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
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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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