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LC (liquid chromatogram)-MS/MS(mass spectrometry/mass spectrometry)method for synchronously detecting 21 fungal toxins in grains

A technology of mycotoxins and tandem mass spectrometry, applied in the field of liquid chromatography-tandem mass spectrometry, can solve the problems of immaturity and achieve the effect of simple operation and strong qualitative and quantitative ability.

Active Publication Date: 2018-12-14
INSPECTION & QUARANTINE TECH CENT SHANDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there are many types of QuEChERS products for pesticide residues on the market. The QuEChERS technology for pesticide residues is quite mature, but the QuEChERS technology for the detection of mycotoxins is not mature enough. The selection of adsorbents suitable for mycotoxin purification is the key to the development of mycotoxin QuEChERS technology. The essential

Method used

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  • LC (liquid chromatogram)-MS/MS(mass spectrometry/mass spectrometry)method for synchronously detecting 21 fungal toxins in grains
  • LC (liquid chromatogram)-MS/MS(mass spectrometry/mass spectrometry)method for synchronously detecting 21 fungal toxins in grains
  • LC (liquid chromatogram)-MS/MS(mass spectrometry/mass spectrometry)method for synchronously detecting 21 fungal toxins in grains

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] The detection method of 21 kinds of mycotoxins provided by the present embodiment comprises the following steps:

[0053] (1) Sample pretreatment

[0054] (i) Extraction: Accurately weigh 2.0 g of the sample, add 10 mL of acetonitrile solution containing 1% acetic acid, homogenize for 2 min, and centrifuge at 10,000 rpm for 5 min.

[0055] (ii) Purification: Take 2 mL of the supernatant after centrifugation in the previous step, add 1 mg of multi-walled carbon nanotubes, vortex for 1 min, and centrifuge again at 10,000 rpm for 5 min, take 1 mL of the supernatant and pass it through a 0.22 μm filter membrane to prepare for high performance liquid phase Chromatography-tandem mass spectrometry injection.

[0056] (2) LC-MS / MS detection

[0057] Liquid phase conditions

[0058] Agilent Zobax SB-C18, (4.6mm×150mm, 5μm), injection volume 20μL; mobile phase A is water, B is acetonitrile; gradient elution; gradient elution conditions are as follows:

[0059] Liquid Chromato...

Embodiment 2

[0081] Embodiment 2 recovery rate experiment

[0082] (1) Sample addition:

[0083] Take blank wheat, rice and corn samples respectively for three levels of addition, the addition levels are shown in the table, and 6 parallels are made for each level.

[0084]

[0085]

[0086] (2) Sample pretreatment

[0087] Extraction: Accurately weigh 2.0 g of the sample, add 10 mL of acetonitrile solution containing 1% acetic acid, homogenize for 2 min, and centrifuge at 10,000 rpm for 5 min.

[0088] Purification: Take 2 mL of the supernatant after centrifugation in the previous step, add 1 mg of multi-walled carbon nanotubes, vortex for 1 min, and centrifuge again at 10,000 rpm for 5 min, take 1 mL of the supernatant and pass it through a 0.22 μm filter membrane to prepare HPLC-tandem Mass spectrometry injection.

[0089] (3) Liquid chromatography-tandem mass spectrometry detection

[0090] The conditions of liquid chromatography and mass spectrometry refer to Examples 1 and 2...

Embodiment 5

[0094] One portion of rice and one portion of corn were randomly purchased in the market, and this method was used to detect various mycotoxins in the samples.

[0095] (2) Sample pretreatment

[0096] Accurately weigh 2.0 g of the sample, add 10 mL of acetonitrile solution containing 1% acetic acid, homogenize for 2 min, and centrifuge at 10,000 rpm for 5 min. Take 2 mL of the supernatant, add 1 mg of multi-walled carbon nanotubes, vortex for 1 min, and centrifuge again at 10,000 rpm for 5 min, take 1 mL of the supernatant and pass it through a 0.22 μm filter membrane to prepare for high performance liquid chromatography-tandem mass spectrometry injection.

[0097] (3) Liquid chromatography-tandem mass spectrometry detection

[0098] The conditions of liquid chromatography and mass spectrometry refer to Examples 1 and 2, respectively.

[0099] (4) Experimental results

[0100] The results showed that no mycotoxins were detected in rice, and zearalenone and deoxynivalenol w...

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Abstract

The invention discloses an LC (liquid chromatogram)-MS / MS(mass spectrometry / mass spectrometry) method for synchronously detecting 21 fungal toxins in grains. The method comprises the following steps:(1) pre-treatment of a sample; (2) purification; and (3) LC-MS / MS detection. The method is simple and convenient in operation and accurate in qualitative and quantitative analysis, and therefore, themethod can be taken as a reliable method for detecting various fungal toxins in the grains.

Description

technical field [0001] The invention relates to a liquid chromatography-tandem mass spectrometry method for simultaneously detecting 21 kinds of mycotoxins in grains, belonging to the technical field of instrument detection. Background technique [0002] Mycotoxins are a class of toxic secondary metabolites produced by fungi. Plant products such as crops, food and feed are widely polluted. At present, there are more than 300 kinds known, of which a considerable part has strong carcinogenicity and teratogenicity, and can be divided into aspergillus toxins (such as aflatoxin, ochratoxin, etc.), penicillin Mycotoxins (such as patulin, citrinin, etc.), fusarium toxins (such as ochratoxin A, zearalenone, etc.) and other types (such as spores, etc.). The contamination of mycotoxins in food is inevitable, and some food poisoning, chronic diseases and cancers are all related to mycotoxins. In warm and dry climates, aflatoxins are often produced in corn and peanuts; in low-tempera...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 静平罗忻吴振兴张鸿伟张晓梅梁君妮许艳丽
Owner INSPECTION & QUARANTINE TECH CENT SHANDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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