Determination of 31 Drug Residues in Raw Milk by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry Based on PRiME-HLB
A method for the determination of 31 kinds of veterinary drugs in raw milk by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)based on PRiME-HLB(Hydrophilic lipophilic balance).The samples were extracted by 1％formic acid-acetonitrile,ultrasoniced for 20 min and oscillating vortex for 5 min.After centrifugation,the supernatant was purified through a PRiME HLB solid phase extraction column,concentrated to near dryness,and re-dissolved in 10％methanol-water solution.Separation was achieved using a Hypersil GOLD C18 column with 0.1％formic acid-water/methanol as the mobile phase in gradient elution,and analysis was performed in the electron spray ionization(ESI)positive ion multiple reaction monitoring(MRM)mode.Under the optimized conditions,the total analysis time of 31 drugs was only 10 min,and the peak shape of ion chromatogram of each group was good,the retention time was between 1.5-9.0 min.The correlation coefficients(R2)for the linear range of mass concentrations between 10 μg/kg and 200 μg/kg were all greater than 0.99.The limit of detection and limit of quantification were 0.5-20.0 μg/kg and 5.0-80.0 μg/kg,respectively.At three spiked levels of 80,40,and 20 μg/kg,the recovery rates of the method were in the range of 62.4％-99.8％.The relative standard deviations were less than 10％(n=6).The method has the advantages of simple operation,fast analysis and little matrix interference,and is suitable for high-throughput screening of various veterinary drugs in raw milk.
ultra performance liquid chromatography-tandem mass spectrometryPRiME HLBraw milkveterinary drug residuesrapid screening
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维普
