49 results about "Pre column derivatization" patented technology

The invention relates to a method for detecting the content of amino acid in a pesticide through pre-column derivatization liquid chromatography, and relates to the technical field of chemical analys.The method comprises the steps that a pesticide sample to be detected is extracted, and a solution containing amino acid is obtained; then, under the optimized alkaline pH and heating conditions, 4-fluoro-7-nitro-2, 1, 3-benzoxadiazole (NBD-F) is adopted as a derivatization reagent to be subjected to a pre-column derivatization reaction with amino acid, and a stable high-fluorescence NBD-F derivative is formed; injecting the derivative liquid into a high performance liquid chromatography system provided with a phenyl bonded phase chromatographic column, and efficiently separating the NBD-F derivative by utilizing pi-pi interaction and hydrophobic interaction of the phenyl column; and finally, detecting and quantifying through a fluorescence detector. Through the synergistic effect of NBD-F derivation and the phenyl column, the separation selectivity and the detection sensitivity are remarkably improved, and the reaction efficiency and the derivative stability are guaranteed through optimized derivation conditions.

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.

The invention relates to a method for detecting a phenolic antioxidant through dansyl chloride precolumn derivatization-high performance liquid chromatography-tandem mass spectrometry. The invention relates to a method for detecting a phenolic antioxidant by dansyl chloride pre-column derivatization-high performance liquid chromatography-tandem mass spectrometry, which comprises the following steps: carrying out pre-column derivatization treatment and acid neutralization treatment on a sample to be detected by dansyl chloride to terminate derivatization reaction to obtain a derivatized sample; and determining the derivatization sample by adopting a high performance liquid chromatography-tandem mass spectrometer so as to realize the ultra-trace detection of the phenolic antioxidant in the sample to be detected. The method solves the problem that the existing determination method cannot meet the ultra-trace detection requirement of the phenolic antioxidants, and also solves the problem that the existing determination method is difficult to realize the ultra-trace detection of various phenolic antioxidants.

The invention relates to the field of medicine detection, and particularly provides a method for detecting the residual content of triethanolamine by ion exchange-high performance liquid chromatography, and the chromatographic conditions in the method are as follows: a chromatographic column adopts a bonded cation exchange medium sulfonic group or carboxyl as a filler; a mobile phase is a phosphate buffer solution, and isocratic elution is carried out. According to the method disclosed by the invention, the triethanolamine does not need to be subjected to pre-column derivatization, and macromolecular protein and triethanolamine separation development (direct flow-through of macromolecular protein) is also not needed, so that the problem that the macromolecular protein is precipitated and removed to detect the triethanolamine when the gas chromatography is used is solved; and the problem that other detector modules such as a mass spectrum detector, an evaporative light detector and an electric conductivity detector need to be equipped and maintained is also solved. The method has the advantages of simple operation, accurate result, small interference and high sensitivity.

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 technical field of pharmaceutical analysis, in particular to a method for detecting the content of guanidine nitrate by precolumn derivatization-high performance liquid chromatography, which comprises the following steps: oscillating and uniformly mixing a guanidine nitrate reference substance or sample and pure water at room temperature, adding sulfuric acid concentrated liquor in cold water bath to perform derivatization reaction, after the reaction is finished, placing at room temperature, and performing column chromatography to obtain the guanidine nitrate content. Adding liquid caustic soda for neutralization, carrying out gradient constant volume by using a mobile phase, and filtering by using a microporous filter membrane to respectively obtain a derivatization reference solution and a derivatization sample solution; and respectively injecting the derivatization reference substance solution and the derivatization sample solution into HPLC, recording peak areas, and calculating the content of guanidine nitrate in the sample by adopting an external standard method. The guanidine nitrate sample is pretreated through the precolumn derivatization reaction, the guanidine nitrate derivative generated through the reaction has the advantages of being high in stability and easy to separate, ammonium nitrate and nitric acid impurities can be effectively prevented from interfering the detection result, the explosive picric acid is not adopted in the detection method, and the detection method is simple, safe and easy to implement.

The invention discloses a method for establishing a fingerprint spectrum of oyster formula granules. The method comprises the following steps: preparing a qualitative reference substance mother solution; preparing an oyster formula granule test solution; pre-column derivatization-high performance liquid chromatography is adopted for sample injection and determination, and a fingerprint spectrum of a qualitative reference substance mother solution and a fingerprint spectrum of a test solution are established under the same chromatographic condition; and comparing and analyzing the fingerprint spectrum of the qualitative reference substance mother solution and the fingerprint spectrum of the test solution to obtain the fingerprint spectrum of the oyster formula granules. The invention further discloses a method for determining the content of multiple components of the oyster formula granules. According to the present invention, the types and the multi-component content of the amino acids contained in the oyster formula granules are subjected to the related research by using the pre-column derivatization-high performance liquid chromatography, the oyster formula granule fingerprint spectrum is established, the 14 amino acids are identified, the 5 amino acid content method is established, and the established method has characteristics of good repeatability, high accuracy, and good clinical application prospect. And a basis is provided for quality control of the oyster formula granules.

The application provides a kind of water buffalo horn medicinal materials, standard decoction and its formula granules HPLC characteristic chromatogram construction method, comprising: A) water buffalo horn raw materials are extracted using solvent, to obtain the test solution;B) after the test solution is subjected to pre-column derivatization reaction, using high performance liquid chromatography, to obtain the HPLC characteristic chromatogram of water buffalo horn raw materials;The high performance liquid chromatography chromatographic conditions are: the chromatographic column is C18 column;Mobile phase A is acetonitrile-methanol-100mmol / L sodium acetate aqueous solution, mobile phase B is tetrahydrofuran-11mmol / L sodium acetate aqueous solution, gradient elution.The application uses high performance liquid chromatography, selects the above mobile phase for gradient elution, with alanine as reference, establishes the HPLC characteristic chromatogram of water buffalo horn medicinal materials, standard decoction and its formula granules, with good repeatability, precision, stable and reliable method, can control the quality of water buffalo horn medicinal materials, standard decoction and its formula granules.

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.

The invention provides a method for determining the content of methylhydrazine by pre-column derivatization-high performance liquid chromatography, which comprises the following steps: S1, uniformly mixing a methylhydrazine hydrate sample solution, 9-fluorenylmethoxycarbonyl chloride and an alkaline solution, standing for 20-50 minutes at room temperature to perform a derivatization reaction, and adding an acid solution to terminate the reaction; and S4, detecting the sample derived in the S1, establishing a chromatogram of methylhydrazine in the sample solution to be detected, obtaining a chromatogram retention time range of methylhydrazine, and calculating the content of methylhydrazine in the methylhydrazine hydrate according to the standard curve fitted in the S3. The pretreatment method is simple, the reaction condition is mild, the reaction rate is high, the detection sensitivity is high, the methylhydrazine derivative generated in a pre-column derivatization mode has ultraviolet absorption, a methylhydrazine derivative peak can be separated from a 9-fluorenylmethoxycarbonyl chloride chromatographic peak through reversed-phase high performance liquid chromatography, and detection of methylhydrazine is not interfered.

The invention belongs to the field of medicines, and particularly provides a method for determining the content of formaldehyde and acetaldehyde in polyethylene glycol and a preparation thereof by using a high performance liquid chromatography, and the specific chromatographic conditions are as follows: water and acetonitrile are used as mobile phases, and the flow velocity is 0.8-1.2 ml / min; and the detector is an ultraviolet detector. The method comprises the following steps: deriving trace formaldehyde and acetaldehyde in polyethylene glycol into substances with ultraviolet absorption by adopting a pre-column derivation method, then detecting through an ultraviolet detector, and calculating the content of formaldehyde and acetaldehyde in polyethylene glycol and a preparation thereof through an external standard method. The determination method has the advantages of high specificity, simplicity, convenience and rapidness in operation, high sensitivity and the like.

The invention discloses an RP-HPLC-RID method for detecting the (R)-isomer of pregabalin, belonging to the field of drug analysis. The method uses a polysaccharide derivative coated chiral reversed-phase chromatographic column and a differential refractometer to directly and effectively separate pregabalin and the (R)-isomer, and the detection result has good accuracy and high sensitivity. Compared with the existing evaporative light scattering detector method and pre-column derivatization reversed-phase chromatography method, the method is simpler to operate, has lower cost and is more environmentally friendly. The invention provides a better guarantee for the quality control of pregabalin and its preparations.

The invention relates to the technical field of analysis and detection, and discloses a method for detecting ethanolamine in a Nicodil bulk drug, which comprises the following specific steps: (1) carrying out derivatization reaction on ethanolamine in the Nicodil bulk drug by using 9-fluorenylmethyl chloroformate as a derivatization reagent to obtain a sample containing an ethanolamine derivatization product; and (2) preparing a test solution from the sample containing the ethanolamine derivatization product, and detecting the test solution by high performance liquid chromatography. According to the method, the chloroformic acid-9-fluorenylmethyl ester is used as a derivatization reagent, the pre-column derivatization HPLC method is established to measure the ethanolamine in the Nicodil bulk drug by optimizing derivatization conditions and methodology verification, the conditions are mild, the operation is simple, and the sensitivity is high.

The present invention discloses a high performance liquid chromatography method for detecting free chiral amino acid fingerprints of protein products and its application. First, free amino acids are extracted from protein products, and pre-column derivatization treatment is performed using Nα-(2,4-dinitro-5-fluorophenyl)-L-aminopropionamide, and separation and detection are performed using a high performance liquid chromatography-ultraviolet detector equipped with an Acclaim C18 chromatographic column, and finally the content of each amino acid is calculated using a standard curve. In this method, the derivative product has good stability within 15 hours; the analysis time for a single sample is 75 minutes; it makes up for the defects of the current high equipment cost of such methods, low stability of derivatized products, and long detection time for a single sample; it realizes the qualitative and quantitative characterization of the free chiral amino acid fingerprints of protein products, and provides key information for research on the nutritional metabolism and physiological functions of food-borne D-amino acids.

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 invention provides a method for detecting a genotoxic impurity o-tolualdehyde in indobufen, which comprises the following steps of: firstly dissolving raw material medicines and then carrying out low-temperature treatment to obtain a test solution with detectable concentration. According to the method, a common ultraviolet detector is used for detection, the method is simple, accurate, efficient and easy to operate, interference of various other organic impurities and genotoxic impurities in the indobufen is avoided, and the problems of high cost and operation complexity caused by pre-column derivatization ultra-high performance liquid chromatography in the prior art are solved.

The invention discloses a method for determining the content of 15 amino acids in cornu gorais in a phlegm-heat-clearing injection, and the method comprises the following steps: taking a test solution and a reference solution, carrying out pre-column derivatization, and then detecting, the phlegm-heat-clearing injection is composed of scutellaria baicalensis, bear gall powder, cornu gorais, honeysuckle, fructus forsythiae and propylene glycol, the reference substance is 15 amino acids, and the chromatographic conditions of the detection are as follows: a chromatographic column with octadecylsilane chemically bonded silica as a filler is adopted, a mobile phase A is an acid aqueous solution, an alkali aqueous solution and / or a buffer salt aqueous solution, and a mobile phase B is selected from one or more of acetonitrile, methanol, tetrahydrofuran and water; and obtaining content information of 15 amino acids in cornu gorais in the phlegm-heat-clearing injection according to a detection result. The method disclosed by the invention is simple, convenient, efficient and rapid, and provides a theoretical basis for the quality control of the Tweenqing injection and the deep research of a pharmacodynamic material basis by detecting the content of 15 amino acids in cornu gorais in the Tweenqing injection.

The invention discloses a pre-column derivatization device and a pre-column derivatization method for liquid chromatography, and relates to the technical field of chromatographic column derivatization. The pre-column derivatization device for liquid chromatography comprises: a storage chamber; the carrying platform can enter or move out of the storage chamber, and a raw material bottle, a sample bottle and a derivatization bottle which are required by pre-column derivatization are carried on the carrying platform; the manipulator is positioned on one side of the carrying table and is used for clamping the sampling needle, and the sampling needle can be used for extracting liquid from the raw material bottle, preparing required sample liquid in the sample bottle and uniformly mixing the sample liquid, and preparing required derivative liquid in the derivative bottle and uniformly mixing the derivative liquid; according to the pre-column derivatization device and the pre-column derivatization method for the liquid chromatogram, the sampling needle repeatedly sucks and mixes liquid, the straight liquid inlet pipe and the netted liquid discharge pipe are arranged, the liquid inlet pipe adopts the straight pipe, so that the liquid suction resistance can be greatly reduced, and the liquid discharge pipe adopts the netted pipe structure during liquid discharge, so that the liquid discharge resistance is greatly reduced; therefore, the liquid is uniformly mixed in a shearing, shunting and converging manner.

The invention belongs to the technical field of pharmaceutical analysis, and particularly relates to a method for separating and determining ethyl gatetate and impurities thereof through gas chromatography pre-column derivatization. The impurities comprise one or more of an impurity SM1c5, an impurity SM1c8 and an impurity SM1c. The method comprises the following steps: respectively carrying out pre-column derivatization treatment on each component by taking ethanol as a derivatization agent to obtain an impurity SM1c5 derivative, an impurity SM1c8 derivative and / or an impurity SM1c derivative; separating the derivatized compound by adopting gas chromatography; in the gas chromatography, a capillary column taking 6% cyanopropyl phenyl-94% dimethyl polysiloxane as a stationary liquid is adopted as a chromatographic column, a heating program is utilized for separation, and a product enters a detector for detection; and determining the nature of each component according to the chromatogram, and judging whether the impurity content in the detected product is qualified or not by adopting a limit method. The method has the characteristics of good separation degree, good durability, high sensitivity and good reproducibility.

The present invention relates to the field of pharmaceutical and chemical analysis and detection technology, and mainly to an analytical method for the chiral purity of an amino acid and its derivatives, which adopts pre-column derivatization-reverse-phase high performance liquid chromatography for analysis and determination, which mainly includes using 2,4-dinitrofluorobenzene for pre-column derivatization. The technical solution of the present invention is simple and easy to operate, easier to standardize operation, and more suitable for industrial application. In addition, the derivatization reaction conditions of the technical solution of the present invention are mild and rapid, and the analytical method has a stable baseline, high sensitivity, good repeatability, and a separation degree of up to 4.2 during system operation, and the test results are accurate and effective, providing reliable information for product research and development, production and purification, and laying a solid foundation for establishing quality control standards for amino acids and their derivatives.

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.

This invention belongs to the field of pharmaceutical technology, specifically relating to a Cistanche deserticola polysaccharide, its preparation method, and its applications. The Cistanche deserticola polysaccharide provided by this invention has a weight-average molecular weight (Mw) of 85.34 kDa, a number-average molecular weight (Mn) of 56.39 kDa, and a dispersion factor (Mw / Mn) of 1.51. This invention uses pre-column derivatization via PMP to determine the monosaccharide composition, followed by methylation-GC / MS to identify sugar residue linkage sites. Finally, it combines nuclear magnetic resonance spectroscopy to comprehensively analyze the sugar ring configuration and sequence information, providing a material basis for subsequent activity studies. The polysaccharide purified by this invention has lipid-lowering effects, increasing the added value of Cistanche deserticola. Simultaneously, it achieves the intensive processing and comprehensive utilization of this unique resource. Furthermore, the polysaccharide is derived from green and natural sources, and the product is safe and has no toxic side effects, making it promising for the development of lipid-lowering products.

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 invention discloses an amino acid trace analysis method for impure protein in a glucose polymer, which is characterized in that the content of amino acid after acidolysis of impure protein is used as a detection object, and the content of amino acid is measured by solid phase extraction-acidolysis-precolumn derivatization-high performance liquid chromatography. The method can effectively determine the content of 18 amino acids after acidolysis of the impure protein. The detection method disclosed by the invention is specific, reliable, universal, good in recovery rate, high in sensitivity and accuracy and wide in detection range, and plays a positive role in safety research and quality control of the medicinal raw material medicines or auxiliary materials.

The present invention discloses a method for determining the amino acid content in rice peptides by pre-column derivation-high performance liquid chromatography, which is characterized by comprising the following steps: Step S1, preparation of a standard solution; Step S2, preparation of hydrolyzed amino acids and free amino acids; Step S3, derivation of a sample; Step S4, pre-column derivation-high performance liquid chromatography determination. The present invention uses PITC as a pre-column derivatizing agent and combines an ultraviolet detector to quantitatively detect the content of 16 amino acids. This method is simple, rapid, has little interference, the derivatives are stable, and has wide applications, providing a good way for the rapid analysis of various amino acids.

The present invention relates to a detection method for the enantiomer (S)-4-propyl-dihydrofuran-2-one of the starting material (R)-4-propyl-dihydrofuran-2-one of brivaracetam; the detection method includes derivatizing (R)-4-propyl-dihydrofuran-2-one and its enantiomer (S)-4-propyl-dihydrofuran-2-one with trimethylsilyl iodide (TMSI) and ethanol, so as to change the chromatographic peak shape and improve the ultraviolet absorption, and then using reversed-phase high performance liquid chromatography, with water-acetonitrile as the mobile phase and a chiral column as the chromatographic column to detect the enantiomer (S)-4-propyl-dihydrofuran-2-one in the sample of the starting material (R)-4-propyl-dihydrofuran-2-one of brivaracetam. This detection method can completely separate (R)-4-propyl-dihydrofuran-2-one and its enantiomer and can quantitatively detect the isomer with a content higher than 0.09% in (R)-4-propyl-dihydrofuran-2-one, with high sensitivity, strong practicability, and a simple and fast detection process.

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.