37 results about "Post column derivatization" patented technology

A device for performing a post-column derivatization in connection with liquid chromatography includes a separating column, a detector, an eluent withdrawal unit, connected to an outlet of the separating column, that withdraws eluents from the separating column, a reagent supply unit, arranged between the outlet of the separating column and an inlet of the detector, that supplies reagents to the eluents withdrawn from the separating column and a pump that simultaneously pumps eluents from the eluent withdrawal unit and pumps reagents to the reagent supply unit, wherein the pumping of reagents takes place free of pulsations.

The invention relates to a compound for ultraviolet-detecting anions containing sulfur by ion chromatography post-column derivatization and provides a new method for detecting anions containing sulfur. The method comprises the following steps: anions reacts with acidized iodine solution after being separated by ion chromatography; the acidized iodine solution enters a knotted reaction tube after passing through a post-column derivative device and generates oxidation-reduction reaction with the anions which contains sulfur and also enters the knotted reaction tube after flowing out of chromatography; and finally three-valent iodide ions are generated and leading the three-valent iodide ions generated finally to have the strongest ultraviolet absorption peaks by adjusting the concentration and acidity of different iodine solutions, thus greatly improving the sensitivity of detection. The invention can be applied to aminated compounds for environmental monitoring, food safety, biological medicine, health and epidemic prevention and the like.

The present invention relates to a packing material for ion chromatography, wherein a quaternary ammonium base represented by the following formula (1) is bonded to the substrate directly or through a spacer:

wherein R¹ represents a group having at least one olefinic double bond or conjugated double bond, each R² and R³ independently represents an organic residue which may be the same with or different from R¹; and separating equipment for chemical substances and a separating method using the packing material.

The packing material for ion chromatography, separating equipment for chemical substances and a separating method using the packing material of the present invention, enable to sufficiently separate seven standard inorganic anions and three halogen oxide anions in either of the conductometric detection or ultraviolet detection by postcolumn derivatization while preventing increase in the pressure and imposing no limitations on the measurement temperature or flow rate of mobile phase.

The invention discloses a liquid chromatography pre-column derivatization method for detecting glyphosate in water. The method comprises the steps as follows: S1, production of a standard curve; S2, preparation of a standard working solution; S3, preparation of a sample; S4, glyphosate derivatization; S5, online testing; S6, result determination; S7, quantitative measurement; S8, result calculation. With the adoption of the method, the glyphosate in water can be effectively detected and measured in the absence of a post-column derivatization instrument, a special detection chromatographic column and a post-column derivatization reagent, so that the laboratory cost is greatly saved, and the working efficiency is improved.

The invention discloses a preparation method of a tobacco extracting solution that is used for amino acid analysis, takes HCl solution that contains norvaline as extracting solution, extracts tobacco ashes under ultrasonic oscillation, and obtains the extracting solution by filtering. The extracting solution is combined with a coupling technique of a liquid chromatogram and an electrospray tandom mass spectrometry, thus providing a complete experimental proposal which avoids fuzzy pre-column and post-column derivatization operations of tobacco samples, obtains good chromatogram peak form and proper chromatogram running time in the experiment, further leads the isomerides Leu and Ile to reach baseline separation, and consequently obtains accurate analyzing result.

The invention relates to a method for determining contents of cystine, cysteine and salt thereof in amino acid injection. The method comprises the following steps: measuring a sample to be detected and a reference solution precisely, adding 0.1-1% of sodium pyrosulfite solution, shaking up, heating by 70-100 DEG C. for 10-60 minutes, fetching out, adding formic acid 1.5 ml and 30% superoxol 1.0 ml, shaking up, placing in 30+-2 DEG C. for 30 minutes, adding water to the scale, shaking up, fetching the sample to be tested and injecting into a chromatograph with cation exchange resin, carrying out gradient elution and regeneration balance by a special-purpose mobile phase A6 solution and a special-purpose sodium hydroxide regeneration liquid, carrying out a post-column derivatization reaction by a special-purpose derivatization reagent ninhydrin solution, recording a chromatogram with the detection wavelength 570 nm, and obtaining the contents by calculating peak areas according to external standard method. The invention has the beneficial effects that (1) short analysis time and saved detection time; (2) high sensitivity; (3) low price and saved detection cost; (4) good specialization.

The invention relates to a content detection method of an alprostadil injection. The content detection method of the alprostadil injection comprises the following steps: preparing a beta-naphthol internal standard solution; preparing beta-naphthol internal standard solutions with the same concentration from a test solution and a reference solution, then carrying out column separation on alprostadil by using a high performance liquid chromatography, taking 1 mol/L of a KOH solution as a reaction solution by using a post-column derivatization method, controlling the temperature of a reaction tank to be 60 DEG C, finally detecting alprostadil and beta-naphthol peak area on a wavelength of 278 nm, and calculating the content of alprostadil by using an internal standard method. By adopting the method provided by the invention to detect the content of the alprostadil injection, the problem of small beta-naphthol peak area in the existing method for detecting the content of the alprostadil injection is effectively solved, the detection accuracy of the content of the alprostadil injection is improved, and the content detection method of the alprostadil injection is applicable to detection of the content of the alprostadil injection in different prescriptions.

The invention discloses an online sampling analysis method of aflatoxin, which comprises the following steps: after the sample extract is filtered and diluted, the filtrate passes through an immunoaffinity column containing aflatoxin specific antibody, and the antibody is compatible with aflatoxin B1, B2 , G1, G2 have specific antigen-antibody binding, so that they are retained on the affinity column, other impurities flow out with the mobile phase, the antigen-antibody bond is broken by heating, and the target compound is eluted with water, and the eluent passes through the fully automatic fungal The toxin pretreatment and online sampling platform injects the sample into the high-performance liquid chromatograph online, and the aflatoxin is fully separated. The target compound is derivatized by a post-column derivatization system and can be detected by a fluorescence detector. Each aflatoxin can be obtained separately accurate quantification. This method breaks the antigen-antibody bond by heating, elutes the target compound with water, avoids the use of organic solvents, and is environmentally friendly; fully automatic operation not only improves the production efficiency and repeatability, but also avoids the operator from contacting the highly toxic aflatoxin Standard.

The invention belongs to the technical field of veterinary drug residue analysis, and discloses a detection and analysis method for post-column derivatization reaction of aminoglycosides compound and o-phthalaldehyde. Aminoglycosides compound reacts with o-phthalaldehyde to generate a fluorescent reagent which has unique excitation wavelength and unique emission wavelength. For the optimization selection of the reaction conditions, the result shows that under the alkali condition, aminoglycosides can react easily and quickly with o-phthalaldehyde, so that the reaction is suitable for the post-column derivatization; a derivatization product has the strongest fluorescence intensity at the lambda ex value of 235 nm and lambda em value of 465 nm; the minimum detectable amount is 10 microgram/L with good reproducibility; the variable coefficient of 4 concentrations and 5 independent repetitions is smaller than 15%, so that each index of the method can satisfy the requirements for the residue analysis of aminoglycosides antibiotics, and the sensitivity is greatly increased.

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.

The present invention provides an ion chromatography-fluorescence method for detection of sexavalence chromium in the technical field of chemical detection. The detection method comprises the following steps: (A1)sampling a sample solution and a standard solution; (A2) separating sexavalence chromium in the sample solution and standard solution by ion chromatography column; (A3) by a post-column derivatization system, reacting sexavalence chromium after separation with a fluorescence derivatization reagent for fluorescence derivatization; (A4) detecting the peak area of the derivative fluorescence intensity by a fluorescence detector; (A5) conducting linear fitting on the peak area of the derivative fluorescence intensity in the standard solution with content of sexavalence chromium to obtain a standard curve of the relationship between the peak area and sexavalence chromium content; and (A6) determine the content of sexavalence chromium in the sample solution by the standard curve using the peak area of derivative fluorescence intensity in the sample solution. The invention can effectively analyze the content of the sexavalence chromium content in the samples, such as water or toy, the detection sensitivity is high, and the cost is low.

The invention belongs to the field of biomedicine and particularly relates to a method for measuring content of arginine in an rhTNK-tPA (recombinant human TNK tissue-type plasminogen activator) withHPLC (high performance liquid chromatography). In terms of chromatographic conditions, chromatographic column adopts C8 column; for a mobile phase, the ratio of a 0.05 mol/L phosphate buffer solutionto acetonitrile is (20-60):(30-80); detection wavelength is 200-220 mm; column temperature is 30-35 DEG C; flow rate is 1.0 ml/min; sample size is 10 mu l. The method is particularly applicable to measurement of content of arginine in the rhTNK-tPA, pre-column/post-column derivatization is not needed, the method has the characteristics of high accuracy, high precision, good repeatability, wide linear range and the like, one scientific and strict inner quality standard is set for the rhTNK-tPA product, and quality of the rhTNK-tPA product is improved.

The invention discloses a method for detecting gamma-aminobutyric acid in cosmetics, and the method comprises the following steps: preparation of a reference substance: dissolving the gamma-aminobutyric acid reference substance with hydrochloric acid, and filtering to obtain a reference substance solution of gamma-aminobutyric acid; preparation of a test sample: dissolving the cosmetic test sample with hydrochloric acid, and filtering to obtain a test sample solution; preparation of a blank solution: filtering hydrochloric acid to obtain the blank solution; and measurement: detecting the reference solution, the test solution and the blank solution by using a separation column and a post-column derivatization reaction column so as to obtain the content of gamma-aminobutyric acid in the cosmetic test. The detection method is simple to operate, sensitive in response, high in accuracy and good in repeatability, and can be used for detecting the content of gamma-aminobutyric acid in cosmetics.

The invention discloses a method for determining silicate and phosphate ions with an ion chromatography post-column derivatization method. The method comprises the steps that a water solution of a sample to be determined is diluted to a certain multiple times firstly and then the solution is sampled; after the solution is separated and eluted by an anion exchange chromatography column, the separated and diluted solution is derived by an acidified sodium molybdate solution and reduced by ascorbic acid, a product is strongly absorbed in a near infrared region, so that the silicate and phosphate ions are subjected to separated detection; the concentration and the acidity of a post-column derivatization reagent and a reductant are adjusted before determination, so that a derivative compound has the concentration with maximum absorption value, and further high limit of detection and accuracy can be obtained. According to the method, a conventional anion exchange analytical column is used for separating two ions; compared with other reported separation methods, an ion exchange chromatography has higher separation capability and is usually applied to separating ions with similar properties, and therefore, the ion exchange chromatography can be applied to separating the silicate and phosphate ions in complex matrix systems; the method has high application prospects and values.

The invention relates to the field of biological analysis, in particular to a method for simultaneously detecting alpha-ketoglutaric acid and L-glutamic acid in an enzymatic reaction liquid. A high performance liquid chromatography method is adopted, the enzymatic reaction liquid is injected into a high performance liquid chromatograph, a C18 column is adopted for separation, and an ultraviolet absorption detector is adopted for detection. The content of alpha-ketoglutaric acid and the content of L-glutamic acid in the enzymatic reaction liquid are detected at the same time, reliable data support can be provided for real-time monitoring of alpha-ketoglutaric acid production, pre-column or post-column derivatization treatment is not needed for sample detection, the detection time is greatly shortened, and the detection result is more accurate.

The invention discloses a method for monitoring separation and purification processes of etimicin hydrolysate, which comprises the following steps of sampling the etimicin hydrolysate and eluent purified on a column, detecting by an HPLC-post-column derivatization method, separating a sample to be detected by an HPLC chromatographic column, performing derivatization reaction after separation, and detecting the obtained derivative in a fluorescence detector, wherein the excitation wavelength of the fluorescence detector is 310-350 nm, and the emission wavelength of the fluorescence detector is 440-480 nm. By adopting the method provided by the invention, the purity of the etimicin hydrolysate and the column purification eluent and the content of each impurity can be detected on line by using a conventional detector and a high performance liquid chromatograph, the separation and purification process of the etimicin hydrolysate is monitored, and the method is simple, convenient, feasible, accurate, reliable and good in repeatability.

The invention discloses a method for detecting gentamicin C1a serving as a starting material of etimicin, which adopts a post-column derivatization method and comprises the following steps: separating a to-be-detected sample containing gentamicin C1a through an HPLC (High Performance Liquid Chromatography) chromatographic column, carrying out derivatization reaction after separation, and detecting the obtained derivative in an ultraviolet-visible light detector; wherein the chromatographic conditions are as follows: a mobile phase A is methanol or acetonitrile, and a mobile phase B is 0.01-0.03 M trifluoroacetic acid; the volume ratio of the mobile phase A to the mobile phase B is (35-5): (65-95), and the flow velocity is 0.5-1.0 mL/min; the derivatization reagent is an o-phthalaldehyde solution, the flow velocity of the derivatization reagent is 0.5-1.0 mL/min, and the derivatization reaction temperature is 40-70 DEG C. The detection method is rapid and accurate, and the purity and content of gentamicin C1a in a sample can be detected on line by using a conventional ultraviolet-visible light detector and a high performance liquid chromatograph.

The invention relates to the field of biological analysis, in particular to a method for detecting the content of citrulline in a citrulline raw material. According to the method, a high performance liquid chromatography method is adopted, a solution of the citrulline raw material is injected into a high performance liquid chromatograph, C18 column separation is adopted, and an ultraviolet absorption detector is adopted for detection. Pre-column or post-column derivatization treatment does not need to be carried out on a detection sample, so that the detection time is greatly shortened, and the detection result is more accurate. The used chromatographic column is a common C18 column, the detector is an ultraviolet detector, the chromatographic condition is simple, the detection cost is low, the operation is simple and convenient, and the method is suitable for large-scale popularization and application.

The invention discloses a high performance liquid chromatography method for analyzing benzoyl peroxide in toothpaste. The method belongs to the technical field of analysis. The method comprises stepsof separating samples by high performance liquid chromatography; performing a derivatization process on the benzoyl peroxide by online post-column derivatization technology; detecting a blank sample,a sample solution and a standard curve solution by a fluorescence detector, wherein the blank sample, the standard curve, a specimen, the specimen, and the standard curve are successively detected (notice: the number of introductions of the specimen between two standard curves should not exceed 15, and if the number of introductions of the specimen is more than 15, a quality control sample or a standard curve should be added). The method can quickly accurately, and quantitatively analyze the benzoyl peroxide in toothpaste samples, can be used by a market supervision department to monitor the quality of toothpaste products on the market, has accurate detection results and is reliable.

The invention discloses a tobramycin raw material and related preparation impurity spectrum analysis method. A post-column derivatization-high performance liquid chromatography fluorescence detectionmethod is adopted. The analysis method disclosed by the invention adopts a post-column derivatization-high performance liquid chromatography fluorescence detection (HPLC-FLD) method, has the advantages of high reaction speed, no interference of a derivatization reagent on measurement and the like, can effectively separate process impurities and degraded impurities through screening and optimization of chromatographic conditions, and is relatively high in sensitivity at the same time, analyzes on samples with complex matrixes, such as suspension type eye drops and eye cream, proves that the method is good in specificity and high in generalizability.