Abstract
A rapid and effective high performance liquid chromatographic (HPLC) method with accelerated solvent extraction (ASE)-solid phase extraction cleanup was developed for the determination of sulfonamide and sarafloxacin residues in pork and chicken muscle. Four residues were extracted with acetic acid-acetonitrile at 70°C under 10.3 MPa pressure and 5 min static times with 2 static cycles. The standard curves for the determination of four residues have good linearity (r>0.999). The method limits of quantification (LOQs) were 4-12 μg.kg-1. Intra- and inter-day precisions (RSDs) were 0.3-1.5% and 0.7-1.8%, respectively. Their average recoveries with four spiked levels ranged from 83% to 108% with the RSD of 0.3-1.5%. This method provides an effective extraction procedure and high sensitivity, and can be applied for the determination of 4 residual drugs in pork and chicken muscle at lower than their MRL levels.
Highlights
Sample pretreatment is always a crucial step in deciding the levels of detection limits of the overall method, especially when large number of aquatic product with complex matrices is involved, and rapid extraction becomes even more essential
China Agriculture Department have laid down the maximum residue level (MRL) of 100 μg.kg–1 for SAs, and 10-1900 μg.kg–1 for FQs in animal origin food, in particular MRL of sarafloxacin is lowest as 10 μg.kg–1 for pork and chicken muscle [1,2]
The sensitivity increased and retention time decreased with increase in the ratio of methanol from 25% to 40%
Summary
Sample pretreatment is always a crucial step in deciding the levels of detection limits of the overall method, especially when large number of aquatic product with complex matrices is involved, and rapid extraction becomes even more essential. China Agriculture Department have laid down the maximum residue level (MRL) of 100 μg.kg–1 for SAs, and 10-1900 μg.kg–1 for FQs in animal origin food, in particular MRL of sarafloxacin is lowest as 10 μg.kg–1 for pork and chicken muscle [1,2]. It is urgently in need of developing rapid and effective method for simultaneous determination of SAs and sarafloxacin residues at the low concentrations normally present in food in meats. Quantification was carried out by using standard curve calibration based on peak area toward concentration in 7 concentration points
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