Rapid detection of chlorpyrifos in honey by neutral desorption-electrospray extraction ionization mass spectrometry

A neutral desorption and honey poisoning technology, applied in the field of detection, can solve the problems of cumbersome operation steps, inconvenient and time-consuming chlorpyrifos detection, achieve high desorption efficiency, increase strength, and avoid false positive effects

Active Publication Date: 2017-11-21
江西山蜂食品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods generally require a complicated sample pretreatment process, and have the disadvantages of cumbersome and time-consuming operation steps, which bring a lot of inconvenience to the detection of chlorpyrifos in honey

Method used

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  • Rapid detection of chlorpyrifos in honey by neutral desorption-electrospray extraction ionization mass spectrometry
  • Rapid detection of chlorpyrifos in honey by neutral desorption-electrospray extraction ionization mass spectrometry
  • Rapid detection of chlorpyrifos in honey by neutral desorption-electrospray extraction ionization mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] This experiment uses figure 1 The shown ND-EESI-MS method was tested on chlorpyrifos honey solution (100ng / mL),

[0028] (1) Chlorpyrifos standard solution: Accurately weigh an appropriate amount of chlorpyrifos standard product, dissolve it in methanol, make a chlorpyrifos standard solution with a concentration of 2 mg / mL, and store it at -3°C in the dark. Take 100 μL 2mg / mL chlorpyrifos standard solution and dilute to 4 mL with ultrapure water, the concentration is 50 μg / mL.

[0029] (2) Adding standard honey chlorpyrifos solution: place the measuring cylinder on an analytical balance, peel and return to zero, accurately measure 9.9 mL of honey with the measuring cylinder, and weigh it, which is 13.96232 g. Then put each 10mL Erlenmeyer flask into an analytical balance, peel and return to zero, and weigh 13.96g of honey respectively. After weighing, seal it with plastic wrap and bathe in water at 65°C for 5 minutes, measure 100 μL of 50 μg / mL dilution solution into ...

Embodiment 2

[0036] A method for directly detecting chlorpyrifos in honey by neutral desorption-electrospray extraction ionization mass spectrometry, comprising the following steps:

[0037] (1) preparation of standard-added honey: take the sample honey to be tested and set aside;

[0038] Preparation of spiked honey: Weigh several portions of chlorpyrifos-free honey with the same weight as the sample honey to be tested, add chlorpyrifos solution with gradient concentration respectively, stir evenly, and prepare spiked honey for later use;

[0039] Seal the sample honey and the spiked honey with plastic wrap in a 65°C water bath for 5 minutes; wait for the honey to cool to room temperature before testing;

[0040] (2) Neutral desorption—electrospray extraction ionization mass spectrometry detection: set ND-EESI-MS to positive ion detection mode, and the scanning range of mass spectrometry detection is m / z 50-400; methanol aqueous solution is used as neutral desorption reagent; ionization v...

Embodiment 3

[0046] (1) Weigh 13.96g of commercially available honey into a 10mL Erlenmeyer flask, seal with plastic wrap and bathe in water at 65°C for 5 minutes; wait for the honey to cool down to room temperature, then test;

[0047] (2) Neutral desorption-electrospray extraction ionization mass spectrometry detection: set ND-EESI-MS to positive ion detection mode, and the scanning range of mass spectrometry detection is m / z 50-400; the volume ratio of methanol:water is 1:1 as the medium Desorption spray reagent; ionization voltage 3.5kV; ion transfer tube temperature 300°C; atomizing gas nitrogen, pressure 1.0MPa; extractant formic acid: methanol: water volume ratio 1:2:2, flow rate 4μL / min;

[0048] In the collision-induced dissociation experiment, the m / z 352 width of the chlorpyrifos parent ion was set to 1.2Da, the collision energy was 30%, and the collision duration was 30ms; the secondary m / z 324 ion width was set to 1.4Da, and the collision energy was 15%. The collision duration...

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Abstract

The invention belongs to the technical field of detection, and discloses a method for directly detecting chlorpyrifos in honey by neutral desorption-electrospray extraction ionization mass spectrometry, including (1) preparation of standard-added honey; (2) neutral desorption-electrospray extraction ionization mass spectrometry detection of chlorpyrifos extraction (3) Select the tertiary characteristic fragment ion m / z 296 of m / z 352 for quantitative analysis to obtain the amount of chlorpyrifos in honey. The invention does not need to pretreat the sample to be tested, realizes the rapid detection and identification of chlorpyrifos in honey, and improves the defects of the existing analysis technology such as complex operation steps and time-consuming.

Description

technical field [0001] The invention belongs to the technical field of detection, in particular to a detection method for chlorpyrifos in honey. Background technique [0002] Chlorpyrifos is a widely used high-efficiency broad-spectrum organophosphorus pesticide. It can not only kill mites, but also be used as a hygienic insecticide. It is mainly used for the control of diseases and insect pests of various crops such as vegetables, fruit trees, and cotton, but it poses a greater threat to honey plants. . Toxicological studies have shown that chlorpyrifos can significantly inhibit the activity of cholinesterase, produce toxicity to the central nervous system of mice, and have certain teratogenic effects. The analysis and research of organophosphorus pesticide residues in honey showed that the phenomenon of excessive residues of chlorpyrifos in honey was common. China is the largest beekeeping country in the world, as well as a major producer and exporter of bee products. W...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/68G01N1/28
Inventor 罗丽萍陈焕文刘星星黄学勇方小伟郭夏丽罗火林
Owner 江西山蜂食品有限公司
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