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84 results about "Precolumn derivatization" patented technology

Method for detecting free amino acids in tea by using reversed-phase high-performance liquid chromatography

The invention relates to a method for detecting free amino acids in tea by using the reversed-phase high-performance liquid chromatography. The method comprises the following steps: drying and grinding fresh tea, and adding boiling water for digestion; after supernatant liquor is collected, repeatedly extracting and merging the supernatant liquor; after the supernatant liquor is sucked and filtered, carrying out precolumn derivatization for a tea soup sample with an AccQ.Tag derivatization reagent; optimizing chromatographic separation and detection conditions with HPLC and AccQ.Tag C18 special amino acid analysis columns, and finally separating and detecting 19 kinds of free amino acids such as glutamine. The method can simultaneously determine the contents of 19 kinds of free amino acids such as glutamine in the tea, makes up the vacancy that glutamine in the tea cannot be quickly and accurately analyzed based on the high-performance liquid chromatography qualitatively and quantitatively at present, and provides a new idea for researching the synthesis path of amino acids in the tea.
Owner:ANHUI AGRICULTURAL UNIVERSITY

Precolumn derivatization-UPLC(ultra performance liquid chromatography)-ESI(electronic spray ion)+-MS/MS (mass spectrometry) detection method of glyphosate and glufosinate-ammonium pesticide residue in tea

The invention discloses a precolumn derivatization-UPLC(ultra performance liquid chromatography)-ESI(electronic spray ion)+-MS / MS (mass spectrometry) detection method of glyphosate and glufosinate-ammonium pesticide residue in tea, sodium borate is used as a buffer salt, a relatively pure target derived product can be obtained by derivatization of glyphosate and glufosinate-ammonium and FMOC-Cl and then ultra performance liquid chromatography (UPLC) washing out and separation, and response signals can be detected by tandem mass spectrometry (MS-MS). According to the method, competition between the two pesticide residue derivatization can be eliminated, the detection effect caused by matrix effect can be effectively weakened, and the derivatization time is shortened. By experimental verification, the detection method of glyphosate and glufosinate-ammonium pesticide (herbicide) residue in tea has the characteristics of being efficient, fast and accurate, good in sensitivity and the like, is applicable in detection of the glyphosate and glufosinate-ammonium pesticide residue in tea samples of sundried green crude tea, fermented tea and substitutional tea (green food substitutional tea of agricultural industry standards of NY / T2140-2012 of the people's Republic of China) and finished tea (brick tea, Tuo tea, melon-shaped tea, cake tea, scattered tea and bagged tea and the like).
Owner:MENGHAI TEA IND

Pretreatment method for measuring pesticides of glyphosate and phosphinothricin in tea leaves

ActiveCN103869028AExtraction does not affectImprove derivation efficiencyComponent separationPretreatment methodPhenolic content in tea
The invention provides a pretreatment method for measuring pesticides of glyphosate and phosphinothricin in tea leaves. In general, acidic precipitation, solid phase extraction, precolumn derivatization and a liquid chromatograph / mass spectrometer are used for measuring, and a method for measuring the residual amounts of glyphosate and phosphinothricin in the tea leaves by using the liquid chromatograph / mass spectrometer is established. In the method, a large quantity of tea polyphenols in the tea leaves are precipitated, so that the deviation efficiency of solid phase extraction liquid and 9-fluorenylmethyl chloroformate is increased, the interference of impurities is reduced, and the high sensitivity is realized. The method is accurate, efficiency and stable, can meet the requirement of residue detection, and can be applied to the qualitative and quantitative analysis of the glyphosate and the phosphinothricin in the various tea leaves.
Owner:TEA RES INST CHINESE ACAD OF AGRI SCI

Method for high-sensitivity detection of aflatoxin and application of aflatoxin

The invention discloses a novel method for rapidly detecting aflatoxin in food. The method comprises main steps as follows: an existing precolumn derivatization technology and post-column derivatization technology for aflatoxin are combined, precolumn derivatization is performed under the irradiation of ultraviolet light, a derivative reaction is performed completely, produced fluorescence is strong, the fluorescence stability of a derived product is good, and meanwhile, the detection sensitivity is also improved. Compared with methods for measuring aflatoxin in existing standards, the method has the characteristics that the detection sensitivity is high, post-column light derivatization equipment is not required, the reproducibility is good, the detection is accurate and the like.
Owner:云南健牛环境监测有限公司

Reverse-phase chromatography and mass-spectrometry combined detection method for complete low-molecular-heparin degradation product through precolumn derivatization

ActiveCN103630647AEnsure safetySolve the problem that only 8 common heparin disaccharides can be detectedComponent separationReversed-Phase Liquid ChromatographyMass Spectrometry-Mass Spectrometry
The invention relates to a reverse-phase chromatography and mass-spectrometry combined detection method for a complete low-molecular-heparin degradation product through precolumn derivatization. All components of the complete low-molecular-heparin degradation product are detected by combining reversed-phase chromatography and a high-resolution mass spectrum; all the components in a sample are separated through the reversed-phase chromatography, and a precision molecular weight can be obtained through the high-resolution mass spectrum; besides detection of eight common heparin disaccharides, tail end modification structures and special structures such as 3-O-tetrose-hydrosulfates relevant to anticoagulation and trisaccharides obtained through peeling reaction can be also detected; therefore, the structure of each complete low-molecular-heparin degradation product can be precisely represented. According to the reverse-phase chromatography and mass-spectrometry combined detection method, the problem that only the eight common heparin disaccharides can be detected in the prior art is solved; the reverse-phase chromatography and mass-spectrometry combined detection method has an extremely large practical value in research, development and production control of low-molecular-heparin imitating drugs and guarantee of the safety of the drugs.
Owner:HEBEI CHANGSHAN BIOCHEM PHARMA

Pericarpium Trichosanthis or Pericarpium Trichosanthis injection liquid chromatography fingerprint test method

The invention discloses a test method of liquid spectrum finger diagram of melon, or melon injection, comprising that (1), preparing melon, or melon injection into a sample solution, (2), respectively absorbing citrulline water solution and the sample solution, to be filled into a liquid spectrometer, and using the solution of phthalaldehyde and the solution of chloride aminic acid fluorenes methyl ester to process derivatization, (3), testing liquid spetrum. The inventive test method first discloses a liquid spectrum finger diagram of melon or melon injection, with high accuracy, stability and repeatability, as one analysis test method which can control the product quality, used in product quality test. The inventive method first obtains the high-effect liquid spectrum contrast finger diagram of melon and melon injection, as diagram 1 and diagram 2.
Owner:SPH NO 1 BIOCHEM & PHARMA CO LTD

Detection method for simultaneously measuring three kinds of isocyanates by using precolumn derivatization-gas chromatography-mass spectrography

The invention provides a detection method for simultaneously measuring residual toluene 2,4-diisocyanate (2,4-TDI), toluene 2,6-diisocyanate (2,6-TDI) and diphenylmethane diisocyanate (MDI) in the product by using precolumn derivatization-gas chromatography-mass spectrography. The method comprises the following specific steps: performing ultrasonic extraction on a sample, performing rotary evaporation and concentration on the extracting solution, reacting in an acidic aqueous solution, neutralizing with an alkali liquor, extracting by using an organic solvent, performing organic phase derivatization, removing excessive derivatization reagents with a buffer solution, taking the organic phase as a to-be-measured solution after solution separation, measuring and confirming by using a gas chromatography-mass spectrometer, carrying out a blank experiment, quantifying by using an external standard method, measuring the target compound in the sample solution, and the like. According to the method, the measurement parameters and test steps of the gas chromatography-mass spectrography are reasonably selected, the content of 2,4-TDI, 2,6-TDI and MDI in leather, artificial leather and textiles can be simultaneously measured by adopting selective ion scanning detection and external standard method quantification, and the results are simultaneously obtained by virtue of one-step pretreatment. The method has the characteristics of high precision, high interference resistance and low detection limit.
Owner:SICHUAN UNIV

Method for measuring optical purity of (R)-3-quinuclidinol

The invention belongs to the technical field of pharmaceutical chemical engineering, and in particular relates to a method for measuring the optical purity of (R)-3-quinuclidinol. The method for measuring the optical purity of (R)-3-quinuclidinol comprises the steps of (a) preparing a sample; (b) preparing a test solution; (c) preparing a chromatographic condition, and performing detection. According to the method, a precolumn derivatization chiral chromatography method is adopted to measure the optical purity of (R)-3-quinuclidinol; specifically, the precolumn derivatization method is used for enabling (RS)-3-quinuclidinol racemate and paratoluensulfonyl chloride to react to generate (RS)-3-quinuclidinol paratoluensulfonyl chloride derivative, namely quinuclidinol 3-paratoluene sulfonate; then the chiral chromatography method is used for measuring the optical purity; therefore, the technical difficulty in measurement of the optical purity of (R)-3-quinuclidinol is creatively solved.
Owner:JINAN ASIA PHARMA TECH

Method for quantitatively analyzing perfluorocarboxylic acid compounds through precolumn derivatization-gas chromatography

The invention relates to a method for quantitatively analyzing perfluorocarboxylic acid compounds through precolumn derivatization-gas chromatography. The determination method comprises the following steps that standard curves of nine perfluorocarboxylic acid compounds are formulated; a water sample is subjected to derivatization with 2,4-difluoroaniline and DCC after being subjected to solid-phase extraction pretreatment, after filtering is conducted through an organic microfiltration membrane, determination is conducted through gas chromatograph, and the variety and content of the perfluorocarboxylic acid compounds in the to-be-determined sample are obtained by contrasting the standard curves and regression equations. The correlation coefficients (R2) of the regression equations of the standard curves of the nine perfluorocarboxylic acid compounds are all larger than 0.99, the relative standard deviations (RSD) of the regression equations range from 1.3% to 7.5%, the accuracy is high, and the perfluorocarboxylic acid compounds in the sample are accurately and quantitatively analyzed through the linear regression equations on the basis of qualitative analysis. By means of the method, the nine perfluorocarboxylic acid compounds can be determined and analyzed simultaneously, and the method has the advantages of being high in precision and anti-jamming capability, low in detection limit and good in reproducibility.
Owner:ZHEJIANG WANLI UNIV

Method for detecting content of urea in brewed wine by using high performance liquid chromatography

The invention relates to a method for detecting the content of urea in brewed wine by using high performance liquid chromatography. The method comprises the following steps: weighing an appropriate sample, selecting a proper solvent, and performing pre-treatment on the sample by using precolumn derivatization, rotary evaporation concentration and the like; and detecting urea derivatives by using a high performance liquid chromatograph connected with a fluorescence detector, wherein the organic flow phase and the inorganic flow phase are in variable ratio, the flow speed is set as 1mL / min, the sampling amount is set as 10 microliters, the chromatographic column is selected as the C18 chromatographic column, the column temperature is 40-50 DEG C, and the detection wavelength of the fluorescence detector as follows: the lambda ex is 208nm, and the lambda em is 308nm. The detection method provided by the invention has the characteristics of being simple, fast and high in recycling rate.
Owner:CENT TESTING INT GRP CO LTD

Method for splitting DL-menthol by means of pre-column derivatization high performance liquid chromatography

The invention discloses a method for splitting DL-menthol by means of pre-column derivatization high performance liquid chromatography. The method comprises the following steps: firstly, carrying out a precolumn derivatization esterification reaction on DL-menthol and aromatic acid to obtain corresponding ultraviolet absorption DL-mint alcohol; then, preparing the DL-mint alcohol ester to a 0.2-1.0mg / mL sample solution by adopting an opposite mobile phase system formed by an aqueous phase and an organic phase by using an amylase chiral chromatographic column through the high performance liquid chromatograph; controlling the flow rate at 0.4-1.0mL / min, the sample size at 2-10 microlitre, the detecting wave length at 220-280nm and the temperature of the wave length at 20-35 DEG C for chromatographic column separation so as to separate the DL-mint alcohol ester; and finally, respectively hydrolyzing to obtain D-menthol and L-menthol. The method for detecting and splitting menthol is convenient, practical and high in sensitivity.
Owner:SHANGHAI INST OF TECH

Qualitative and quantitative method for various biogenic amines in white wine

The invention discloses a qualitative and quantitative method for various biogenic amines in white wine and belongs to the technical field of white wine analysis and detection. According to the qualitative and quantitative method, the liquid-liquid extraction is utilized to enrich the biogenic amines in the white wine; derivation is required by both gas phase qualitative treatment and liquid phase quantitative treatment; a derivation agent adopted by the gas phase is TFAA (Trifluoroacetic Anhydride); and dansyl chloride precolumn derivatization is taken as the derivation agent for the liquid phase. According to the method provided by the invention, 9 biogenic amines are firstly determined in the white wine; the limit of detection of the quantitative method can be reduced to about 10ug / L; the linearly dependent coefficient is more than 0.99; the recovery rate is 80.19%-104.05%; the relative standard deviation is within 4%; the biogenic amines in the white wine can be detected by using the qualitative and quantitative method; the feasibility is excellent; and the precision is high.
Owner:JIANGNAN UNIV

Method for resolving R/S-3-quinuclidinol by adopting precolumn derivation high performance liquid chromatography

The invention discloses a method for resolving R / S-3-quinuclidinol by adopting a precolumn derivation high performance liquid chromatography. The method comprises the following steps of firstly, carrying out precolumn derivation esterification reaction on R / S-3-quinuclidinol to obtain R / S-3-quinuclidinol ester; then, preparing a 1.0mg / mL sample solution from R / S-3-quinuclidinol ester by using a high performance liquid chromatograph, wherein an amylose chiral column is used as a chromatographic column, a mixed solution of n-hexane, an alcohol and an alkaline additive is used as a positive mobile phase, and the flow rate, the sample volume, the detection wavelength and the chromatographic column temperature are controlled at 0.6-1mL / min, 5mul, 220-280nm and 20-35 DEG C respectively; and resolving the R / S-3-quinuclidinol ester chirally. The chromatographic peak obtained by adopting the method is good in pattern and symmetry and high in degree of resolving, and the method can be used for detecting and resolving R / S-3-quinuclidinol efficiently, rapidly and sensitively.
Owner:上海柏狮生物科技有限公司

Method for measuring organic acid content based on precolumn derivatization LC-MS

The invention discloses a method for measuring organic acid content based on precolumn derivatization LC-MS, and belongs to the field of analytical chemistry.The method comprises the steps that 1, a sample to be tested, sodium carbonate and 2-bromoacetophenone are added to a solvent, a derivatization reaction is carried out for 20 h to 28 h at the temperature of 50 DEG C to 60 DEG C after even mixing, and the product is cooled for use; 2, the reaction product in the step 1 is taken for liquid chromatogram-mass spectrum analysis, and the content of organic acid in the sample to be detected is calculated by referring to a standard curve.A chemical modification technology is adopted for derivatization of the organic acid, the physicochemical characteristic of the organic acid is changed, the ionization efficiency can be improved in hygroplasm combined detection, matrix interference can be reduced, meanwhile, interference of inorganic salt and endogenous impurities is reduced, the signal strength ofanalyte is improved, and chromatographic separation and mass spectrometric detection are convenient; then a liquid chromatogram-mass spectrum combined technology is adopted for analyzing and detecting the derivatization product, qualitative and quantitative analysis on the organic acid can be achieved, and the advantages of being simple, efficient, high in detecting sensitivity, good in accuracy and the like are achieved.
Owner:HENAN UNIVERSITY

Adulteration identification method for cod-liver oil

InactiveCN108802209ARapid identificationAdulteration identification method scienceComponent separationCod liver oilVegetable oil
The invention relates to an adulteration identification method for cod-liver oil. The adulteration identification method comprises the following steps: performing peak area determination on fatty acidin the cod-liver oil and fish oil for adulteration by adopting precolumn derivatization capillary gas chromatography, calculating the percentage of typical fatty acid relative to total fatty acid according to an area normalization method and establishing a threshold, wherein the threshold of vegetable fatty acid references to national standards; finding out fatty acid with characteristic indexesby comparing the threshold of the fatty acid in the cod-liver oil with that of the fatty acid in the oil for adulteration; rapidly identifying the adulterated fish oil in the cod-liver oil by establishing a two-dimensional adulteration model of characteristic fatty acid and drawing an adulteration identification analysis chart; rapidly identifying adulterated vegetable oil in the cod-liver oil byadopting linoleic acid in the vegetable oil as a characteristic index and analyzing and comparing the content of the linoleic acid in a sample with the threshold of the cod-liver oil. The adulterationidentification method based on the characteristic indexes of the fatty acids in the cod-liver oil, the fish oil and the vegetable oil, provided by the invention, has the characteristics of science, accuracy, simplicity and convenience.
Owner:ZHOUSHAN INST FOR FOOD & DRUG CONTROL

Method for quickly detecting monosaccharide composition in medicine mulberry polysaccharide through UPLC-TUV

The invention discloses a method for rapidly detecting the composition of monosaccharides in mulberry polysaccharides by using UPLC-TUV. (PMP) pre-column derivatization, and then enter the UPLC-TUV system for detection. The invention discloses detection conditions for ultra-high performance liquid chromatography detection. The method is fast, sensitive, good in separation effect and high in repeatability, and can quickly and accurately detect the composition of monosaccharides in the polysaccharide of mulberry fruit.
Owner:SOUTHWEST UNIVERSITY

Method for determining content of salivary acid in serum by using UIO-66-NH2 material

The invention belongs to the technical field of application of metal-organic framework composite material, and in particular, relates to a method for determining the content of salivary acid in serum by using a UIO-66-NH2 material. The method comprises the steps: hydrolyzing a serum sample by using trifluoroacetic acid, removing proteins, and then centrifuging to obtain a serum treatment fluid; mixing the serum treatment fluid with the UIO-66-NH2 material, carrying out vortex oscillation extraction, extracting the salivary acid in the serum treatment fluid into the UIO-66-NH2 material, and centrifuging to obtain a salivary acid-containing UIO-66-NH2 material; carrying out ultrasonic elution of the salivary acid-containing UIO-66-NH2 material obtained after centrifugation with an acetic acid aqueous solution, and making the salivary acid completely eluted from the UIO-66-NH2 material, to obtain an eluate; and carrying out precolumn derivatization of the eluate with a fluorescence derivatization reagent, and then carrying out high performance liquid chromatography detection. The method for determining the content of the salivary acid in the serum has the advantages of high selectivity and high sensitivity.
Owner:QUFU NORMAL UNIV

Method for determining 4-nitrobenzaldehyde in chloramphenicol or preparations thereof through derivatization HPLC-UV/Vis

The invention discloses a method for determining 4-nitrobenzaldehyde in chloramphenicol or preparations thereof through derivatization HPLC-UV / Vis. The method comprises the following steps: subjecting4-nitrobenzaldehyde to derivatization generation of a product with strong absorption in an ultraviolet-visible light zone in virtue of a nitrophenylhydrazine derivatization reagent; and with a reaction solution as a loading sample, determining the derivatization products of 4-nitrobenzaldehyde in the ultraviolet-visible light zone by using HPLC-UV / Vis based on the principle of reversed phase partition chromatography so as to realize qualitative or quantitative determination of 4-nitrobenzaldehyde. According to the invention, since the 4-nitrobenzaldehyde derivatization products based on the nitrophenylhydrazine derivatization reagent have obvious bathochromic shift effect due to generation of hydrazone bonds at nitro para-positions, the simple and universal method for determining 4-nitrobenzaldehyde through pre-column derivatization HPLC-UV / Vis is established. Methodological verification results show that the method has good specificity.
Owner:CHINA PHARM UNIV

Method for determination of free amino acid in spleen aminopeptide

The invention discloses a method for determination of free amino acid in spleen aminopeptide, comprising the following steps: Step 1, solution preparation: a reference stock solution, an internal standard stock solution, a mobile phase A and a mobile phase B are prepared; Step 2, sample treatment; Step 3, precolumn derivatization; Step 4, chromatographic separation, sample introduction, gradient elution, detection wavelength being 338 nm and 262 nm respectively, and determination of peak area; and Step 5, free amino acid content calculation. The invention has the following advantages and effects: by liquid chromatogram of precolumn derivatization, a sample undergoes derivatization and then sample introduction is carried out, and through gradient elution during chromatographic separation, free amino acid in spleen aminopeptide is successively eluted; through selection of an amino acid standard substance for chromatographic elution, equation of linear regression is calculated by linear regression of solution mass concentration X to peak area Y, and content of free amino acid in spleen aminopeptide is calculated according to the peak area. Accuracy of determination results is high, and it is convenient to control the content of a spleen aminopeptide product.
Owner:ZHEJIANG FENGAN BIOPHARM

Method for extraction and derivatization of piperazine residues in tissue of fowls and pigs

The invention specifically relates to a method for extraction, purification and derivatization of piperazine residues in the tissue of fowls and pigs. The method comprises the following steps: with pure acetonitrile as an extraction solvent and n-hexane as a degreasing agent, treating a tissue sample by using an accelerated solvent extraction instrument (ASE); continuously carrying out on-line degreasing and piperazine extraction; subjecting the obtained extract to purification via a solid-phase extraction method, concentration by a vacuum centrifugation concentration instrument and acetic anhydride-process precolumn derivatization; and carrying out confirmatory analysis on the extracted, purified and derivatized sample by using gas chromatography-tandem mass spectrometry (GC-MS / MS). With the method, the extraction rate of piperazine reaches 90% or above.
Owner:YANGZHOU UNIV

Separation detection method of pregabalin chiral isomers

The invention provides a derivatizing separation detection method of pregabalin chiral isomers and belongs to the field of analytical chemistry. According to the method, pre-column derivatization is performed on pregabalin by taking fluorenylmethoxycarbonyl chloride as a derivatization reagent; a CHIRALPAK. AD-H chiral chromatographic column is taken as a chromatographic column, and the mixture of n-hexane and absolute ethyl alcohol is taken as a moving phase, and separation detection can be realized by use of efficient liquid chromatography. The precolumn derivatization method has the advantages of mild reaction conditions, stable derivation products, high reaction speed, few side reactions, no interference of excessive derivatization reagent on the measurement, realization of separation of the pregabalin and the pregabalin chiral isomers, and the like.
Owner:北京紫萌医药科技有限公司

Method for determining monosaccharide constitution of Yupingfeng polysaccharide

The invention discloses a method for determining the monosaccharide constitution of Yupingfeng polysaccharide. The method comprises the following steps: (1) preparing a Yupingfeng polysaccharide hydrolysis sample; (2) preparing a mixed monosaccharide standard product; (3) carrying out pre-column derivatization: respectively mixing the Yupingfeng polysaccharide hydrolysis sample obtained in the step (1) and the mixed monosaccharide standard product obtained in the step (2) with a 0.5mol / L PMP methanol solution and a 0.3mol / L NaOH solution, adequately shaking, reacting for 30 minutes under a 68DEG C water bath condition, cooling to the room temperature, adding 0.3mol / L hydrochloric acid for neutralization, adding chloroform, carrying out extraction and centrifugation, abandoning an organiclayer, repeatedly carrying out extraction for 2-3 times to obtain an upper-layer liquid, and filtering by virtue of a 0.22-micron micro-hole filtration film, so as to respectively obtain a Yupingfengpolysaccharide derivatization treatment solution and a mixed monosaccharide derivatization treatment solution for later use; and (4) carrying out high performance liquid chromatography analysis: determining the monosaccharide constitution and content of Yupingfeng polysaccharide. The method is high in sensitivity, small in sample dosage and good in stability, and the monosaccharide constitution ofYupingfeng polysaccharide can be determined through simple operation and relatively low cost.
Owner:FOSHAN UNIVERSITY

Method for separating and determining 1,2-propylene glycol enantiomers by using gas chromatography

The invention discloses a method for separating and determining 1,2-propylene glycol, bulk drugs containing 1,2-propylene glycol and 1,2-propylene glycol enantiomer impurities in preparations of the bulk drugs by using precolumn derivatization gas chromatography. The method employs an aldehyde ketone compound as a derivative reagent, carries out precolumn derivatization on the aldehyde ketone compound and 1,2-propylene glycol in the presence of a catalyst and a water reducer and determines trace enantiomer impurities by using gas chromatography. The method provided by the invention overcomes the defect of incapability of accurate quantification of 1,2-propylene glycol enantiomer impurities due to serious trailing of peaks during frequently-used chiral gas chromatographic column separation and guarantees that the quality of 1,2-propylene glycol, the bulk drugs containing 1,2-propylene glycol and the preparations thereof is controllable.
Owner:CHONGQING PHARMA RES INST

Application and detecting method of 3,2'-diaminobenzidine (DAB) and quinoxaline analogues thereof on diacetyl detection

The invention discloses an application and a detecting method of 3,2'-diaminobenzidine (DAB) and quinoxaline analogues thereof on diacetyl detection and provides a method for detecting content of diacetyl (2,3-butanedione, C4H6O2) in liquid samples by adopting a precolumn derivatization-HPLC (high performance liquid chromatograph) method. The DAB and the quinoxaline analogues thereof are taken as a derivatization reagent to detect the content of the diacetyl in the liquid samples, reaction can be completely performed for 5 minutes at the indoor temperature, and PH (potential of hydrogen) value of the reaction system does not need to be strictly controlled. Compared with an existing precolumn-derivatization-HPLC method, the detecting method has the advantages of moderate derivatization reaction conditions, easiness in operation, rapidness and the like.
Owner:NORTHWEST UNIV

Precolumn derivatization and high-efficiency liquid-phase fluorescence detection method for tetrodotoxin and kit based on the method

The invention discloses a precolumn derivatization and high-efficiency liquid-phase fluorescence detection method for tetrodotoxin. The method includes following steps: (1) preparing a sample solution of a sample to be measured and a standard substance solution of tetrodotoaxin; (2) adding 0.2 ml of a pH maintenance solution to 0.4 ml of the sample solution for controlling pH of the sample solution at a range between 11.6 and 11.9, then adding 0.1 ml of a derivatization agent 1 and 0.1 ml of a derivatization agent 2, mixing uniformly, carrying out a water-bath heating process for 20 min and then carrying out a cooling process to room temperature, adding 0.1 ml of a stopping solution for enabling the pH of the sample solution to be neutral, and then carrying out a then diluting to volume with ultrapure water, adding the standard substance solution of the tetrodotoxin to the sample solution, mixing uniformly, and then carrying out a fluorescence derivatization process to the sample solution; and (3) with a liquid-phase chromatograph instrument equipped with a fluorescence detector, analyzing the sample solution which is subjected to the fluorescence derivatization process in the step (2) and the standard substance solution of the tetrodotoxin to detect the tetrodotoxin qualitatively and quantitatively in the sample solution. The invention also discloses a kit which is suitable for the method. The method is used for detecting the tetrodotoxin in aquatic products qualitatively and quantitatively and is reliable in result and low in detection limit.
Owner:SOUTH CHINA SEA FISHERIES RES INST CHINESE ACAD OF FISHERY SCI

Pre-column electrochemical derivatization one-time total quantity measuring method for malachite green and leucomalachite green in aquatic products

The invention provides a pre-column electrochemical derivatization one-time total quantity measuring method for malachite green and leucomalachite green in aquatic products and belongs to one-time total quantity measuring methods for converting leucomalachite green into malachite green. The key of the method is that it is found that after a leucomalachite green solution is subjected to oxidation voltage +650 mv of an electrochemical Coulomb detector (ECD), averagely 98.86% of leucomalachite green is converted into malachite green, original malachite green is unchanged, and the total concentration of leucomalachite green and malachite green can be measured through a high performance liquid chromatograph in the one-time measurement process of leucomalachite green and malachite green in a sample. Sample pre-treatment time is greatly shortened, use of reagent consumables is reduced, and electrochemical precolumn derivatization is used for replacing post-column derivatization of lead dioxide in the national standard. The method has the advantages of being simple in sample pre-treatment, good in purification effect, high in derivatization rate and high in recovery rate.
Owner:SICHUAN ENTRY EXIT INSPECTION & QUARANTINE BUREAU INSPECTION & QUARANTINE TECHN CENT

Method for analyzing glucosamine content in whey protein glycosylation product by reverse-phase high performance liquid chromatography (RP-HPLC)

The invention relates to a quantitative detection method for glucosamine content in a whey protein glycosylation product, belonging to the technical field of detection and analysis. According to the method, hydrochloric acid is adopted for hydrolysis of glucosamine in glycosylation whey protein and precolumn derivatization, and then a reverse-phase high performance liquid chromatography (RP-HPLC) is utilized for determining glucosamine content in a protein hydrolysate. The method is rapid, simple and convenient, high in sensitivity, and suitable for determination of glucosamine content in various protein glucosamine glycosylation products.
Owner:NORTHEAST AGRICULTURAL UNIVERSITY

Method for detecting content of alpha-homonojirimycin in suregade glomerulata medicinal materials

ActiveCN108828121AStrong alpha-glucosidase inhibitory activityIncrease contentComponent separationAcetonitrileChloroform
The invention relates to the field of traditional Chinese medicine content detection, in particular to a method for detecting content of alpha-homonojirimycin in suregade glomerulata medicinal materials. According to the method, alpha-homonojirimycin is taken as a control, acyl chloride derivatization reagents are used for precolumn derivatization of alpha-homonojirimycin, dichloromethane or chloroform is added to accelerate the reaction, an AgilentExtendC18 chromatographic column is used as the chromatographic column, and the mixture of methanol, acetonitrile and water is used as the mobile phase, and separating determination and quantitative analysis of alpha-homonojirimycin is conducted with high performance liquid chromatography. The detection method for the suregade glomerulata medicinal materials is quick, accurate and convenient.
Owner:CHINA RESOURCES SANJIU MEDICAL & PHARMA +1

Method for extracting and analyzing trivalent chromium and hexavalent chromium in water sediments

The invention belongs to the technical field of heavy metal detection and discloses a method for extracting and analyzing trivalent chromium and hexavalent chromium in water sediments. The method comprises steps of sampling, sample pretreatment, ion exchange state chromium test sample preparation, carbonate combined state chromium test sample preparation, trivalent chromium and hexavalent chromiumdetermination and the like. The method is advantaged in that a pre-column derivatization mode is adopted, Cr(III) and Cr(VI) in the test sample are directly extracted by using EDTA-2Na aqueous solution, complexation reaction of Cr (III) and EDTA-2Na occurs at a certain temperature, then a Hamilton PRP-X100 anion exchange chromatographic column is selected to separate Cr (III) and Cr (VI) baselines, and 52Cr is determined by ICP-MS (Inductively Coupled Plasma Mass Spectrometry), and thereby quantitative analysis of Cr (III) and Cr (VI) in a water sample is realized, pretreatment operation of the sample is simple, convenient and rapid, Cr (III) and Cr (VI) are separated and determined within 6 minutes, requirements of chromium form detection and analysis can be met, and method support is provided for guaranteeing the quality safety of aquatic products and researching a chromium pollution remediation technology.
Owner:MARINE FISHERIES RES INST OF ZHEJIANG
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