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Method for efficient detection of neonicotinoid insecticides in honey

A neonicotinoid and detection method technology, applied in the detection field, can solve the problems affecting the pollination and survival of honeybees, no high-resolution mass spectrometry, long residual period, etc., so as to improve detection accuracy and reliability, good repeatability, The effect of a high degree of automation

Active Publication Date: 2016-10-26
ANIMAL AND PLANT & FOOD DETECTION CENTER JIANGSU ENTRY EXIT INSPECTION AND QUARANTINE BUREAU
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Problems solved by technology

This type of insecticide has a quick effect and a long residual period, which may seriously affect the pollination and survival of bees. The European Union, the United States, Canada, Brazil and my country have successively launched the review and restriction of neonicotinoid insecticides
At present, the pretreatment methods for the determination of neonicotinoid insecticides in honey are mostly manual solid-phase extraction, which consumes more manpower and has poor repeatability, while online solid-phase extraction saves manpower and has good repeatability; the instrument method is mostly high-efficiency liquid Phase chromatography tandem triple quadrupole mass spectrometry, no high-resolution mass spectrometry, especially the application of electrostatic field orbitrap high-resolution mass spectrometry in the determination of neonicotinoid insecticides in honey

Method used

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  • Method for efficient detection of neonicotinoid insecticides in honey
  • Method for efficient detection of neonicotinoid insecticides in honey
  • Method for efficient detection of neonicotinoid insecticides in honey

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Embodiment

[0021] Example: An efficient method for detecting neonicotinoid insecticides in honey, including the following steps:

[0022] (1) Standard solution preparation: The neonicotinoid standard drug is formulated into a standard solution with a concentration of 1 mg / mL with methanol, and stored at 4°C; then it is gradually diluted with methanol to a standard solution with a concentration of 1 μg / mL;

[0023] (2) Treatment of the sample to be tested: stir evenly the honey sample to be tested, weigh 1g and place it in a 50mL centrifuge tube, add 15mL of phosphate buffer with pH 7.8, vortex to fully dissolve it evenly; place in a sonicator Ultrasound for 20min; filter, take the filtrate to the injection vial;

[0024] (3) On-line solid phase extraction: use HLB extraction column, activate with 1mL methanol and 1mL water respectively, with a flow rate of 5mL / min; then inject the sample with 0.5ml sample volume and 0.5ml water as the sample solvent , The flow rate is 0.5mL / min; the cleaning s...

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Abstract

The invention discloses a method for efficient detection of neonicotinoid insecticides in honey. The method includes steps: (1) standard solution preparation; (2) to-be-detected sample treatment; (3) online solid-phase extraction; (4) high performance liquid chromatography and electrostatic field orbitrap high-resolution mass spectrometric determination. By combination of a high-efficiency high-repeatability online solid-phase extraction method and high performance liquid chromatography and electrostatic field orbitrap high-resolution mass spectrometric determination for detection of the neonicotinoid insecticides in honey, qualitative and quantitative determination of the neonicotinoid insecticides in samples can be realized, and detection results are sensitive and reliable; by adoption of the method, a sample pretreatment process is quick, simple and convenient, and operation efficiency is improved; due to appropriate selection of an extraction solvent, a cleaning agent, an eluent and mass spectrometric detection parameters according to characteristics of the neonicotinoid insecticides, precision and reliability in detection are improved.

Description

Technical field [0001] The invention belongs to the technical field of detection, relates to a detection method of neonicotinoid insecticides in honey, and specifically relates to an online solid phase extraction-high performance liquid chromatography series electrostatic field orbitrap high-performance liquid chromatography of neonicotinoid insecticides in honey Resolution mass spectrometry method. Background technique [0002] Neonicotinoid insecticides include: imidacloprid, clothianidin, acetamiprid, flonicamid, thiamethoxam, thiacloprid, dinotefuran, nitenpyram, etc. Such pesticides can be widely used in various crops, such as rice, wheat, cotton, beans, rape, sesame, potatoes, tomatoes and so on. Can kill piercing and sucking mouthparts, Coleoptera, Lepidoptera, Diptera, etc. in a broad spectrum. This type of insecticide has a quick effect and a long residual period, which may seriously affect the pollination and survival of bees. The European Union, the United States, Ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/06G01N30/88
Inventor 张睿柳菡沈伟健丁涛赵增运吴斌沈崇钰张晓燕陈磊费晓庆刘芸
Owner ANIMAL AND PLANT & FOOD DETECTION CENTER JIANGSU ENTRY EXIT INSPECTION AND QUARANTINE BUREAU
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