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建立了超高效液相色谱-电喷雾串联质检测鸡组织中利巴韦林残留量的方法。采用10%乙腈-三氯乙酸溶液提取鸡组织中的利巴韦林,经磷酸酶水解,苯硼酸(PBA)固相萃取小柱净化,NUCLEOSHELL HILIC(3.0 mm×100 mm,2.7μm)色谱柱分离,采用电喷雾离子源串联质谱法,在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。在优化条件下,利巴韦林在0.5~50 ng/m L范围内线性关系良好(r2>0.99),方法的检出限(信噪比为3)为0.1~0.3μg/kg,定量限(信噪比为10)为0.4~0.9μg/kg;鸡肉、鸡肝、鸡肾、鸡蛋和皮蛋在添加浓度1.0~10.0μg/kg范围内,其平均回收率为84.2%~92.6%,相对标准偏差(n=6)为5.0%~12%。
A method for the determination of ribavirin residues in chicken tissues by ultra performance liquid chromatography-electrospray tandem mass spectrometry was established. Ribavirin in chicken tissues was extracted with 10% acetonitrile-trichloroacetic acid solution and purified by phosphatase and PBA solid phase extraction cartridges. NUCLEOSHELL HILIC (3.0 mm × 100 mm, 2.7 μm) column Separation, using electrospray ionization tandem mass spectrometry, in positive mode with multiple reaction monitoring (MRM) mode determination, isotope internal standard method. Ribavirin had a good linearity (r2> 0.99) in the range of 0.5-50 ng / mL under optimal conditions. The detection limit (signal to noise ratio of 3) was 0.1-0.3 μg / kg and the limit of quantification (Signal to noise ratio of 10) was 0.4 ~ 0.9μg / kg; the average recovery of chicken, chicken liver, chicken kidney, egg and preserved egg in the range of 1.0 ~ 10.0μg / kg was 84.2% ~ 92.6% The standard deviation (n = 6) was 5.0% to 12%.