15 results about "Pre column derivatization" patented technology

The invention discloses an online pre-column derivatization coupled liquid chromatography-mass spectrometry amino acid detection method, and relates to the technical field of analysis and detection, and the method comprises the following steps: obtaining a to-be-detected sample, and carrying out protein hydrolysis treatment to obtain hydrolysate; mixing the hydrolysate with a derivatization reagent, carrying out on-line derivatization reaction through multiple sections of reaction zones which are connected in series, and maintaining different pH environments in the reaction zones; an online detection unit is arranged at an outlet of the reaction zone to monitor the concentration of derivative products and adjust reaction conditions in real time; performing chromatographic separation on the derivative reaction liquid; switching an ion source ionization polarity mode according to an elution time window to carry out mass spectrometry detection; and substituting the mass spectrum response signal into the standard curve to calculate the amino acid concentration value. The method realizes automatic derivation and high-sensitivity detection of amino acid, and has the advantages of simplicity and convenience in operation, controllable reaction conditions and high detection efficiency.

This invention discloses an online pre-column derivatization coupled with liquid chromatography-mass spectrometry (LC-MS) for amino acid detection, relating to the field of analytical detection technology. The method includes: obtaining a sample for protein hydrolysis to obtain a hydrolysate; mixing the hydrolysate with a derivatizing reagent and performing an online derivatization reaction through multiple reaction zones arranged in series, each zone maintaining a different pH environment; setting an online detection unit at the reaction zone outlet to monitor the concentration of the derivatized product and adjust the reaction conditions in real time; performing chromatographic separation of the derivatized reaction solution; switching the ionization polarity mode of the ion source according to the elution time window for mass spectrometry detection; and substituting the mass spectrometry response signal into a standard curve to calculate the amino acid concentration value. This invention achieves automated derivatization and high-sensitivity detection of amino acids, with advantages such as simple operation, controllable reaction conditions, and high detection efficiency.

The invention relates to the field of detection, in particular to a method for determining the residual quantity of methoprene and methoprene in citrus through pre-column derivatization liquid chromatography-tandem mass spectrometry, and the method comprises the following steps: S1, preparation of a standard sample and a to-be-detected sample: S11, preparation of the standard sample, and S12, preparation of the to-be-detected sample; s2, preparation and derivation of a standard sample solution and a to-be-detected sample solution: S21, extraction, S22, purification and S23, derivation; s3, measuring; s4, establishing a linear equation; and S5, analyzing the sample to be detected. The technical problems that in the prior art, the ionization efficiency of methoprene and methoprene in the electrospray process is low due to the non-polar property of methoprene and methoprene, and electrospray ionization tandem mass spectrometry detection of methoprene and methoprene lacks the sensitivity required by trace analysis can be solved. The detection sensitivity of methoprene and methoprene in citrus fruits can be obviously improved.

This invention relates to the field of detection and analysis technology, and discloses a pre-column derivatization-liquid chromatography-tandem mass spectrometry (LC-MS / MS) method for the detection of perfluorocarboxylic acids and their substitutes. The highly sensitive and selective method provided by this invention, based on 3-nitrophenylhydrazine pre-column derivatization-LC-MS / MS, achieves good correlation (R0) of nine target analytes (C2-C9 perfluorocarboxylic acids and GenX) within a wide linear range of 0.0001-100 ng / mL. 2 The method has a detection limit as low as 0.83 ng / L and a quantitation limit of 2.76 ng / L, with a sensitivity of 0.83 ng / L for short-chain trifluoroacetic acid, significantly better than traditional gas chromatography. The spiked recoveries in ultrapure water matrix range from 88.2% to 115.7%, with inter-day and intra-day precisions of 0.2% to 17.61% and 3.5% to 16.3%, respectively, demonstrating good accuracy and reproducibility. This method incorporates highly polar short-chain perfluorocarboxylic acids, previously only analyzable by GC-MS, into the LC-MS / MS detection system. It also achieves trace detection of the novel pollutant GenX at the ng / L level, with significantly higher sensitivity than existing methods.

The application discloses application of a phenylpropionic acid compound in detection of monosaccharide composition of traditional Chinese medicine polysaccharide. The phenylpropionic acid compound has a structure as shown in formula (I). The application provides a new application of the phenylpropionic acid compound, and preliminary realization of quality control research on traditional Chinese medicine preknowing polysaccharide. Compared with a method for detecting monosaccharide composition of traditional Chinese medicine polysaccharide by using 1-phenyl-3-methyl-5-pyrazolone as a pre-column derivatization reagent, the application has the following advantages: 1. Derivatization of aldehyde sugar and ketose can be simultaneously realized; 2. The reaction temperature is more moderate, and the safety of the reaction is greatly improved; 3. The detection wavelength of HPLC-UV is improved from 245 nm to 274 nm, interference is reduced, and sensitivity is improved; and 4. The pre-column derivatization reagent is low in cost and easy to obtain.

The invention belongs to the technical field of pharmaceutical analysis, and particularly relates to a method for separating, detecting and determining an initial raw material SM3 and impurities thereof of ibrutinib. The impurities comprise one or more of propionyl chloride, 3-chloropropionyl chloride and benzoyl chloride. A mobile phase is a phosphate buffer solution as a mobile phase A, acetonitrile is a mobile phase B, a chromatographic column adopts octadecylsilane chemically bonded silica as a filler, and linear gradient elution of high performance liquid chromatography is carried out after pre-column derivatization. And then, according to a chromatogram, an external standard method is adopted to calculate the impurities according to a peak area. The method has the characteristics of good separation degree, good durability, high sensitivity and good reproducibility.

The invention discloses a method for screening AD biomarkers in blood based on a liquid chromatography-mass spectrometry technology, and relates to the technical field of biological analysis. The method comprises the following steps: S1, sample pretreatment: collecting a blood sample of a subject, and separating serum or plasma; the method comprises the following steps: adding an internal standard mixed solution containing a stable isotope label into a sample, adding an organic solvent to precipitate protein, carrying out vortex mixing, centrifuging, and taking a supernatant; s2, derivatization treatment: dividing the supernate obtained in S1 into a first sample and a second sample which are equal in volume; adding a chiral derivatization reagent into the second sample to carry out pre-column derivatization reaction to generate a diastereoisomer derivative; s3, carrying out liquid chromatography-mass spectrometry analysis; and S4, data processing. Through a 13C stable isotope internal standard correction strategy, the matrix effect of a blood sample is effectively eliminated, especially for quantification of D-amino acid, the detection limit can reach the nanomole level, the quantitative repeatability error is controlled between 3% and 8%, and the method is remarkably superior to a traditional method.

This invention discloses an online detection method and system for health hazard factors in drinking water based on pre-column derivatization, belonging to the field of water quality testing technology. The method includes: introducing a drinking water sample into a microfluidic chip-type derivatization reaction cell, where it reacts with a pH / temperature dual-response intelligent derivatization reagent to generate characteristic spectral derivatized products; acquiring spectral data using a micro fiber optic spectrometer, and calculating the derivatization efficiency in real time using a PID dynamic control model, automatically adjusting the reagent dosage and reaction conditions until the target is met; the target derivatized products are separated and purified twice by a two-dimensional chromatographic separation component and then transmitted to a dual internal standard correction machine learning model, where peak shape analysis, overlapping peak decomposition, dual internal standard correction, and quantitative regression calculations are performed to output the detection results and feed them back to the PID dynamic control model to update parameter thresholds. This invention improves the specificity, stability, and accuracy of the detection.

The application discloses a method for determining the content of potential genotoxic impurity tert-butyl hydroperoxide in deoxycholic acid bulk drug or an intermediate thereof, which adopts pre-column derivatization high performance liquid chromatography for detection, and adopts triphenylphosphine for derivatization treatment of the sample in pre-column derivatization; the detection conditions of the high performance liquid chromatography are as follows: a chromatographic column is an Agilent Eclipse Plus C18 column or a Waters Symmetry C18 column; a mobile phase A is 0.01% to 0.10% phosphoric acid solution; a mobile phase B is acetonitrile; a flow rate is 0.9 to 1.1 ml / min; a detection wavelength is 210 to 250 nm; a sample injection volume is 5 to 10 ul; a column temperature is 30 to 40 DEG C; a diluent is methanol or acetonitrile; and an elution mode is gradient elution. The method has the characteristics of low cost, simple operation, high accuracy and good sensitivity, and is suitable for quality control of medicines.

The application discloses a kind of brain tissue and blood plasma double matrix amino acid class matter pretreatment and detection method, the method includes the following steps: standard preparation;Differential sample preparation and homogenization;Double protein precipitation and preliminary purification;Solid phase extraction (SPE) depth purification and enrichment;Microenvironment control's pre-column derivatization;HPLC-FLD chromatographic separation and detection;Result calculation.The application is by optimizing sample pretreatment process, introduce SPE depth purification and pre-column derivatization technology under specific pH condition, effectively solve the problem of brain tissue and blood plasma matrix complex, many interferents and amino acid derivatization efficiency low.This method has the advantages of simple steps, high accuracy, good sensitivity and excellent reproducibility, can realize the rapid, synchronous detection of 13 kinds of amino acid class matters in rat brain tissue and plasma, provides reliable technical means for neurotransmitter and related metabolite research.

The application discloses a method for determining chiral amino acids in cetrotide acetate. Specifically relates to a method for determining the content of chiral amino acids in cetrotide acetate based on pre-column derivatization high performance liquid chromatography. Simple operation, without extraction separation of the sample after derivatization, the content of 10 kinds of chiral amino acids after hydrolysis of cetrotide acetate can be determined simultaneously, the sensitivity is high, more basis can be provided for structure confirmation, and reference can be provided for separation of chiral amino acids of polypeptide drugs.

The invention discloses a method for determining glycine by pre-column derivatization high performance liquid chromatography, which specifically comprises the following steps: S1, mixing glycine with a first solvent to prepare a glycine standard solution with a certain concentration gradient; s2, respectively putting glycine standard solutions with a certain concentration gradient into colorimetric tubes with stoppers, respectively adding an anhydrous sodium carbonate buffer solution and a dansyl chloride solution, carrying out pre-column derivatization, standing in a dark place at room temperature, and respectively and immediately adding methylamine hydrochloride solutions to obtain derivatized glycine standard solutions; and S3, determining the derived glycine standard solution by adopting high performance liquid chromatography to obtain a standard mixed solution chromatogram, and calculating by adopting a peak area through an external standard method to obtain a standard curve. The problem that an existing glycine detection method is complex is solved.

The invention relates to a method for determining the iron content in sucrose iron oxyhydroxide by high performance liquid chromatography. The chromatographic conditions of the liquid chromatograph are as follows: octadecylsilane chemically bonded silica is selected as a filler, the column length is 150mm, the column temperature is 30 DEG C, and the flow velocity is 1.0 ml / min; the liquid chromatograph adopts reversed-phase high-performance liquid chromatography for isocratic elution, a mobile phase is a buffer solution and a polar organic solvent, the buffer solution is a phase A, the polar organic solvent is a phase B, and the polar organic solvent of the phase B in the mobile phase is acetonitrile; pre-column derivatization is carried out by adopting a complex reagent, an iron element in sucrose hydroxyl iron oxide is converted into bivalent iron, and then derivatization is carried out by using the complex reagent. The method has the advantages that the stable ferrous complex is generated by using the complex, and the derivatization-high performance liquid chromatography is adopted for determination, so that the detection specificity and accuracy are improved, background interference is effectively removed, and the iron content in a test sample is accurately determined.

The invention discloses an online detection method and system for health hazard factors in drinking water based on pre-column derivatization, and belongs to the technical field of water quality detection.The online detection method comprises the steps that a drinking water sample is guided into a micro-fluidic chip type derivatization reaction pool and reacts with a pH / temperature double-response type intelligent derivatization reagent in the pool to generate a characteristic spectrum derivative product; collecting spectral data through a micro optical fiber spectrometer, calculating the derivation efficiency in real time through a PID dynamic regulation and control model, and automatically regulating the reagent addition amount and the reaction conditions until the standard is reached; the standard derivative product is separated and purified twice by the two-dimensional chromatographic separation assembly and then is transmitted to the double-internal-standard correction machine learning model, and a detection result is output and fed back to the PID dynamic regulation and control model through peak shape analysis, overlapping peak decomposition, double-internal-standard correction and quantitative regression operation so as to update a parameter threshold value; according to the invention, the detection specificity, stability and accuracy are improved.

The present application relates to the technical field of amino acid detection, and specifically relates to a method for quantitatively detecting free amino acids in a polypeptide drug starting material protective amino acid, wherein the liquid chromatography conditions are as follows: the chromatographic column is AQ-C18, the mobile phase A is 0.1+ / -0.02% formic acid aqueous solution, the mobile phase B is 0.1+ / -0.02% formic acid acetonitrile solution, and the diluent is acetonitrile aqueous solution; the CAD detector conditions are as follows: the evaporation temperature is 50+ / -2 DEG C, and the gas adjustment mode is the analysis mode; and the free amino acid content is calculated by substituting the peak area of the amino acid reference solution and the peak area of the Fmoc protective amino acid solution into the external standard method. Compared with the pre-column derivatization-high performance liquid chromatography method, the present application does not need expensive derivatization reagents and complex derivatization processes; compared with the ultra-high performance liquid chromatography-tandem mass spectrometry method, the present application does not need to configure expensive mass spectrometers, has good economic efficiency and practical value, and can quantitatively detect the free amino acid content.