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
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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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