613 results about "Derivatization" patented technology

The invention relates to the field of establishment of fingerprints of traditional Chinese medicinal materials, in particular to an establishment method and application of a salvia miltiorrhiza polysaccharide HPLC (High Performance Liquid Chromatography) fingerprint. The establishment method comprises the following steps: preparation of a test solution: taking a salvia miltiorrhiza polysaccharide hydrolysis solution, carrying out derivatization in a reaction bottle, and passing through a 0.1-0.3 [mu] m microporous filter membrane; preparing a reference substance solution, namely weighing mannose, ribose, rhamnose, glucuronic acid, galacturonic acid, glucose, galactose and arabinose reference substances, and preparing into a mixed reference substance solution; performing HPLC (high performance liquid chromatography) determination; and establishing the salvia miltiorrhiza polysaccharide HPLC fingerprint spectrum. According to the method, the difference of monosaccharide composition and content in salvia miltiorrhiza medicinal materials from different producing areas and the spectrum-effect relationship between antioxidant activity and anticoagulant activity are clarified, and a certain reference basis is provided for quality control and evaluation of the salvia miltiorrhiza medicinal materials from the aspect of polysaccharide.

The invention relates to the technical field of chemical synthesis of dyes, in particular to a 5, 5 '-disubstituted amino-3, 3'-dipyridyl derivative as well as a preparation method and application of the 5, 5 '-disubstituted amino-3, 3'-dipyridyl derivative. According to the 5, 5 '-disubstituted amino-3, 3'-dipyridyl derivative and the preparation method thereof, the ornamental blue is used as a parent body for derivatization reaction, different structures are introduced to amino groups, the 5, 5 '-disubstituted amino-3, 3'-dipyridyl derivative is obtained and can be used as a dye, and the dye has relatively high color development intensity, bright color, deep dyeing and comprehensive color fastness. The preparation method of the 5, 5 '-disubstituted amino-3, 3'-dipyridyl derivative is continuous in process step, high in controllability, large in treatment capacity and suitable for large-scale industrial production, the 5, 5 '-disubstituted amino-3, 3'-dipyridyl derivative is applied to fabric dyeing, and the fabric has the advantages of washing resistance, acid resistance, sublimation resistance, wet friction resistance and the like.

The invention discloses a non-derivatization quantitative detection method for amino acid in a high-concentration protein preparation, which comprises the following steps: separating by using a graphitized carbon chromatographic column, adding an ion pair reagent trifluoroacetic acid into a mobile phase, and detecting by using an electric fog detector (CAD); the method comprises the following steps: preparing a plurality of groups of amino acid standard substance solutions with different concentration groups, wherein the concentration range is 1mmol / L-20mmol / L; drawing a quadratic equation standard curve of the amino acid standard product concentration and the peak area as a detection equation for detecting the amino acid concentration; the method comprises the following steps: diluting a test sample by using ultrapure water for multiple times, carrying out ultrafiltration centrifugal treatment, removing protein, introducing the sample, obtaining a corresponding peak area according to the spectrum integral of the test sample, and substituting the peak area into the detection equation to obtain the concentration of amino acid in the test sample. The method has the advantages of high detection precision, high detection efficiency and simple operation, and greatly reduces the adverse effect of high-concentration protein on the chromatographic column.

The invention discloses a method for detecting the hydrazine content in a medicine containing carbidopa. The invention provides a method for detecting hydrazine content in a medicine containing carbidopa, which comprises the following steps: (1) mixing a sample to be detected and an aldehyde substance in a solvent under the action of acid, deriving hydrazine in the sample to be detected and the aldehyde substance to obtain a test solution, and (2) detecting the content of hydrazine in the test solution. Compared with the prior art, the method has the advantages that the carbidopa does not need to be removed through pretreatment, hydrazine introduced in the determination process can be ignored, operation is simple, derivatization time and sample injection time do not need to be accurately controlled, repeatability is good, and quantification is accurate.

The invention discloses a method for detecting organic carbon components in soil based on gas chromatography-mass spectrometry, and particularly relates to the technical field of soil detection. The method comprises the following steps: pretreating fresh soil to obtain a fresh soil sample and an air-dried soil sample, respectively extracting organic carbon components to obtain a DOC extracting solution and an LOC extracting solution, and sequentially and respectively carrying out purification treatment, concentration treatment and derivatization on the DOC extracting solution and the LOC extracting solution to obtain a DOC to-be-detected solution and an LOC to-be-detected solution; respectively detecting the DOC to-be-detected liquid and the LOC to-be-detected liquid in a GC-MS instrument to obtain a total ion flow chromatogram, and carrying out qualitative and quantitative analysis to obtain organic carbon component data. Through step-by-step extraction, selective derivatization and GC-MS accurate analysis, molecular level separation, identification and quantification of water-soluble organic carbon DOC and oxidizable organic carbon LOC in soil are achieved, the method is particularly suitable for evaluating contribution of carbohydrate, amino acid and organic acid to the carbon turnover rate, and the method is good in selectivity and high in sensitivity.

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 discloses a derivatization device and a derivatization method for on-line production of a derivatization reagent, the device comprises a chemical column suppressor, a reaction reagent, a six-way valve, a derivatization reactor, a pump system and a flow path system, and the chemical column suppressor, the reaction reagent, the six-way valve and the derivatization reactor are connected through the flow path system; the six-way valve is provided with a regeneration flow path, a cleaning flow path and a generation flow path, and the three suppression columns of the chemical column suppressor are respectively connected with the regeneration flow path, the cleaning flow path and the generation flow path in turn; the three suppression columns of the chemical column suppressor respectively and sequentially displace hydrogen ions in the regeneration flow path, clean in the cleaning flow path and react in the generation flow path to generate hydriodic acid. By adopting the chemical column suppressor with the three suppression columns, derivative reagents can be continuously generated, and the generation efficiency of the derivative reagents is improved.

The invention discloses a method for in-situ determination of higher fatty acid in Baijiu, and belongs to the technical field of Baijiu detection. In order to realize in-situ simultaneous detection of a plurality of higher fatty acids in Baijiu, the invention provides a method for determining a plurality of higher fatty acids in Baijiu based on combination of ultra-high performance liquid chromatography and a quadrupole-electrostatic field orbitrap mass spectrometer, according to the method, liquid sample introduction is carried out directly or after membrane passing, and analysis is carried out through a high-resolution liquid mass spectrometer. And performing external standard method quantification after SIM mode scanning to obtain the content of the 14 higher fatty acids in the to-be-detected sample. According to the method, tedious pretreatment and derivatization processes are avoided, the 14 trace or trace higher fatty acids in the Baijiu can be accurately quantified at the same time, accurate verification can be achieved in Luzhou-flavor Baijiu, Fen-flavor Baijiu, Maotai-flavor Baijiu and rice-flavor Baijiu, the steps are simple, and operation is convenient.

The present invention discloses a method for measuring the hydroxyl value of a polyether polyol using nuclear magnetic resonance phosphorus spectroscopy, comprising: 1) adding a polyether polyol sample to be tested and an internal standard bisphenol A to a deuterated reagent and dissolving them by ultrasonication; 2) adding a phosphorus oxychloride compound and an acid binding agent to the mixture and allowing them to react fully to obtain corresponding different derivatized phosphorus-containing products; 3) performing a phosphorus spectroscopy test in a nuclear magnetic resonance analyzer to obtain nuclear magnetic resonance phosphorus spectroscopy data, processing and analyzing the data, integrating the nuclear magnetic resonance characteristic peak areas of the phosphorus-containing products after derivatization of the polyether polyol sample and the internal standard bisphenol A, and normalizing them to 100%, and calculating the hydroxyl value of the sample to be tested based on the molar ratio relationship between the products. The hydroxyl value result obtained by the present method has a relative deviation of less than 5% from the result obtained by the phthalic anhydride acylation method in the national standard GB / T 12008.3-2009, and the two results are close and highly accurate. The analytical testing method of the present invention is simple, has low pollution, and is short in time.

The invention discloses a method for detecting the content of chlorophenol substances in a bamboo material and a product for food contact, and belongs to the technical field of detection. The method specifically comprises the steps of standard liquid preparation, sample treatment and sample testing. According to the method, a content and migration quantity pretreatment mode without derivatization treatment is adopted, and an ultra-high performance liquid chromatography-tandem mass spectrometry detection technology is matched, so that the method for testing the content of the chlorophenol substances in the bamboo and wood materials and products for food contact, which is simple in pretreatment process, accurate in test, efficient, rapid, high in sensitivity and high in practicability, is realized.

The invention relates to the technical field of raw malt, and particularly discloses a raw malt extraction method which comprises the following steps: preparing a phosphate buffer solution; preparing a boric acid buffer solution; preparing a derivatization solution by using the prepared boric acid buffer solution; the method comprises the following steps: breaking walls of dried raw malt and crushing into powder by using a multifunctional crusher to obtain raw malt powder, dissolving the raw malt powder in distilled water, and carrying out ultrasonic extraction to obtain a raw malt stock solution; after a trichloroacetic acid solution is added into the raw malt stock solution, the raw malt stock solution is subjected to centrifugal treatment, and supernate is obtained; adding a sodium hydroxide solution into the supernate to enable the pH value of the first mixed solution to be neutral, and adding a phosphate buffer solution into the first mixed solution to obtain a second mixed solution; carrying out sampling derivatization on the second mixed solution and the derivatization solution, and carrying out ultraviolet determination within 2min. By adopting the derivatization-ultraviolet spectrophotometry, the analysis time can be remarkably shortened, the operation complexity and cost can be reduced, and the method is more suitable for daily use in laboratories.

The invention discloses a method for analyzing and detecting hydroxyl and amino substances in Baijiu and application, and relates to the technical field of Baijiu detection and analysis. The method comprises the following steps: carrying out derivatization reaction on bromine nicotinoyl chloride and hydroxyl and amino compounds in a white spirit sample to obtain a derivatized white spirit sample, carrying out data acquisition on the derivatized white spirit sample by utilizing a UPLC-HRMS platform, screening derivatized products by virtue of bromine isotope mass spectrum peaks, and determining the content of the bromine isotope mass spectrum peaks. And finally, performing high-coverage annotation on hydroxyl and amino compounds in the white spirit by combining multi-dimensional information including retention time, a primary mass spectrum and a secondary mass spectrum. The derivatization reaction does not need heating, the reaction time is short, a rapid and mild derivatization method is established, the loss of volatile compounds is avoided, and the analysis efficiency is improved; according to the invention, the natural isotope characteristics of bromine atoms are utilized to efficiently screen labeled compounds, and other heavy isotope labeling reagents are prevented from being additionally synthesized and used.

The invention relates to the technical field of chemical detection, in particular to a sample pretreatment method and a GC-MS (Gas Chromatography-Mass Spectrometer) method for simultaneously detecting glycidol and monochloropropanol in heated cigarette aerosol. The sample pretreatment method for simultaneously detecting the glycidol and the monochloropropanol in the heated cigarette aerosol comprises the following steps: capturing particulate matters in the heated cigarette aerosol; mixing the trapping material with ethyl acetate and an internal standard substance, extracting to obtain an extracting solution, and diluting with n-hexane; adding heptafluorobutyrylimidazole to perform derivatization reaction, washing with water after the derivatization reaction is completed, and drying to obtain a solution to be detected. According to the present invention, ethyl acetate is adopted for extraction, and detection analysis can be performed through dilution, HFBI derivatization, water washing and drying, such that the sample pretreatment step is substantially simplified, and the analysis sensitivity and the accuracy of the simultaneous detection of the three compounds such as the glycidyl, the 3-chloro-1, 2-propylene glycol and the 2-chloro-1, 2-propylene glycol can be easily improved.

The present invention belongs to the field of pharmaceutical chemical technology, and specifically relates to a method for analyzing chiral impurities of L-carnitine key intermediate L-carnitine. The method first uses (S)-2-(6-methoxy-2-naphthyl) propionyl chloride as a derivatization reagent to derive L-carnitine, and then uses high performance liquid chromatography to separate and detect the derivatized L-carnitine. The present invention proposes for the first time to use HPLC to determine the chiral purity of L-carnitine, which has simple steps and mild conditions, and is conducive to industrial promotion and application; the method of the present invention has strong specificity, high sensitivity, and good durability, and can be used for the accurate determination of the chiral purity of L-carnitine.

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 method for determining the content of penicillamine enantiomers by pre-column derivatization liquid chromatography, namely a method for detecting L-penicillamine in D-penicillamine or a method for detecting D-penicillamine in L-penicillamine, derivatization is carried out under conventional alkaline conditions, a termination reaction is carried out by conventional acid, the derivatization steps are simplified, the detection efficiency is improved, and the detection cost is reduced. According to the method, various interferences of other amino acids and corresponding isomers in the raw materials can be effectively avoided due to the gradient of the mobile phase, the damage to a chromatographic column is well reduced due to the fact that conventional reagents such as phosphoric acid and acetonitrile serve as the mobile phase, and the method is easy to operate, high in sample preparation speed and high in accuracy. The method has the advantages of strong anti-interference capability, good separation effect, high sensitivity, accurate result and good stability, realizes effective separation of penicillamine isomers, has a separation degree of greater than 2, can perform content determination on another main drug while performing impurity detection on one isomer, and has good practicability.

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 relates to the technical field of Baijiu detection, and particularly provides a method for detecting low-molecular aldehyde substances in Baijiu. The detection method comprises the following steps: adding an isotope internal standard substance into a white spirit sample, carrying out water bath derivatization, adding sodium chloride into a sample solution to saturate the solution, adding an extracting agent in proportion, carrying out ultrasonic centrifugation, and dehydrating with anhydrous Na2SO4 to obtain a sample solution. The method comprises the following steps: preparing an aldehyde compound mixed standard solution by adopting a simulated matrix, and treating according to a white spirit sample pretreatment method to obtain a standard solution; and simultaneously injecting the sample solution and the standard solution into a gas chromatograph-mass spectrometer, and determining the mass concentration of each aldehyde compound in the sample solution by adopting an internal standard curve method. According to the method, various aldehyde compounds in the white spirit can be detected at the same time, detection errors caused by the difference between a standard solution and a sample matrix are eliminated, the detection limit of the method is 0.47 microgram / L-6. 10 microgram / L, and the method has the advantages of being high in specificity, low in detection limit, high in accuracy and stable in result.

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 relates to the technical field of sample pretreatment and analytical chemistry, in particular to a derivatization-electric membrane extraction method for separating polar compounds. According to the specific technical scheme, the derivatization-electromembrane extraction method for separating the polar compound comprises the following steps: adding a derivatization reagent into a sample solution containing a polar target compound, and carrying out a derivatization reaction; taking the reacted sample solution as a donor phase, and migrating the polar target compound after the derivatization reaction into the acceptor phase solution through the supported liquid membrane under the action of an external electric field. According to the invention, the problem of poor extraction efficiency caused by poor hydrophobicity and low partition coefficient of the polar compound in an electric membrane extraction system in the prior art is solved.

The invention discloses a method for detecting 2-chlorine-propylene glycol and 3-chlorine-propylene glycol, and belongs to the technical field of food pollutant detection. The method for detecting 2-chlorine-propylene glycol and 3-chlorine-propylene glycol comprises the following steps: purifying a sample solution to be detected through a purification column to obtain a purified solution; removing water from the purified liquid, and adding a derivatization reagent for derivatization treatment to obtain a derivative liquid; the derivatization reagent is prepared from quinolaldehyde acyl chloride and 4-dimethylaminopyridine; and carrying out liquid chromatography-mass spectrometry detection on the derivative solution. The method provided by the invention can effectively distinguish two MCPD isomers, shorten derivatization time (20-30 min), increase hydrophobicity, promote chromatographic separation and improve electrospray ionization mass spectrometry (ESI-MS) sensitivity, and breaks through the limitation that a traditional method is limited to GC-MS.

The invention discloses an analysis method for determining the content of galactosamine in sulfated polysaccharide based on high-temperature hydrochloric acid hydrolysis and an ion chromatograph method, which comprises the following steps: hydrolyzing a test sample with hydrochloric acid at high temperature to release galactosamine, separating with an ion chromatograph and a sugar analysis column, detecting with a pulsed ampere detector, and determining the content of galactosamine in sulfated polysaccharide according to a galactosamine reference substance. And quantitatively analyzing the content of galactosamine in the test sample. The method disclosed by the invention has the advantages of simplicity, rapidness, accuracy, high efficiency, no need of derivation treatment and the like.

The invention relates to an unsaturated lipid analysis method, an unsaturated lipid analysis system and an on-line supercritical fluid derivative extraction-phase change focusing device thereof, the unsaturated lipid analysis method comprises the following steps: S1, under the action of a selective adsorbent, unsaturated lipid and a derivatization reagent are subjected to an epoxidation reaction in carbon dioxide in a supercritical state to obtain an extract liquid; the selective adsorbent is TiO2, and the derivatization reagent is m-CPBA; s2, changing the carbon dioxide in the supercritical state into a gas state by controlling the temperature and / or pressure, so as to enrich an epoxidation product of unsaturated lipid; and S3, analyzing the epoxidation product by adopting chromatography-mass spectrometry to obtain diagnosis ions of the epoxidation product, and determining the positions of double bonds in the unsaturated lipid according to the diagnosis ions. According to the method, derivation and extraction can be carried out in the same container, the extract directly analyzed by the supercritical fluid chromatography-mass spectrometry is provided, and the sample pretreatment step is simplified, so that sample degradation and artificial errors are reduced.

The invention provides an extracting agent and a method for separating high-economic-value metal in waste water by using the extracting agent, and belongs to the technical field of waste water purification, the extracting agent takes binary heterocycle as a molecular skeleton, the binary heterocycle is large in space volume, it can be guaranteed that the molecular structure of the extracting agent presents a specific space structure, and selective extraction of target metal is guaranteed; through chemical derivatization of binary heterocycle, the length of a molecular chain segment is directionally regulated and controlled, the chemical activity of a functionalized functional group can be changed, and the dimension of spatial extension of a molecular main chain of the extraction agent is regulated and controlled; according to the invention, through esterification reaction with aliphatic cyclic mercaptan, thioester groups are formed, so that the introduction of activation sites of the extraction agent is realized, the purpose of selective chelation / complexation with target metal ions is achieved, the interference of other impurity metal ions in a wastewater solution system is avoided, and meanwhile, the extraction agent can be suitable for solution systems of various complex anion types.

The present disclosure reveals the method for the quantitative determination of ethylene oxide (EO) and 2-chloroethanol (2CE) as contaminants in food products. The method is based on concentrated hydrochloric acid-mediated derivatization of the processed samples under specific treatment conditions, which provides the quantitative conversion of EO to 2CE, followed by the quantitative determination of thus formed 2CE with gas chromatography coupled with mass spectrometry (GC / MS-MS). The method enables a highly accurate procedure for the analysis of EO and 2CE in food samples at the concentration range from 0.019-0.19 mg / kg.

The invention provides a method for synchronously detecting eight catecholamines and metabolites thereof based on liquid chromatography-tandem mass spectrometry and application of the method. The detection method comprises the following steps: mixing a plasma or urine sample to be detected with an internal standard and acetonitrile; centrifuging, taking supernate, blowing liquid with nitrogen, and adjusting the pH value; mixing the supernate with a propionic anhydride solution, and carrying out derivatization reaction to obtain a test solution; performing liquid chromatography-tandem mass spectrometry detection on the test solution and the standard solution, separating dopamine, epinephrine, noradrenaline, epinephrine, noradrenaline, 3-methoxytyramine, homovanillic acid and vanillic mandelic acid by liquid chromatography, and determining the concentration of the standard substance as an X axis by using a mass spectrometry isotope internal standard quantification method. The ratio of the peak area of the standard substance to the peak area of the internal standard substance is the Y axis, establishing a standard curve, and calculating the concentrations of catecholamine and the metabolites thereof in the test solution. The method is high in detection efficiency, high in sensitivity and good in equipment compatibility, the detection time is shortened, and the cost can also be saved.

The invention provides a full-automatic online detection method for trace polycyclic aromatic hydrocarbon derivatives (SPAHs) in water, which comprises the following steps: (1) pretreatment: standing a water sample, centrifugally filtering to remove suspended matters, adding a prepared mixed standard solution, and directly loading on a machine; (2) enrichment and separation: adopting a Turbo flow C18-XL on-line solid phase extraction column to realize automatic enrichment and matrix purification of the 15 SPAHs, and combining an ultra-high performance liquid chromatography gradient elution program (methanol-ultrapure water system) to realize efficient enrichment and separation; and (3) detection and analysis: performing Full MS-ddMS2 scanning in an APCI (Amplified Peripheral Component Interconnect) source-Orbitrap high-resolution mass spectrum positive and negative ion switching mode to realize synchronous detection of hydroxyl, nitro and oxygen-containing SPAHs. According to the method, a unified detection system covering six hydroxyl polycyclic aromatic hydrocarbons, six oxygen-containing polycyclic aromatic hydrocarbons and three nitro polycyclic aromatic hydrocarbons is constructed for the first time, the detection limit is as low as 0.02 ng / L, and compared with a traditional GC-MS method, the sensitivity is greatly improved, and the sample pretreatment time is greatly shortened. Compared with the prior art, derivatization treatment is not needed, continuous sample injection is achieved through an online solid-phase extraction column regeneration technology, complex matrix interference is effectively eliminated in cooperation with a dynamic elimination function, and a high-sensitivity and high-throughput analysis method is provided for ecological risk assessment of trace SPAHs in underground water and surface water.

The invention discloses a liquid chromatography-tandem mass spectrometry detection method for catecholamine and metabolites thereof, which comprises the following steps: step 1, sequentially adding a sample to be detected, an internal standard solution, a derivatization buffer solution and a derivatization solution into holes in the third / ninth column of a 96-well plate, oscillating at room temperature, replenishing water, and continuing oscillating; step 2, adding an activating solution and magnetic beads into the first / seventh column of the 96-well plate; adding equilibrium liquid into the second / eighth column; a first leacheate is added into the fourth column and the tenth column; adding a second leacheate in the fifth / eleventh column; adding the eluent into the 6 / 12th column; then placing the sample on a 32-channel sample pretreatment system for magnetic solid-phase extraction; and step 3, liquid chromatography-tandem mass spectrometry detection. According to the method, the sample is firstly derivatized and then is subjected to magnetic solid-phase extraction, so that only less sample size is needed, the sensitivity is higher, and the economical efficiency is better; according to the method for directly derivatizing the sample, the sample does not need to be derivatized after being subjected to protein precipitation and supernatant removal, and the steps are simpler, more convenient and more automatic.