Determination of Fipronil and Amide Alcohol Antibiotics Residues in Egg by dSPE EMR-Lipid with UPLC-MS/MS
A confirmative method was developed for the determination of fipronil and amide alcohols in eggs by using ultra high performance liquid chromatography tandem mass spectrometry.The sample was dispersed in water,extracted with acidified acetonitrile,purified with dSPE EMR Lipid enhanced lipid adsorbent,and Phenomenex Kinetex F5 chromatography column separation was performed using a 5 mmol/L ammonium acetate aqueous solution acetonitrile as the mobile phase for gradient elution.Ionization was performed under ESI ion source positive and negative modes,and detection was performed under multiple reaction monitoring(MRM)mode.Fluconazole and its metabolites were quantified using external standard method,while amide alcohol drugs were quantified using internal standard method.The linear relationship is good withchloramphenicol at a mass concentration of 0.1-5 μg/L,other drugs within 1-50 μg/L,and the correlation coefficient r is greater than 0.99.At the spiked levels of LOQ,2 LOQ,and 10 LOQ,the recovery rates(relative standard deviation)were 68.6％to 86.4％(4.48％to 8％),72.8％to 88.3％(3.89％to 12.2％),and 74.9％to 94.6％(2.1％to 7.1％),respectively.This method is easy to operate,highly sensitive,and suitable for the quantitative detection of fipronil and amide alcohol drug residues in eggs.
eggsfipronil and its metabolitesamide alcohol antibioticsUPLC-MS/MS
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