Experimental method for the determination of chalcones residues in animal tissues

Summary

Quinolone residues in tissues are predominantly prodrugs, so prodrugs are generally chosen as indicator residues. Most of the metabolites are metabolized quickly, such as demethylated products, which may be mainly present in excreta, and some metabolites of quinolones, such as demethylated difloxacin and deethylated enrofloxacin (i.e., ciprofloxacin), still have strong biological activity and should be included in the total residues. Source: Food Safety Monitoring Technology (Chemical Industry Press)

Operation method

High Performance Liquid Chromatography

Materials and Instruments

Animal Tissue
Acetic acid-acetonitrile n-hexane phosphate-triethylamine buffer
Phase Chromatography Conditions Columns Centrifuge Tubes Syringes

Move

1. Pre-treatment Weigh about 2 g of thawed sample, cut into thin slices and put into a 50 mL centrifuge tube, add 20 mL of 1% acetic acid-acetonitrile solution, homogenize for 1 min and then put into the ultrasonic cell to ultrasonic for 3 min, centrifuged at 4500 r/min for 5 min, and then the supernatant was carefully transferred into a 100 mL plastic centrifuge tube, and the centrifugal residue was extracted with 20 mL of 1% acetic acid-acetonitrile solution once more, and then combined with the supernatant. The combined supernatant was purified by degreasing with 25 mL of acetonitrile-saturated n-hexane, the upper solution was discarded, and the lower solution was transferred to a 100 mL flask, rotary evaporated in a 40 ℃ water bath to near-dryness, and blown dry with nitrogen. To the residue, 1 mL of HPLC mobile phase was added, and the residue was dissolved by rapid mixing and sonication for 3 min. The dissolved solution was transferred to a 1 mL secondary syringe and filtered through a syringe filter membrane (0.45 um) into an HPLC injection vial for HPLC determination. 2. Instrumental parameters Liquid chromatographic conditions: 4.0 mm × 250 mm × 5 um, Hyprsil ODS; Column temperature: 30 ℃; Elution mode 1: 0.01 mol/L phosphate-triethylamine buffer (pH 3.0) (0.68 mL of phosphoric acid was diluted to 1 L with water, and then the acidity was adjusted to pH 3.0 with triethylamine). Phosphate-triethylamine buffer-acetonitrile (80 + 20) mixture, flow rate: 1 mL/min. Elution Mode 2: Gradient elution at a flow rate of 0.8 mL/min.

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