Most of the reported methods for the detection of nitrofuran residues still analyze the prodrugs. In recent years, research organizations have begun to focus on the study of methods for the detection of their metabolites. Source: Food Safety Monitoring Technology (Chemical Industry Press)

Operation method

HPLC-MS/MS method

Materials and Instruments

Animal Tissue
Polytetrafluoroethylene Na3PO4 NaOH Ethyl acetate
Centrifuge tube Tandem mass spectrometry

Move

1. Extraction 2.000 g of sample was taken in a 50 mL PTFE centrifuge tube, and 100 uL of mixed internal standard working solution (10 ng/mL), 5-20 mL of 0.2 mol/L HCl solution (subject to the complete infiltration of the sample), and 50 uL of 100 mmol/L 2-NBA solution were added sequentially, and then shaken for 30 min, and then the reaction mixture was placed in a thermostat at 37 ℃ overnight. (16 h). 2. Purification Remove the sample and cool to room temperature. Add 0.5-2 mL of 0.3 mol/L Na3PO4 (5 mL of HCl corresponds to 0.5 mL of Na3PO4), and adjust the pH 7.4 (±0.2) with 2 mol/L NaOH. Extracted with 5-20 mL (the same volume as the added HCl solution) of ethyl acetate, shaken for 20 min, centrifuged at 4000 r/min for 5 min, and the upper liquid layer was collected; 5-20 mL of ethyl acetate was extracted again, and the ethyl acetate extracts were combined, and blown dry under N2 at 40 ℃. The residue was dissolved with 1 mL of mobile phase A, and then extracted with 3 mL of n-hexane (saturated with acetonitrile) in two times to remove the fat. The lower aqueous phase was passed through a 0.20 um microporous filter membrane, and then 100 L was taken into the sample for detection. 3. Tandem mass spectrometry conditions Capillary voltage 3.5 KV, source temperature 120 ℃, desolventization temperature 350 ℃, cone pore gas flow 100 L/h, desolventization gas flow 60 L/h, collision gas is argon, collision gas pressure 2.60 × 10-4 Pa. ESI+ , MRM mode detection.

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