Method for determining residue of triazine pesticide in tea by dispersive liquid-liquid micro-extraction and magnetic solid-phase extraction

A technology for pesticide residues and liquid-liquid dispersion is applied in the field of liquid-liquid microextraction combined with magnetic solid-phase extraction to determine the residues of triazine pesticides in tea leaves, which can solve the problems of limited application and the like, and achieve the reduction of experimental costs, the simplicity of the method, the Environmentally friendly effect

Inactive Publication Date: 2012-10-03
HUAZHONG NORMAL UNIV
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  • Method for determining residue of triazine pesticide in tea by dispersive liquid-liquid micro-extraction and magnetic solid-phase extraction
  • Method for determining residue of triazine pesticide in tea by dispersive liquid-liquid micro-extraction and magnetic solid-phase extraction
  • Method for determining residue of triazine pesticide in tea by dispersive liquid-liquid micro-extraction and magnetic solid-phase extraction

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Embodiment Construction

[0023] This method was used for the determination of three triazine pesticide residues in tea.

[0024] Weigh 0.5 g of the sample, accurate to 0.01 g, put it in a 10 ml stoppered polypropylene centrifuge tube, add 3 ml of acetonitrile, shake fully (3 minutes), centrifuge at 4000 rpm for 5 minutes, and remove the supernatant solution to another centrifuge tube, then add 3 ml of acetonitrile to the residue, repeat the above steps, and combine the two extracts; blow to dryness with nitrogen at 40 degrees Celsius, pipette 5 ml of water and vortex for 5 minutes, add 20 μl of n-octyl Alcohol, shake for 90 seconds, then add 200 microliters of 20 mg / ml magnetic nanoparticle solution, shake for 90 seconds, so that the n-octanol droplets are adsorbed to the surface of the nanoparticles, and the magnetic nanoparticles are attracted to the surface of the centrifuge tube with a super strong magnet. wall while carefully removing waste with a disposable dropper. Add 50 microliters of methan...

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Abstract

The invention discloses a method for determining the residue of triazine pesticide in tea by dispersive liquid-liquid micro-extraction and magnetic solid-phase extraction. The method is a tea sample pretreatment method. The tea sample pretreatment method comprises the following steps of: putting 0.5 g of sample into a 10ml polypropylene centrifugal tube with a stopper, adding 3 ml of acetonitrile, shaking, centrifuging, moving supernatant to another centrifugal tube, adding 3 ml of acetonitrile into residue, repeatedly executing the steps, and combining extracting solutions which are obtained at two times; drying by nitrogen, moving 5 ml of water, whirling, adding 20 microliters of n-octyl alcohol, shaking, adding 200 microliters and 20 mg/ml of magnetic nano particle solution, shaking, attracting magnetic nano particles to the wall of the centrifugal tube by using a magnet, and removing effluent; and adding 50 microliters of methanol into the centrifugal tube, whirling, attracting the magnetic nano particles to the bottom of the centrifugal tube by using the magnet, taking the solution out by using a microsyringe, and performing efficient liquid chromatography-mass spectrometry analysis. The method is easy and convenient to operate, short in analysis time, low in cost, high in sensitivity and applicable to detection of pesticide residue of the tea.

Description

technical field [0001] The invention relates to a sample pretreatment method for the analysis of tea pesticide residues, which is a dispersion liquid-liquid micro-extraction combined with magnetic solid-phase extraction method, which is applied to the analysis of tea pesticide residues. Background technique [0002] Tea is a traditional drink in my country, and is widely loved by people because of its special fragrance and health-preserving effect. Tea is the main economic crop of my country's export projects. In order to increase crop yield and reduce pest damage, various insecticides and herbicides are used for prevention and control during the planting process. In recent years, many countries have continuously increased the testing items of pesticide residues in tea, and continuously lowered the detection limit of the tested substances. These are undoubtedly a huge challenge for tea exporting countries. Tea is drunk by brewing tea leaves with boiling water, but this incr...

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Application Information

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IPC IPC(8): G01N30/06G01N30/08
Inventor 徐晖张玉王帅梁璐
Owner HUAZHONG NORMAL UNIV
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