快速溶剂萃取-超高效液相色谱-串联质谱法测定蜂花粉中氯霉素

Determination of chloramphenicol residue in bee pollen by accelerated solvent extraction-ultra performance liquid chromatography-tandem mass spectrometry

摘要: 建立了快速溶剂萃取-超高效液相色谱-串联质谱法（UPLC-MS/MS）测定蜂花粉中氯霉素的分析方法。样品以乙酸乙酯为萃取溶剂经快速溶剂萃取仪（ASE）萃取,硅胶固相萃取柱净化,采用液质联用多反应监测负离子模式测定,同位素内标法定量。方法线性范围0.5¹0 ng/m L,相关系数为R2=0.9936,回收率在88.3%¹10.0%之间,相对标准偏差在5.3%⁸.9%之间,检出限为0.1μg/kg。该方法具有效率高、试剂用量少、选择性好、灵敏度高等优点。

Abstract: A method for analysis of chloramphenicol residue in bee pollen was developed. Sample was extracted using accelerated solvent extraction with ethyl acetate as extraction reagent and purified by Silica solid phase.Mass spectrometer was operated in the negative ion mode using select reaction monitoring. Isotope internal standard was used for quantitative analysis. The linearity of the calibration curve was from 0.5 to 10 ng/m L with correlation coefficient was 0.9936. Recovery rates for chloramphenicol in a negative bee pollen sample spiked at three levels were between 88.3% and 110.0%,with RSD range of 5.3% ⁸.9%. The limit of detection in the method was 0.1 μg/kg. This method proved to be of high efficiency,small amount of reagent,good selectivity and high sensitivity.