Development of an accelerated solvent extraction, ultrasonic derivatisation LC‐MS/MS method for the determination of the marker residues of nitrofurans in freshwater fish

Abstract

A rapid method using accelerated solvent extraction (ASE) and ultrasound enhanced derivatisation has been developed for the quantitative determination of metabolites of nitrofurans, namely 3‐amino‐2‐oxalidinone (AOZ), 5‐morpholinomethyl‐3‐amino‐2‐oxalidinone (AMOZ), 1‐amino‐hydantoin (AHD) and semicarbazide (SEM), in muscle and skin of carp and finless eel. The target analytes were extracted using ASE, ultrasonic derivatisation for 1 h and then purified by solid phase extraction. Averaged decision limits (CCα) and detection capability (CCβ) of the method were in the range of 0.07–0.13 and 0.31–0.49 µg kg⁻¹ in carp and finless eel, respectively. The accuracy in terms of recovery was in the range 77.2–97.4%. The simplified and traditional methods were compared with incurred residue samples. The simplified method reduced the derivatisation time and has been applied to the determination of nitrofurans residues in fish.

Keywords:

• chromatography, LC/MS
• clean‐up
• extraction, ASE
• method validation
• animal products
• veterinary drug residues, antibiotics
• fish and fish products

Acknowledgements

The authors thank the Ministry of Agriculture the People's Republic of China for the financial support, which enabled this work to be carried out.