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目的用高效液相色谱-串联质谱法快速测定水产品中13种喹诺酮类药物残留量的方法。方法色谱柱为Ultimate XB-C18(2.1 mm×150 mm,5μm),确定了最佳检测参数:离子源为电喷雾(ESI)离子源、正离子扫描、选择反应监测(SRM)、电喷雾电压4 500 V、鞘气35 units、辅气5 units、离子源温度350℃、源内碰撞诱导解离电压为10 V。从提取和净化两个方面确立了前处理的最佳条件与步骤。结果平均回收率74.6%～113.0%,相对标准偏差为3.24%～12.11%(n=6),定量检出限(LOQ)为1.00μg/kg,线性范围在3.0～200.0 ng/ml。结论所建立的方法可以用于日常水产品中13种喹诺酮类药物残留量的检测分析。
Aim To rapidly determine the residues of 13 quinolones in aquatic products by high performance liquid chromatography-tandem mass spectrometry. Methods The optimal detection parameters were determined with Ultimate XB-C18 (2.1 mm × 150 mm, 5 μm). The ion source was electrospray ionization (ESI), positive ion scan, selective reaction monitoring (SRM), electrospray voltage 4 500 V, 35 units of sheath gas and 5 units of auxiliary gas. The temperature of the ion source was 350 ℃ and the induced dissociation voltage was 10 V. From the extraction and purification of two aspects established the best pre-treatment conditions and steps. Results The average recoveries ranged from 74.6% to 113.0%. The relative standard deviations (RSDs) ranged from 3.24% to 12.11% (n = 6). The limit of quantification (LOQ) was 1.00 μg / kg and the linear range was from 3.0 to 200.0 ng / ml. Conclusion The established method can be used to detect and analyze 13 kinds of quinolone residues in daily aquatic products.