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Pretreatment method for finished tea sample for dicofol pesticide residue detection

A technology for dicofol and intermediate products, which is applied in the field of pesticide residue detection, can solve the problems of not being able to give accurate results quickly, consume too much organic solvent, and cannot be reused, and achieves the advantages of convenient washing and assembly, easy access, and cost reduction Effect

Inactive Publication Date: 2015-08-05
HUNAN AGRICULTURAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] 1. Complicated and time-consuming
The entire sample pretreatment steps include 2-3 times of solvent extraction, concentrated sample loading, purification and elution, concentration, constant volume, and detection. From the beginning of sample crushing to the end of instrument detection, the entire process takes more than 4 hours. , the steps are cumbersome, the workload is heavy, and accurate results cannot be given quickly
[0007] 2. High cost
Many of these technologies require special equipment and consumables. For example, SPE technology requires special SPE cartridges. The current market price ranges from a dozen to tens of yuan each (the type and quality of the filler determine the price), such as GB / T 23204- The Cleanert TPT used in the 2008 national standard method is generally priced at about 100 yuan / piece; and this SPE cartridge is a disposable consumable and cannot be reused; in addition, the supporting solid-phase extraction device and booster pump are required for charging. Pressure-controlled speed, generally the lowest price is more than 3,000 yuan / set, so the actual consumption cost of a sample is more than 100 yuan
[0008] 3. Toxic and harmful organic solvents are consumed more (80-120ml) in the pretreatment process, causing environmental pollution and threatening the health of personnel

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Preparation of dicofol molecularly imprinted polymer: Add 2mmol of p,p'-DDT and 8mmol of methacrylic acid to 30ml of chloroform, react at 4°C for 1 hour, then add 50mmol of ethylene glycol dimethacrylate and 240mg azobisisobutyronitrile, ultrasonically for 5 minutes to completely dissolve ethylene glycol dimethacrylate and azobisisobutyronitrile to obtain a mixed solution; then add the mixed solution dropwise to pre-dissolved 3.0g polyethylene In 120ml of aqueous solution of pyrrolidone, shake and react at 50°C for 24 hours. The obtained polymer precipitate is first passed through a nylon filter membrane with a pore size of 0.45 microns, and the filtrate is discarded. The precipitate was subjected to Soxhlet extraction, and the extraction was repeated 6 times, each time for 6 hours, and then washed with 120ml of deionized water and methanol for 15 minutes, repeated 4 times until the solution was neutral, and finally vacuum-dried at 50°C to obtain a powder. .

Embodiment 2

[0027]Grind the finished tea leaves (dry tea) to be tested, pass through a 20-mesh sieve, and make the sample to be tested for later use; take a chromatographic column (0.5-1.0 cm in inner diameter, 5-10 cm in height), and put it in the chromatographic column by Fill in 1.0 cm of absorbent cotton and 50 mg of the imprinted polymer prepared above in sequence from bottom to top; accurately weigh 0.1 g of the tea powder to be tested in a glass mortar, soak it with 0.2 ml of water for 60 minutes, add 0.1 g of the above-mentioned imprinted polymer The dicofol molecularly imprinted polymer adsorbent, mixed and fully ground for 5 minutes, moved the uniformly dispersed mixture to the above-mentioned chromatography column, and pressed 1.0 cm of absorbent cotton into the upper end of the mixture; added 2 ml of deionized water to the chromatography column for washing , and then add 3 ml of acetonitrile and glacial acetic acid mixed solvent with a volume ratio of 95:5. At room temperature,...

Embodiment 3

[0029] Grind the finished tea leaves (dry tea) to be tested, pass through a 20-mesh sieve, and make the sample to be tested for later use; take a chromatographic column (0.5-1.0 cm in inner diameter, 5-10 cm in height), and put it in the chromatographic column by Fill in 0.8 cm of absorbent cotton and 45 mg of the imprinted polymer prepared above in sequence from bottom to top; accurately weigh 0.1 g of the tea powder to be tested in a glass mortar, soak it with 0.3 ml of water for 50 minutes, add 0.15 g of the above-mentioned imprinted polymer The dicofol molecularly imprinted polymer adsorbent, mixed, fully ground for 8 minutes, moved the uniformly dispersed mixture to the above-mentioned chromatography column, and pressed 0.8 cm absorbent cotton into the upper end of the mixture; added 2.5 ml of deionized water to the chromatography column for washing , and then add 3.5 ml of acetonitrile and glacial acetic acid mixed solvent with a volume ratio of 95:5. Dry the solution wi...

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Abstract

The invention discloses a pretreatment method for a finished tea sample for dicofol pesticide residue detection. The pretreatment method comprises the following steps: adding water to moisten a crushed and dried finished tea sample, further adding a dicofol molecularly imprinted polymer, grinding, uniformly mixing, adding into a chromatographic column which is prefilled with the dicofol molecularly imprinted polymer, washing with deionized water, further eluting by using a mixed solvent composed of acetonitrile and glacial acetic acid and taken as an eluent, collecting the eluting liquid, concentrating and drying the eluting liquid, and dissolving and making the volume constant by using n-hexane. By adopting the pretreatment method, a simple grinding technique can be adopted, residual pesticides in the tea sample can be sufficiently adsorbed and extracted while cells of the tea sample are crushed, a great amount or harmful organic solvents are not used, and the analysis and detection cost can be greatly reduced; meanwhile as the dicofol molecularly imprinted polymer is taken as the adsorbent, the pretreatment method has the characteristics of high extraction efficiency on dicofol, good separation effect, small interference, small loss, accurate result and good recyclability.

Description

technical field [0001] The present invention relates to the field of pesticide residue detection, in particular to a sample pretreatment method before the detection of pesticide residues in finished tea leaves, and in particular to a fast, efficient, economical and environmentally friendly sample pretreatment method, which can be applied to various types of finished tea leaves Analysis of dicofol pesticide residues. Background technique [0002] At present, 18 countries and organizations in the world have issued 349 allowable pesticide residue standards for the amount of pesticide residues in tea, and some major tea importing countries have also formulated stricter regulations on the amount of pesticide residues in tea, making my country Tea exports are under enormous pressure. While intensifying inspections on my country's tea imports, more stringent pesticide residue limits (MRLs) have been formulated every year, tea inspection items have been expanded, and technical regul...

Claims

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Application Information

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IPC IPC(8): G01N1/28
Inventor 谭君文洋刘仲华
Owner HUNAN AGRICULTURAL UNIV
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