Studies On Method Of IAC-LC For Determination Of CAP, ZAL And Analogs Veterinary Drug Residues In Food

A method based on immunoaffinity column clean-up and high performance liquidchromatography with ultraviolet detection was developed for the quantitative detection ofCAP residues in honey, eggs and aquatic products (fish and shrimp). The samples wereextracted with ethyl acetate followed by a clean-up step using the immunoaffinity columns,the analytes were detected by HPLC-UV. The mean recoveries of CAP in fish and shrimpsamples at different spiked levels (0.25~2.0μg/kg) were88.2~95.1%, and the relativerepeatability standard deviations were less than9%. The LOD were0.10μg/kg and0.15μg/kg, respectively, and the LOQ were both0.25μg/kg for CAP in milk and powdermilk samples. The mean recoveries of CAP in honey and eggs samples were all between89.7%and94.5%at fortified levels of0.2~2.0μg/kg，and the RSDs were less than8%. TheLOD were both0.10μg/kg and the LOQ were both0.20μg/kg for CAP in honey and eggssamples.A method using immunoaffinity column clean-up and high performance liquidchromatography tandem mass spectrometry was also developed for the quantitativedetection of CAP residues in honey, eggs and aquatic products (fish and shrimp). Thesamples were extracted with ethyl acetate followed by an immunoaffinity column clean-upstep. The analysis was performed by HPLC-MS/MS, the analytes were detected bymultiple reaction monitoring (MRM) using electrospray ionization (ESI) negative mode.The mean recoveries of CAP in fish and shrimp samples at different spiked levels (0.1~0.5μg/kg) were89.7~96.0%, and the relative repeatability standard deviations were less than8%. The LOD were both0.03μg/kg and the LOQ were both0.10μg/kg for CAP in fish andshrimp samples. The mean recoveries of CAP in honey and eggs samples were all between88.4%and95.3%at fortified levels of0.05~0.5μg/kg，and the RSDs were less than7%. The LOD were0.02μg/kg and0.03μg/kg, respectively, and the LOQ were both0.05μg/kg for CAP in honey and eggs samples.An analytical method for simultaneous determination of residues of zeranol and itsanalogs in milk and powder milk was established by immunoaffinity column clean-up andhigh performance liquid chromatography with ultraviolet detection. The samples wereextracted with acetonitrile, purified by immunoaffinity column. The analytes were detectedby HPLC-UV. The mean recoveries of the six target compounds at different spiked levelsin milk (5、10、20μg/L) and powder milk (1.0、10、15μg/kg) samples were82.7~102%and84.7~103%, respectively, and the RSDs were less than10%. LOD (S/N≥3) and LOQ(S/N≥10) for each zeranol in milk and powder milk samples were in the ranges of0.3~2.0μg/L and1.0~5.0μg/kg, respectively.A method for simultaneous determination of residues of zeranol and its analogs inmilk and powder milk was also established by immunoaffinity column clean-up and highperformance liquid chromatography tandem mass spectrometry. The samples wereextracted with acetonitrile. After cleaned up by immunoaffinity column, analysis wascarried out on HPLC-MS/MS by electrospray ionization(ESI－) using multiple reactionmonitoring. The mean recoveries of six analogs at different spiked levels in milk (0.10、0.25、0.50μg/L) and powder milk (0.05、0.25、0.50μg/kg) samples were84.5~97.4%and86.5~97.2%, respectively, and the RSDs were less than9%. LOD (S/N≥3) and LOQ (S/N≥10) for each zeranol in milk and powder milk samples were in the ranges of0.02~0.05μg/L and0.05~0.1μg/kg, respectively.