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Method for detecting amine harmful substances in food

A detection method and a technology of hazardous substances, which are applied in the field of agricultural product quality and safety detection, can solve problems such as ineffective removal, achieve good selectivity and specificity, high sensitivity, and overcome interference

Inactive Publication Date: 2020-11-27
GUANGDONG UNIV OF PETROCHEMICAL TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in the actual detection process, it was found that QuEChERS technology still cannot effectively remove caffeoylquinic acid, chlorogenic acid and other acidic substances and negatively charged impurities such as melanoidin in the food matrix.

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  • Method for detecting amine harmful substances in food
  • Method for detecting amine harmful substances in food
  • Method for detecting amine harmful substances in food

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Embodiment 1: Determination of mass spectrometry conditions

[0043] According to the structural characteristics of acrylamide and heterocyclic amine compounds, select the positive ion mode; use the peristaltic pump to directly inject the sample, respectively, for the single standard solution of acrylamide and its isotope internal standard, heterocyclic amine compound and its isotope internal standard Perform a full scan to obtain the molecular ion peak [M+H] of each compound + ; Then carry out the full scan of the secondary mass spectrometry on the molecular ions, and find that the cracking laws of various amine compounds are similar; each compound selects 2-3 main characteristic fragment ions as qualitative and quantitative ions, and optimizes the collision voltage and declustering voltage etc. to maximize the characteristic fragment ion intensity, the optimized mass spectrometry conditions are shown in Table 1.

[0044] Table 1 Abbreviations of amine hazards and the...

Embodiment 2

[0047] Embodiment 2: the determination of chromatographic conditions

[0048] In this experiment, the separation effect of Phenomenex Kinetex C18 column (2.6μm, 2.1mm×100mm) and AcquityUPLC BEH C18 column (1.7μm, 100mm×2.1mm) was compared. The results show that the retention time of the highly polar small molecule acrylamide on the BEH C18 chromatographic column is shorter than that of the Kinetex C18 chromatographic column, and is more easily interfered by the polar impurities flowing out in the early stage, so the detection method in the present invention is preferably Phenomenex Kinetex C18 column.

[0049] Under the ESI+ mode, the present invention also studies the influence of different acetic acid concentrations (0.02%, 0.04%, 0.06%, 0.1%, 0.2% acetic acid, volume percent) on the separation effect of the analyte in the ammonium acetate solution containing acetic acid, and it is found that When the volume percentage of acetic acid in the ammonium acetate solution is 0.04...

Embodiment 3

[0052] Embodiment 3: the optimization of purification condition

[0053] This experiment first tried to dissolve the sample with water to investigate the liquid-liquid extraction effect of acetonitrile (NaCl salting out). It was found that although acetonitrile can effectively precipitate the protein in the sample matrix, the target substances are not easily distributed in the acetonitrile layer, and the extraction recovery rate is very low. Then, the extraction effect of different proportions of acetonitrile aqueous solution (the sample was first dissolved in water, and then acetonitrile was added, so that the volume percentage of acetonitrile was respectively 90%, 80%, 75% and 50%) was observed, and it was found that the volume percentage was 75% The precipitation effect of the above acetonitrile aqueous solution is better, and the acetonitrile-water extract is yellowish brown, slightly viscous, severely inhibited by the matrix, and the extraction recovery rate is about 84% ...

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Abstract

The invention discloses a method for detecting amine harmful substances in food. The detection method comprises the following steps: (1) adding a dispersed adsorbent into a sample, uniformly performing mixing, adding an acrylamide isotope internal standard and a heterocyclic amine compound isotope internal standard, carrying out ultrasonic extraction and centrifugal separation by adopting an acetonitrile aqueous solution, taking supernate, blowing nitrogen to 0.5-1mL, and fixing the volume by using an ammonium acetate solution containing acetic acid to obtain a purified solution; (2), adding ferroferric oxide nanoparticles into the purified liquid, carrying out vortex oscillation decolorization and centrifugation, and taking supernatant as to-be-detected liquid; and (3), detecting the amine harmful substances in the to-be-detected liquid by using an ultra-high performance liquid chromatography-tandem mass spectrometry method. The method has the advantages of excellent purification effect, high sensitivity and strong specificity, and is suitable for simultaneous determination of a plurality of amine harmful substances in food.

Description

technical field [0001] The invention relates to the technical field of agricultural product quality and safety detection, in particular to a detection method for amine hazards in food. Background technique [0002] Food components are complex. During thermal processing, the reducing sugars and amino acids or proteins undergo reactions such as Maillard reaction and caramelization reaction. In addition to a series of flavor substances, these reactions also produce small molecule ketones, Aldehydes and heterocyclic compounds, among which amine compounds such as acrylamide and heterocyclic amines have carcinogenic and mutagenic effects, and eating foods containing too many amine hazards will cause harm to human health. Therefore, it is imperative to carry out high-throughput detection research on amine hazards in food. [0003] At present, the detection methods of amine hazards in food mainly include gas chromatography, gas chromatography-mass spectrometry, high performance liq...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72
CPCG01N30/02G01N30/06G01N30/72G01N2030/045
Inventor 张玲董浩李春海陈淇刘忆思
Owner GUANGDONG UNIV OF PETROCHEMICAL TECH
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