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目的建立超高效液相色谱-串联质谱同位素内标法测定鸡肝中恩诺沙星残留量。方法样品加入内标和EDTA-Mcllvaine缓冲溶液,超声提取,HLB固相萃取柱净化后,采用电喷雾(ESI+)多反应监测(MRM)方式进行检测。结果恩诺沙星在10.0~480 ng/ml浓度范围具有良好的线性关系,相关系数r值为0.9993,在空白样品中添加4.0μg/kg、32μg/kg、80μg/kg 3个浓度水平的恩诺沙星标准品,平均回收率和相对标准偏差分别在91.0%~96.2%、2.9%~7.1%之间,恩诺沙星定量限为1.5μg/kg,与Qu ECHERS快速净化方法相比,该方法净化效果较好,同时加入同位素内标有效的降低基质对定量结果的影响;运用该方法测定鸡肝中恩诺沙星能力验证,结果满意。结论该方法能准确、灵敏测定鸡肝中恩诺沙星,可为了解鸡肝中恩诺沙星残留水平提供方法依据。
OBJECTIVE To establish a method for the determination of enrofloxacin in chicken livers by ultra performance liquid chromatography-tandem mass spectrometry (ISSR). Methods The samples were added with internal standard and EDTA-Mcllvaine buffer solution. The samples were cleaned up by ultrasonic and HLB solid phase extraction (SPE). The electrospray (ESI) multi-reaction monitoring (MRM) Results Enrofloxacin had a good linearity in the concentration range of 10.0 ~ 480 ng / ml, the correlation coefficient r was 0.9993. The concentration of enrofloxacin in the blank samples was 4.0 μg / kg, 32 μg / kg and 80 μg / kg respectively The average recoveries and relative standard deviations of norfloxacin standard ranged from 91.0% to 96.2% and 2.9% to 7.1%, respectively. The limit of quantification of enrofloxacin was 1.5 μg / kg. Compared with Qu ECHERS rapid purification method, The method has a good purification effect, while adding an isotope internal standard effectively reduces the influence of the matrix on the quantitative results. The method is applied to the determination of the enrofloxacin capacity in the chicken liver with satisfactory results. Conclusion This method can accurately and sensitively determine enrofloxacin in chicken livers and provide a basis for understanding the residual levels of enrofloxacin in chicken livers.