphere at 105-115 DEG C, blow-drying, and dissolving with a hydrochloric acid solution to obtain a test sample stock solution; adding a derivatization reagent into the test sample stock solution, and carrying out derivatization treatment, extraction and dilution to obtain a test sample solution; and (2) high performance liquid chromatography determination. According to the detection method provided by the invention, the residual quantity of the host cell protein in the 3D-MLA can be rapidly and accurately determined, and the quality control of the 3D-MLA is realized.

The invention provides a method for detecting free amino acids in camellia oleosa seed oil, and establishes a method for detecting the free amino acids in the camellia oleosa seed oil based on ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS), which comprises the following steps: pre-treating various amino acids in the camellia oleosa seed oil by using a non-derivation method; the problems of complicated operation, impurity interference and the like caused by derivatization are avoided, the extraction solvent is environment-friendly and economical, the extraction efficiency is high, and the pretreatment time is greatly shortened; then selecting a proper chromatographic column and a mobile phase, separating a plurality of free amino acids under the condition of not introducing excessive derivatization agents and ion pair reagents, and controlling the collection time to be 12 minutes. The method for detecting the free amino acids in the camellia oleosa seed oil has the characteristics of no need of derivatization treatment, simplicity and convenience in operation, high detection efficiency and good sensitivity and accuracy, and can effectively separate and detect 14 free amino acids such as alanine, phenylalanine and aspartic acid in the camellia oleosa seed oil.

The invention provides a method for detecting the hydroxyl value of a polyether material. The method comprises the following steps: (1) constructing a standard quantitative system of a derivatization reagent; (2) fully reacting a to-be-detected polyether material with the excessive derivatization reagent; (3) testing the peak area of the unreacted derivatization reagent by adopting chromatography; (4) comparing with a standard quantitative system of the derivatization reagent, and calculating the content of the unreacted derivatization reagent; and (5) calculating the consumption of the derivatization reagent in the step (2) by using the calculated content of the unreacted derivatization reagent, thereby calculating the hydroxyl value of the polyether material according to the stoichiometric relationship. Wherein the derivatization reagent comprises at least one hydroxyl esterifying agent selected from the following groups: phthalic anhydride, acetic anhydride and benzoyl chloride.

The invention provides a capillary electrophoresis analysis method of serum amino acid. The capillary electrophoresis analysis method comprises the following steps: S1, preparing an operation buffer solution; s2, selection and pretreatment of a quartz capillary column; s3, conditions are analyzed through electrophoresis; s4, drawing a quasi curve; s5, sample derivatization; s6, quantitative analysis. According to the method, a mixed reagent of alpha-cyclodextrin, beta-cyclodextrin and gamma-cyclodextrin is adopted for the first time, the amino acid migration behavior is cooperatively adjusted, a migration time window is expanded, the separation resolution of amino acids with similar structures is effectively improved, and the separation degree and the atlas definition are remarkably improved. According to the invention, sodium taurocholate is added, pH is regulated and controlled, a weakly alkaline buffer system with moderate conductivity and stable migration behavior is formed, separation and detection of FITC derived amino acids are facilitated, and balance of migration time distribution is optimized. The method is suitable for scenes of clinical sample analysis, disease marker screening and the like, and has good universality, stability and popularization value.

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 provides a method for detecting the contents of collagen and regenerated silk fibroin in a composite material, which comprises the following steps: (1) hydrolyzing the composite material for a certain time, and neutralizing to obtain a solution to be detected; (2) preparing a tyrosine reference solution; and (3) detecting the peak areas of the solution to be detected and the tyrosine reference substance solution by adopting high performance liquid chromatography, and calculating to obtain the content of regenerated silk fibroin in the composite material, and (4) detecting the total nitrogen content of the composite material by using a Kjeldahl method, and calculating to obtain the collagen content in the composite material. According to the method, the high performance liquid chromatography is combined with the Kjeldahl determination method, accurate determination of two components can be realized without derivatization treatment, the operation is simple and convenient, and the detection cost is low; the limit of quantitation of the method reaches 10.35 mu g / mL (S / N is greater than or equal to 16.59), the precision RSD is less than 1%, and the method has high sensitivity and accuracy.

The invention belongs to the field of chemical detection, and particularly relates to a method for detecting ethylene oxide, 2-chloroethanol and acetaldehyde in a frozen beverage by solid-phase microextraction gas chromatography-mass spectrometry. The invention relates to a method for detecting ethylene oxide, 2-chloroethanol and acetaldehyde in a frozen beverage by solid-phase microextraction gas chromatography-mass spectrometry, which comprises the following steps: S.1) taking a frozen beverage sample to be detected, homogenizing and uniformly mixing; s.2) weighing a certain amount of sample, and adding sodium chloride and hydrochloric acid; s.3) determining the sample by adopting a solid-phase microextraction gas chromatography-mass spectrometry method; and S.4) quantitatively analyzing the contents of ethylene oxide, 2-chloroethanol and acetaldehyde in the frozen drink sample to be detected by adopting an external standard method. According to the method disclosed by the invention, the derivatization reaction and the solid-phase microextraction process are combined into one, and the difficulties of complicated pretreatment, long time consumption, low accuracy, unstable result, high detection limit and the like in the traditional analysis technology are overcome. Meanwhile, the precision of a detection result is high, the influence of a complex matrix is removed, and the reproducibility is good.

The invention provides a method for detecting trace dimethyl sulfate in nicergoline, which comprises the following steps of: carrying out derivatization reaction on an azacyclo-compound serving as a derivatization agent and dimethyl sulfate in nicergoline to generate a derivatization product, and determining the amount of the derivatization product by using a high performance liquid chromatograph-mass spectrometer, therefore, the content of dimethyl sulfate in nicergoline is obtained. Compared with the prior art, the detection method provided by the invention has the characteristics of good specificity, high sensitivity, good reproducibility and the like, and makes up the vacancy of how to detect trace dimethyl sulfate in nicergoline in the prior art.

The invention provides a method for detecting taurine in magnesium acetyltaurate, which comprises the following steps: (1) derivatization treatment: carrying out derivatization reaction on a derivatization reagent and magnesium acetyltaurate containing taurine under an alkaline condition to obtain a derivatization product; (2) detection: detecting the derivatization product in the step (1) by adopting a high performance liquid chromatography-ultraviolet detector; wherein the derivatization reagent is selected from the group consisting of 2, 4-dinitrofluorobenzyl cyanide. The determination method has the advantages of high sensitivity, good specificity, simple operation, high accuracy, good reproducibility, good stability and low cost, improves the quality standard of taurine detection in magnesium acetyltaurate, can strictly control the quality of taurine in magnesium acetyltaurate, ensures the safety and reliability of magnesium acetyltaurate, and has a wide application prospect. The practical significance is realized.

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 present invention discloses an efficient C-H arylation reaction between quinoxalinone compounds and aryltriazenes induced by ionic liquids. Specifically, it relates to a method for the electrochemical synthesis of 3-arylquinoxalinone compounds, using aryltriazenes as stable arylation reagents and ionic liquids as promoters and electrolytes. Under mild, metal-free, and oxidant-free conditions, the method can synthesize a variety of 3-arylquinoxalinone compounds and arylated quinoxaline compounds in moderate to excellent yields. This scheme has the remarkable characteristics of simple operation, excellent functional group tolerance, high selectivity, strong product derivatization, and suitability for gram-scale continuous flow chemical synthesis.

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 invention discloses an in-situ derivatization mass spectrometry imaging method, which belongs to the technical field of mass spectrometry imaging detection, and comprises the following steps: preparing a sample slice and attaching the sample slice to a conductive glass slide; the method comprises the following steps: dissolving a derivatization reagent and a catalyst in a volatile organic solvent to prepare a derivatization reagent system solution, and spraying the derivatization reagent system solution on the surface of the tissue slice for derivatization reaction; coating a matrix on the surface of the derivatization slice, and identifying and analyzing by using an MALDI-MSI method; the structure of the derivatization reagent is shown in the specification. The derivatization reagent can perform mild and rapid in-situ derivatization on trace carbonyl-containing compounds in biological tissues, significantly improve the mass spectrum signal response of target compound molecules and significantly inhibit the delocalization (diffusion) phenomenon of analytes, and the MALDI-MSI technology is adopted to analyze the derivatized tissue slices. High-spatial-resolution in-situ visualization characterization of trace carbonyl-containing compounds in biological tissue slices is realized, and the problems in the prior art are effectively solved.

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 invention belongs to the technical field of analytical chemistry, and particularly relates to a multifunctional chiral selection reagent solution (CSS) and application of the multifunctional chiral selection reagent solution. More specifically, the invention relates to a multifunctional chiral selection reagent solution for chiralMS (chiralMS) analysis, and the solution is prepared from CuCl2, D-Phe, L-Ph-d5 and D-or L-3'and / or 4 'hydroxyl substituted Kelin lactone. According to the present invention, the on-line non-covalent derivatization can be performed on the enantiomers in the complex system sample by using the multifunctional chiral selection reagent solution and by using the post-column injection liquid chromatography-mass spectrometry (post-column injection liquid chromatography-mass spectrometry / MS, PCI-LC-MS / MS) system so as to achieve the qualitative and quantitative analysis of the enantiomers and the rapid screening of the chiral selection reagent (CS).

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 relates to the technical field of chiral stationary phase fillers, in particular to an underived beta-cyclodextrin chiral stationary phase as well as a preparation method and application thereof. Underived beta-cyclodextrin is bonded on the surface of silica gel through urea or thiourea groups respectively, and the structure is shown as a formula I in the specification. The preparation process of the underived beta-cyclodextrin chiral stationary phase filler provided by the invention has the advantages of simple and easily-controlled conditions, no need of complex derivatization and good repeatability. The novel chiral stationary phase is suitable for different mobile phase systems of high performance liquid chromatography, can efficiently separate N-containing chiral compounds such as imidazole antibacterial drugs and triazole pesticides in various structure types, and can meet the requirements of daily analysis, production process and use process quality control and the like of the chiral drugs and the chiral pesticides.

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 present invention relates to a hollow nanocage structured silver-doped nickel cobaltate / nickel oxide gas-sensitive material, and its preparation method and application. The method uses dimethyl imidazole cobalt as a structure-directing agent, combined with a nickel-cobalt layered double hydroxide derivatization method and a chemical reduction method, to simultaneously achieve triple optimization of the material's microstructure, interface energy band gap, and composition. The unique hollow nanocage structure of the prepared composite material greatly increases its contact area with the gas being detected; the interface heterojunction formed by nickel cobaltate and nickel oxide in the material accelerates the efficiency of interfacial electron transmission; and silver doping increases the number of electron transitions during the detection process. Gas-sensing experiments have shown that the composite material has high selectivity, sensitivity, and stability for the volatile organic gas n-butanol at a relatively low operating temperature, and is suitable for the detection of trace n-butanol in complex environments. The preparation method has mild conditions, low cost, and good industrialization prospects, and has broad application prospects in the field of gas-sensitive material preparation.

Disclosed are 1,5,6-polysubstituted-2-oxo-3-oxabicyclo[3.1.0]hexane and a preparation method thereof. The reaction process comprises the following steps: using α-substituted allyl acetate as a raw material under the action of an inexpensive metal catalyst, the acetic acid acrylate structure contains a cyclopropane-γ-lactone structure, and the substituent types are diverse, making it easy to perform subsequent derivatization modification. The target product is prepared efficiently and with high non-corresponding selectivity through a one-pot process. The method has the advantages of simple and readily available raw materials, mild reaction conditions, simple operation, wide substrate universality, easy large-scale production, no safety hazards, and low cost, and can provide support for relevant drug activity testing.

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.