建立了通过式固相萃取净化-超高效液相色谱-串联质谱法快速测定禽肉中利巴韦林残留量的方法。样品在37 ℃经酸性磷酸酯酶酶解，乙腈提取，EMR-Lipid固相萃取柱净化，以乙腈和0.1%甲酸水（含5 mmol/L甲酸铵）为流动相，经过BEH Z-HILIC色谱柱（100 mm×2.1 mm，1.7 μm）分离，经串联质谱仪，在电喷雾正离子模式下以多反应监测（MRM）模式测定，同位素内标法定量。对前处理条件、液相条件和质谱参数进行了系统的考察。该方法在0.05~5 μg/L质量浓度范围内线性关系良好，定量限（LOQ）为2.0 μg/kg。在2.0、4.0、20 μg/kg添加水平下，回收率为94.5%~112.0%，相对标准偏差（n=6）为1.4%~3.2%。该方法相比标准方法前处理简单、快速，适用于禽肉中利巴韦林残留的批量分析。

A rapid analysis method was established for determining the ribavirin residue in poultry meat through purification by solid-phase extraction and analysis by ultra-performance liquid chromatography-tandem mass spectrometry. After enzymatic hydrolysis with acid phosphatase at 37 ℃, the samples were extracted with acetonitrile and purified with an EMR-Lipid solid phase extraction column to remove liposoluble substances. The purified sample solution was subjected to separation using a BEH Z-HILIC column (100 mm×2.1 mm, 1.7 μm) and a mobile phase consisting of acetonitrile and 0.1% aqueous formic acid solution (containing 5 mmol/L ammonium formate) for analysis by tandem mass spectrometer in positive electrospray ionization mode with multiple reaction monitoring (MRM). An isotope-labeled internal standard method was used for quantitative analysis. The pretreat conditions, HPLC conditions and mass spectrometry parameters were systematically investigated. This method showed good linearity in the range of 0.05~5 μg/L with the limit of quantification (LOQ) being 2.0 μg/kg. When the spiking levels were 2.0, 4.0 and 20.0 μg/kg, the recoveries of ribavirin were in the range of 94.5%~112.0% with the relative standard deviations (n=6) being 1.4%~3.2%. Compared with the standard method, this method is simple and rapid, thus suitable for batch analysis of ribavirin residue in poultry meat.

国家市场监督管理总局科技计划项目（2022MK072）