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Method for detecting melamine and cyanuric acid in carbon [<13>C]-urea

A detection method, melamine technology, applied in the field of chemical analysis, can solve the problems of poor accuracy of melamine and cyanuric acid, shortened life of chromatographic columns, etc.

Active Publication Date: 2021-03-09
JIANGSU HUAGEN TAILAI BIOTECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the chromatographic detection of melamine and cyanuric acid is mainly concentrated in milk, plasma and stones. Due to the differences in the components of the system to be tested, the above existing methods are directly applied to detect carbon[ 13 C]- The accuracy of melamine and cyanuric acid in urea is poor, and it is easy to shorten the life of the chromatographic column

Method used

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  • Method for detecting melamine and cyanuric acid in carbon [&lt;13&gt;C]-urea
  • Method for detecting melamine and cyanuric acid in carbon [&lt;13&gt;C]-urea
  • Method for detecting melamine and cyanuric acid in carbon [&lt;13&gt;C]-urea

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] carbon[ 13 C]-Detection of melamine and cyanuric acid in urea

[0051] Instrument: Shimadzu high performance liquid chromatography;

[0052] Chromatographic column: Agilent Zorbax SB-Aq (4.6×250mm, 5μm);

[0053] Mobile phase A: phosphate buffer solution (10mmol / L potassium dihydrogen phosphate solution, adjust pH to 7.5 with dipotassium hydrogen phosphate);

[0054] Mobile phase B: Methanol;

[0055] Detection wavelength: 200nm;

[0056] Flow rate: 1.0mL / min;

[0057] Injection volume: 10μL;

[0058] Column temperature: 30°C;

[0059] Diluent: phosphate buffer solution (10mmol / L potassium dihydrogen phosphate solution, adjust pH to 7.5 with dipotassium hydrogen phosphate);

[0060] The elution program is shown in Table 1:

[0061] Table 1 Elution program

[0062] time (min) Phosphate buffer solution ratio (%) Methanol ratio (%) 0 100 0 2 100 0 3 80 20 16 80 20 17 100 0 25 100 0

[0063] Need testing soluti...

Embodiment 2

[0081] System suitability and specificity testing of detection methods

[0082] 1. Solution preparation

[0083] (1) Blank solution: the same diluent [10mmol / L potassium dihydrogen phosphate buffer solution (adjust the pH to 7.5 with anhydrous dipotassium hydrogen phosphate)].

[0084] (2) System suitability solution: Accurately weigh 10 mg of melamine and cyanuric acid respectively, put them in different 100ml measuring bottles, add diluent to dissolve and dilute to the mark, shake well, and use them as melamine and cyanuric acid stock solution respectively Measure respectively 1 mL of melamine and cyanuric acid stock solution in a 10 mL measuring bottle, add 100 mg of carbon [ 13 C]-urea, add a diluent to dissolve and dilute to the mark, shake well, and obtain the system suitability solution.

[0085] (3) Melamine and cyanuric acid reference substance solution: Accurately measure 1 mL of melamine stock solution and 1 mL of cyanuric acid stock solution into 10 mL measuring bo...

Embodiment 3

[0095] Quantitation limit and detection limit detection method

[0096] Limits of quantitation (LOQ) and limits of detection (LOD) were determined by the signal-to-noise ratio method. The melamine of embodiment 2 known concentration and cyanuric acid reference substance stock solution are diluted step by step, detect according to embodiment 1 chromatographic conditions, the signal that measures is compared with baseline noise, and when signal-to-noise ratio is 10:1, it is Limit of quantification, detection limit when the signal-to-noise ratio is 3:1, the results are shown in Table 4:

[0097] Table 4 Quantitative limit and detection limit detection result

[0098]

[0099] Note: The percentage equivalent to the concentration of the test substance is the ratio of the quantitative limit concentration or detection limit concentration of melamine and cyanuric acid (divided by) the concentration of the test substance.

[0100] Can know by table 4: the melamine more than 0.0006...

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Abstract

The invention belongs to the field of chemical analysis, and particularly relates to a method for detecting melamine and cyanuric acid in carbon [<13>C]-urea. The method comprises the following steps:a) mixing a carbon [<13>C]-urea sample with a diluent to obtain a test solution, wherein the diluent is a phosphate buffer solution; b) performing liquid chromatographic detection on the test solution to obtain a chromatogram of the test solution, wherein in the process of chromatographic detection, a filler in an adopted chromatographic column is hydrophilic siloxane-bonded silica gel, an adopted mobile phase is composed of a phosphate buffer solution and methanol, and an adopted elution mode is gradient elution; and c) acquiring the detection results of melamine and cyanuric acid in the sample according to the appearance conditions of characteristic peaks corresponding to melamine and cyanuric acid in the chromatogram. The method provided by the invention is suitable for qualitative andquantitative detection and analysis of melamine and cyanuric acid in the carbon [<13>C]-urea product, and is high in accuracy and good in repeatability.

Description

technical field [0001] The invention belongs to the field of chemical analysis, in particular to a carbon [ 13 C] - Determination method of melamine and cyanuric acid in urea. Background technique [0002] carbon[ 13 C]-urea, used in the preparation of carbon[ 13 C]-Urea breath test diagnostic kit, which is used to diagnose whether the human body is infected with gastric Helicobacter pylori. This detection method is the internationally recognized "gold standard" for diagnosing gastric Helicobacter pylori infection. carbon[ 13 C]-urea is 13 CO is used as a raw material, prepared by chemical synthesis, and then obtained by distillation and refining to remove impurities. Melamine and cyanuric acid are carbon[ 13 C] - a by-product produced during the production of urea, in order to ensure that carbon [ 13 C]-The product quality of urea meets the requirements for use, and it is very necessary to detect whether there are melamine and cyanuric acid remaining in the product. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/32G01N30/54
CPCG01N30/02G01N30/06G01N30/34G01N30/32G01N30/54G01N2030/047G01N2030/324
Inventor 龚爱华马胜利申红红曹玲李尚伟夏秋萍
Owner JIANGSU HUAGEN TAILAI BIOTECH
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