27 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.

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.

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 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.

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 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 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 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 present application relates to a kind of dan sulfonyl chloride pre-column derivatization-high performance liquid chromatography-mass spectrometry detection phenolic antioxidant method.Dan sulfonyl chloride pre-column derivatization-high performance liquid chromatography-mass spectrometry detection phenolic antioxidant method, comprising the following steps: using dan sulfonyl chloride to the sample to be measured is carried out pre-column derivatization processing, acid neutralization treatment to terminate derivatization reaction, obtain derivatization sample;Using high performance liquid chromatography-mass spectrometry to determine derivatization sample, to realize the ultra trace detection of phenolic antioxidant in the sample to be measured.The present application solves the problem that existing determination method cannot meet the ultra trace detection requirement of phenolic antioxidant, also solves the problem that existing determination method is difficult to realize the ultra trace detection of multiple phenolic antioxidant.

The invention relates to the technical field of detection methods, in particular to a method for detecting impurities in a polaprezinc production process, which comprises the following steps: performing pre-column derivatization on a sample to be detected by using an ultraviolet derivatization reagent; the method comprises the following steps: detecting a to-be-detected sample subjected to pre-column derivatization by using a high performance liquid chromatography to realize separation and detection of L-histidine, D-histidine, D-carnosine and L-carnosine; a chromatographic column is an ion exchange type chiral chromatographic column; a mobile phase is a mixed solution of methanol, acetonitrile, water, an acidic additive and an alkaline additive; and the detector is an ultraviolet detector. The detection method provided by the invention has good sensitivity, specificity and accuracy, and can rapidly detect the content of impurities D-histidine and D-carnosine in the production process of polaprezinc, thereby further ensuring the product quality of polaprezinc bulk drugs and related preparations synthesized by using L-histidine as an initial raw material and the medication safety of patients.

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 application discloses a method for establishing a fingerprint spectrum of oyster formula granules, which comprises the following steps: preparing a qualitative control mother liquor; preparing a test sample solution of the oyster formula granules; determining the sample by using pre-column derivatization-high performance liquid chromatography, establishing the fingerprint spectrum of the qualitative control mother liquor and the fingerprint spectrum of the test sample solution under the same chromatographic conditions; and obtaining the fingerprint spectrum of the oyster formula granules by comparing and analyzing the fingerprint spectrum of the qualitative control mother liquor and the fingerprint spectrum of the test sample solution. The application further discloses a method for determining the multi-component content of the oyster formula granules. The application performs relevant research on the types and multi-component content of amino acids contained in the oyster formula granules by using pre-column derivatization-high performance liquid chromatography, establishes the fingerprint spectrum of the oyster formula granules, identifies 14 kinds of amino acids, simultaneously establishes five amino acid content methods, and the established method is good in repeatability and high in accuracy, thereby providing a basis for quality control of the oyster formula granules.

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.

The invention belongs to the technical field of analysis and detection, and discloses a method for determining monoethanolamine in petrochemical wastewater, which comprises the following steps: 1) extracting and concentrating monoethanolamine from wastewater, and re-dissolving with an organic solvent to obtain a to-be-detected solution; (2) adding N, N-dimethylformamide, pyridine and a derivating agent into the to-be-detected liquid obtained in the step (1), uniformly mixing, and carrying out silanization reaction at 30-60 DEG C for 30-80 minutes; and (3) adding dichloromethane into the solution obtained in the step (2), uniformly mixing, and detecting by adopting a GC-MS (Gas Chromatography-Mass Spectrometer) method to obtain the concentration of monoethanolamine in the sample to be detected. According to the method, the mixed solvent of N, N-dimethylformamide and dichloromethane is adopted as the solvent to assist the pre-column derivatization reaction, so that the derivatization reaction is mild in condition, can be carried out at normal temperature, is short in reaction time and relatively good in data stability, and can be used for rapid detection and analysis.

The invention belongs to the technical field of biological medicine, and particularly discloses tremella aurantialba polysaccharide with immunomodulatory activity and a preparation method and application thereof. The preparation method comprises the following steps: carrying out water extraction and alcohol precipitation on tremella aurantialba, and carrying out column chromatography separation to obtain tremella aurantialba polysaccharide TAP-2a; meanwhile, the structure of the TAP-2a is determined by adopting methods such as high performance gel permeation chromatography, precolumn derivatization, methylation combined with gas chromatography-mass spectrometry, nuclear magnetic resonance and the like, and the obtained TAP-2a is brand new tremella aurantialba polysaccharide. Meanwhile, the immunoregulation activity of the TAP-2a is further researched, the TAP-2a can promote proliferation of macrophages, up-regulate expression of iNOS, TNF-alpha, IL-6 and IL-1beta mRNA, promote secretion of NO, TNF-alpha, IL-6 and IL-1beta and enhance the phagocytic ability of the macrophages, and the result shows that the polysaccharide has the immunoregulation activity, can be used as a safe natural immunomodulator and has wide application prospects.

The invention discloses a method for rapidly and accurately detecting the content of citrulline, which belongs to the field of detection and comprises the following steps: preparing a standard solution, drawing a standard curve and detecting. The step of drawing the standard curve comprises the following steps: injecting the standard substance solution into a liquid phase instrument for liquid chromatography detection, measuring the peak area, and drawing the standard curve according to the correlation between the concentration of the standard substance solution and the peak area; the detection comprises the following steps: injecting a to-be-detected sample solution into a liquid phase instrument for liquid chromatography detection, determining the peak area, and calculating the content of citrulline in the to-be-detected sample according to the standard curve; when the standard substance solution and the to-be-detected sample solution are injected into a liquid phase instrument for liquid chromatography detection, an OPA pre-column derivatization detection method is adopted; according to the structural characteristics of citrulline, a C18 chromatographic column is selected as a stationary phase, a mobile phase with a proper proportion is combined, parameters are adjusted, the method suitable for citrulline detection is developed, and the method has the advantages of being rapid, simple and convenient to detect.