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Method for rapidly detecting chlorpyrifos in honey by using neutral desorption-extractive electrospray ionization mass spectrometry

A neutral desorption and honey poisoning technology, applied in the field of detection, can solve the problems of complicated operation steps, inconvenient and time-consuming detection of chlorpyrifos, etc., and achieves the effects of high desorption efficiency, improved strength, and avoidance of false positives.

Active Publication Date: 2015-09-09
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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  • Method for rapidly detecting chlorpyrifos in honey by using neutral desorption-extractive electrospray ionization mass spectrometry
  • Method for rapidly detecting chlorpyrifos in honey by using neutral desorption-extractive electrospray ionization mass spectrometry
  • Method for rapidly detecting chlorpyrifos in honey by using neutral desorption-extractive electrospray ionization mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] This experiment uses figure 1 The ND-EESI-MS method shown 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, prepare a chlorpyrifos standard solution with a concentration of 2mg / mL, and store it at -3°C in the dark. Take 100μL of 2mg / mL chlorpyrifos standard solution, dilute to 4mL with ultrapure water, the concentration is 50μg / mL.

[0029] (2) Add standard honey chlorpyrifos solution: place the graduated cylinder on the analytical balance, remove the skin to zero, accurately measure 9.9mL of honey with the graduated cylinder, and weigh it to be 13.96232g. Then put each 10mL Erlenmeyer flask on the analytical balance, peeled to zero, and weighed 13.96g honey. After weighing, seal the 65°C water bath with plastic wrap for 5 minutes, measure 100μL of 50μg / mL diluent into each conical flask containing honey, and stir well. After th...

Embodiment 2

[0036] A method for the direct detection of chlorpyrifos in honey by neutral desorption-electrospray extraction ionization mass spectrometry, including the following steps:

[0037] (1) Preparation of spiked honey: Weigh the honey to be tested and set aside;

[0038] Preparation of spiked honey: Weigh several portions of non-chlorpyrifos honey equal to the weight of the sample honey to be tested, add a gradient concentration of chlorpyrifos solution, stir evenly to form spiked honey, and set aside;

[0039] Seal the honey sample and the spiked honey with plastic wrap in a 65°C water bath for 5 minutes; wait until the honey is cooled to room temperature for 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 voltage 3.5kV; ion transfer tube temp...

Embodiment 3

[0046] (1) Weigh 13.96g of commercially available honey into a 10mL conical flask, seal with a plastic wrap in a 65°C water bath for 5 minutes; wait until the honey is cooled to room temperature, and then perform testing;

[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; use methanol: water volume ratio 1:1 as the medium Desorption spray reagent; ionization voltage 3.5kV; ion transfer tube temperature is 300℃; atomizing gas is nitrogen, pressure is 1.0MPa; extractant formic acid: methanol: water volume ratio 1:2:2, flow rate is 4μL / min;

[0048] In the collision-induced dissociation experiment, the chlorpyrifos precursor ion m / z 352 width is set to 1.2Da, the collision energy is 30%, and the collision duration is 30ms; the secondary m / z 324 ion width is set to 1.4Da, and the collision energy is 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 using neutral desorption-extractive electrospray ionization mass spectrometry. The method comprises the following steps: (1) preparing labeled honey; (2) detecting selection of a chlorpyrifos extraction agent and a neutral desorption agent by using neutral desorption-extractive electrospray ionization mass spectrometry; and (3) selecting three-level characteristic fragment ions m / z296 of m / z352 to perform quantitative analysis, thereby obtaining the amount of chlorpyrifos in honey. According to the method disclosed by the invention, a to-be-detected sample does not need to be pretreated, the chlorpyrifos in honey is rapidly detected and identified, and the defects such as complex operating steps and high time consumption in the existing analysis technology are improved.

Description

Technical field [0001] The invention belongs to the technical field of detection, and particularly relates to a detection method of chlorpyrifos in honey. Background technique [0002] Chlorpyrifos is a widely used high-efficiency broad-spectrum organophosphorus pesticide. It can kill mites and act as a sanitary insecticide. It is mainly used for the prevention and control of various crops such as vegetables, fruit trees and cotton, but it is a greater threat to nectar plants. . Toxicological studies have shown that chlorpyrifos has a significant inhibitory effect on cholinesterase activity, is toxic to the central nervous system of mice, and has a certain teratogenic effect. The analysis and research on the residues of organophosphorus pesticides in honey show that the phenomenon of excessive chlorpyrifos residues in honey is widespread. China is the world's largest beekeeping country, and also a major producer and exporter of bee products. With the improvement of people’s li...

Claims

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Application Information

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Patent Type & Authority Applications(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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