Method for quickly detecting dichlorvos in honey through ND-EESI-MS (neutral desorption-extractive electrospray ionization-mass spectrography)

A neutral desorption and dichlorvos technology, applied in the detection field, can solve the problems of cumbersome operation steps, inability to meet direct and rapid detection, time-consuming, etc., achieve high desorption efficiency, rapid detection, and avoid false positive effects

Inactive Publication Date: 2016-03-30
NANCHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These detection methods need to go through cumbersome sample pretreatment processes such as solvent extraction, solid phase extraction, and supercritical fluid extraction, which have defects such as cumbersome operation steps and time-consuming, and cannot meet the needs of direct and rapid detection.

Method used

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  • Method for quickly detecting dichlorvos in honey through ND-EESI-MS (neutral desorption-extractive electrospray ionization-mass spectrography)
  • Method for quickly detecting dichlorvos in honey through ND-EESI-MS (neutral desorption-extractive electrospray ionization-mass spectrography)
  • Method for quickly detecting dichlorvos in honey through ND-EESI-MS (neutral desorption-extractive electrospray ionization-mass spectrography)

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Experimental program
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Effect test

Embodiment 1

[0025] The mass spectrometer used in the example of the present invention is the LTQ-XL linear ion trap mass spectrometer of Finnigan Company of the United States, and the data processing system is the Xcalibur data processing system of Finnigan Company of the United States.

[0026] The neutral desorption device and EESI ion source are independently developed by the Jiangxi Provincial Key Laboratory of Mass Spectrometry Science and Instruments; the precision electronic balance (METTLERTOLEDO). Methanol (chromatographically pure, American TEDIA company); Dichlorvos standard substance (purity is 98.8%, Bailingwei Technology Co., Ltd.);

[0027] This experiment uses figure 1 The shown ND-EESI-MS method carries out experiment to dichlorvos methanol standard solution (400ng / mL), the result is as follows figure 2 shown. The dichlorvos molecule contains two chlorine atoms, and the isotopic pattern is reflected in the spectrum. In the positive ion mode, m / z221, m / z223, and m / z225 ...

Embodiment 2

[0034] Preparation of commercially available honey: Accurately measure 19.80mL of honey into 50mL conical flasks, seal with plastic wrap, and bathe in water at 45°C for 5 minutes; add 0.2mL of aqueous solution to each conical flask containing honey, stir well; wait for the honey to cool to room temperature for mass spectrometry detection;

[0035] Neutral desorption electrospray extraction ionization mass spectrometry detection: set ND-EESI-MS to positive ion detection mode, mass spectrum scanning range m / z60~300; neutral desorption spray reagent methanol: water (V / V2:3); extractant For methanol: water: formic acid (V / V2:2:1), flow rate 5μL / min; ionization voltage 3.8kV; atomization gas (nitrogen, purity 99.999%) pressure 1.2MPa; sample end auxiliary pressure 1.2MPa; The transfer tube temperature was 200°C. In the collision-induced dissociation experiment, the isolation width of the parent ion of dichlorvos is 1.1Da, the collision energy is 25%, and the collision duration is ...

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Abstract

The invention belongs to the technical field of detection and discloses a method for directly detecting dichlorvos in honey through ND-EESI-MS (neutral desorption-extractive electrospray ionization-mass spectrography). The method comprises steps as follows: (1) m / z 221, 223 and 225 ion peaks produced due to the dichlorvos C1 atom isotope effect in the mass spectrography are presented; (2) m / z 223 is selected as primary characteristic ions of the dichlorvos for splitting, and secondary ions m / z 127 are used for quantitative analysis; (3) structural analysis is performed on secondary characteristic ions m / z 109, 127, 145 and 147 of dichlorvos m / z 223; (4) a 50 mL conical flask is selected to contain 20 mL of the honey, and the condition that the honey is blown to pollute or block a pipeline during desorption is effectively prevented. According to the method, a to-be-tested sample is not required to be pretreated, the influence of complex matrixes in the honey can be borne, and the dichlorvos in the honey is directly and quickly detected.

Description

technical field [0001] The invention belongs to the technical field of detection, in particular to a detection method for dichlorvos in honey. Background technique [0002] China is the largest beekeeping country in the world, as well as a major producer and exporter of bee products. Honey is a pure natural food with high nutritional value. It contains a variety of nutrients needed by human metabolism. It also has the functions of nourishing, moisturizing, pain relief, inhibition and sterilization. However, microbial pollution, metal pollution, pesticide residues and antibiotic pollution in honey have brought great hidden dangers to the honey market and human health. Dichlorvos (Dichlorvos, DDVP) is a broad-spectrum insecticide, cheap and effective, because beekeepers abuse dichlorvos when treating bee colonies and nectar plant diseases and insect pests, resulting in excessive residues of dichlorvos in honey. With the integration of the global economy and the international...

Claims

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Application Information

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IPC IPC(8): G01N27/62
CPCG01N27/62
Inventor 罗丽萍陈焕文刘星星于腾辉方小伟罗火林郭夏丽
Owner NANCHANG UNIV
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