Optimization of the National Standard Method for Determining the Fluoroquinolones Residues in Chicken and Eggs Based on Laboratory Proficiency Testing Requirements
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Abstract:
Based on the characteristics of the laboratory proficiency testing and verification, the liquid chromatography analysis in the two national standard methods of the No. 1025-14-2008 announcement and No. 781-6-2006 announcement from the Ministry of Agriculture of the People’s Republic of China are optimized. In combination with the thermal precipitation process, rapid determination of the fluoroquinolone residues in chicken and egg samples could be accomplished, which provides a quality verification reference for the results of the proficiency testing and verification following the procedure of the national standard method. The test samples of chicken or eggs were extracted according to the national standard method to obtain the standby liquid (with the volume of the egg standby liquid was fixed to 6 mL). 1 mL of the standby liquid was precisely withdrawn for solid phase extraction (SPE) purification, then, the protein was rapidly precipitated by adding 0.2 mL of acetonitrile, vortexing, and heating for 20 min in a water bath at 55 ℃. After centrifugation, the supernatant was collected for rapid determination of the drug residue by high performance liquid chromatography. When the rapid heat precipitation method was applied to chicken and egg samples, the recoveries were 81.08%~103.09% and 77.60%~102.94%, respectively. The remaining standby liquid was further purified in accordance with the national standard method, and the purification processes were slightly optimized as follows: only 3 mL of the standby liquid of egg was taken for SPE purification; whilst the standby liquid of chicken was firstly frozen, then thawed, and centrifuged at a high speed. The supernatant was collected for SPE purification. Overall, the optimized procedure is simple with improved recovery and repeatability, and can not only provide a quality verification reference for the results of proficiency testing and verification, but also allow daily rapid batch detection.
