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Rapid detection method for melamine and analogues based on x-ray diffraction

A melamine and X-ray technology, applied in the direction of material analysis, instruments, and measuring devices using wave/particle radiation, can solve problems such as low analysis efficiency, inability to detect melamine, and inability to adapt, so as to simplify detection steps and prevent production and The phenomenon of selling inferior milk powder and the effect of reducing monitoring costs

Pending Publication Date: 2022-05-13
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are also a series of problems in the inspection process: cumbersome sample pretreatment, low analysis efficiency, which is not conducive to rapid detection and screening; the use of organic solvents increases the cost of detection and sewage treatment; unstable test results lead to False negatives and false positives, etc.
The above-mentioned various detection methods cannot detect melamine and its analogs at the same time, nor can it detect melamine in a combined state, which affects the accuracy of the detection results and cannot adapt to the severe situation of food safety inspection and supervision.

Method used

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  • Rapid detection method for melamine and analogues based on x-ray diffraction
  • Rapid detection method for melamine and analogues based on x-ray diffraction
  • Rapid detection method for melamine and analogues based on x-ray diffraction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] S1. Select commercially available children's milk powder as the base, weigh 2 mg of cyanuric acid and add it to 500 mg of milk powder, grind and mix well, and set aside;

[0041] S2. Use the θ-2θ continuous scanning method, set the Guanglan system: Anti-scatter slit=1, DivergenceSlit=1 / 2, scanning angle: 10-40°, Step size: 0.02°, Time per step: 60s, scanning time About 5min;

[0042] S3. Take an appropriate amount of sample and fill it in the sample tank to press the tablet, load the sample to the sample stage of the X-ray diffractometer, and collect the diffraction information of the sample;

[0043] S4. The concentration of compound cyanuric acid in the milk powder sample is 2mg / 500mg, and the test spectrum shows 19.0°, 19.8°, 29.8° diffraction peaks, which are not owned by the matrix milk powder, and correspond to the strong characteristic peak of cyanuric acid, so as to realize the rapid detection of milk powder doped with melamine analog cyanide uric acid.

Embodiment 2

[0045] S1. Select commercially available muscle-building protein powder as the matrix, weigh 3 mg of cyanuric acid and add it to 1000 mg of protein powder, grind and mix well, and set aside;

[0046] S2. Use the θ-2θ continuous scanning method, set the Guanglan system: Anti-scatter slit=1, DivergenceSlit=1 / 2, scanning angle: 10-40°, Step size: 0.02°, Time per step: 60s, scanning time About 5min;

[0047] S3. Take an appropriate amount of sample and fill it in the sample tank to press the tablet, load the sample to the sample stage of the X-ray diffractometer, and collect the diffraction information of the sample;

[0048] S4. The concentration of cyanuric acid loaded in the milk powder sample is 3mg / 1000mg, and the test spectrum clearly shows 19.74°, 22.3° and 29.8° diffraction peaks, all of which are in non-matrix muscle-building protein powder, corresponding to the strong characteristic peak of cyanuric acid, realizing rapid detection of protein powder mixing Heteromelamine...

Embodiment 3

[0050] S1. Select commercially available milk powder as the substrate, weigh 1 mg of melamine and add it to 500 mg of milk powder, grind and mix well, and set aside;

[0051] S2. Use the θ-2θ continuous scanning method, set the Guanglan system: Anti-scatter slit=1, DivergenceSlit=1 / 2, scanning angle: 15-30°, Step size: 0.0065°, Time per step: 120s, scanning time About 20min;

[0052] S3. Take an appropriate amount of sample and fill it in the sample tank to press the tablet, load the sample to the sample stage of the X-ray diffractometer, and collect the diffraction information of the sample;

[0053] S4. The concentration of melamine loaded in the milk powder sample is 1mg / 500mg, and the test spectrum shows 20.8° and 26.16° diffraction peaks, which are not owned by the base milk powder, corresponding to the three strong characteristic peaks of melamine, and realize rapid detection of milk powder doped with melamine.

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Abstract

The invention discloses a rapid detection method for melamine and analogues based on x-ray diffraction. Comprising the following steps that an X-ray light source irradiates a to-be-detected sample and generates scattered waves, the scattered waves interfere with one another to generate strong x-ray diffraction in a specific direction, strong x-rays contain feature information of the to-be-detected sample, the strong x-rays containing the feature information of the sample are collected through an energy detector, and the collected strong x-rays contain the feature information of the to-be-detected sample; obtaining diffraction pattern data of the sample to be measured through an instrument measurement recording system; the diffractometer detector is used for analyzing and processing the strong diffraction x-ray signal to obtain a detection result of the sample to be detected. The method is simple and rapid, the to-be-detected sample is free of damage and pollution, the melamine detection step is greatly simplified, and the monitoring cost is reduced; interference of milk powder, starch, soybean milk powder and other food and dairy product matrix materials is removed, and doping of melamine and analogues thereof is stably and accurately identified.

Description

technical field [0001] The invention relates to the technical field of analysis and detection of food components, belongs to the field of detection of dairy foods with high protein content, and in particular relates to a fast detection method for melamine and similar substances based on X-ray diffraction. Background technique [0002] The addition of melamine to high-protein foods creates the illusion of high protein content, causing kidney stones in infants and public health hazards, resulting in serious food safety accidents; since 2008, similar incidents have continued to occur, which has attracted great attention and attention from all countries. Trigger social concerns about the safety of dairy products. Melamine, molecular formula C 3 h 6 N 6 , is a triazine nitrogen-containing heterocyclic organic compound, white monoclinic crystal, almost odorless, slightly soluble in water, soluble in methanol, formaldehyde, acetic acid, hot ethylene glycol, glycerin, pyridine, e...

Claims

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Application Information

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IPC IPC(8): G01N23/207
CPCG01N23/207
Inventor 石志锋郑志雯肖娟刘佳徐昕荣
Owner SOUTH CHINA UNIV OF TECH