Efficient liquid chromatography of fenazaquin residue in plant-derived foods

A high-performance liquid chromatography, plant-derived technology, applied in the field of pesticide residue analysis, can solve the problem that fenazaquin cannot be eluted, and achieve the effects of promoting import and export trade, high extraction efficiency, and high recovery rate

Inactive Publication Date: 2015-02-25
谱尼测试科技(天津)有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] (3) The above method uses n-hexane-ethyl acetate=99:1

Method used

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  • Efficient liquid chromatography of fenazaquin residue in plant-derived foods
  • Efficient liquid chromatography of fenazaquin residue in plant-derived foods
  • Efficient liquid chromatography of fenazaquin residue in plant-derived foods

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The mensuration of fenazaquin residual amount in the cucumber of embodiment 1

[0037] 1. Sample extraction: Weigh 10.0g of the prepared cucumber sample into a 50mL centrifuge tube with a cover, add 20mL of acetonitrile, shake and extract for 30min, add 5g of sodium chloride, vortex mix, centrifuge at 8000rpm for 10min, pipette Take 10 mL of the supernatant into a chicken heart bottle, rotatively evaporate in a 40°C water bath until nearly dry, dissolve the residue with 2 mL of n-hexane, and wait for purification;

[0038] 2. Purification of solid-phase extraction column: transfer the solution from the previous step to the activated florisil solid-phase extraction column (activated with 6mL n-hexane), rinse with 20mL n-hexane after loading the sample, and discard the effluent (control the flow rate not to exceed 2mL / min), then elute with 15mL of n-hexane + ethyl acetate (9+1), collect the eluate in a chicken heart bottle, and rotatively evaporate the eluate in a water b...

Embodiment 2

[0055] The mensuration of fenazaquin residual amount in the wheat of embodiment 2

[0056] 1. Sample extraction: Weigh 5.0g of the prepared wheat sample into a 50mL capped centrifuge tube, add 5mL of water, 30mL of acetonitrile, shake and extract for 30min, add 5g of sodium chloride, vortex mix, centrifuge at 8000rpm for 10min, and use Pipette 15 mL of the supernatant into a chicken heart bottle, evaporate in a 40°C water bath until nearly dry, dissolve the residue with 2 mL of n-hexane, and wait for purification;

[0057] 2. SPE column purification: same as example 1.

[0058] 3. Determination by high performance liquid chromatography: with example 1.

[0059] 4. Recovery rate:

[0060] Fenazazafen was not detected in the wheat sample. The wheat sample was used to add two standard solutions of fenazaquin with different content levels, and three parallel samples were carried out for each concentration, and the analysis was carried out according to the above chromatographic c...

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Abstract

The invention provides an efficient liquid chromatography of fenazaquin residue in plant-derived foods. A sample to be tested is subjected to oscillatory extraction via acetonitrile; extract is purified by florisil solid-phase extraction columns and separated by chromatographic columns using carbon octadecyl bonded silica gel as filler; mobile phase, mixed solvent of methyl alcohol and water, is obtained, comprising, by volume, 80-90% of the methyl alcohol and 20-10% of the water; detection wavelength is 220 nanometers; column temperature is 35 DEG C. The efficient liquid chromatography is established for the first time by means of systematic comparative study; the efficient liquid chromatography has the advantages of good separation effect, measurement accurateness, high sensitivity, high specificity, convenience and quickness in analysis and the like.

Description

Technical field: [0001] The invention relates to a method for analyzing pesticide residues, in particular to a high-performance liquid chromatography method for determining fenazaquin residues in plant-derived foods. Background technique: [0002] Fenazaquin is a quinazoline acaricide. It uses anthranilic acid as a raw material to prepare 4-hydroxyquinazoline, and then reacts with phosphorus oxychloride to obtain 4-chloroquinazoline hydrochloride. The mixture is then refluxed with 4-tert-butylphenylethanol to obtain 4-(2-(4-tert-butylphenyl)ethoxy)quinazoline hydrochloride, and this product can be obtained after neutralization. Fenazafen is mainly used on almonds (almonds), apples, citrus, cotton, grapes and ornamental plants, and can effectively prevent and control Tetranychus, Panonychus and Red Tetranychus as well as Brachycarpus purpura. The compound also has fungicidal activity. China, the European Union, Japan and the United States have not established the maximum re...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 宋薇
Owner 谱尼测试科技(天津)有限公司
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