In this work, an HPLC/MS/MS method for determination of gentamicin C components in fish tissues was developed based on strong cation exchange solid-phase extraction (SPE) purification coupled with Hypercarb chromatographic column in separation mode. Sample was extracted using trichloroacetic acid aqueous solution containing EDTA. Ion-pairing reagents were not needed because of the “graphite polarity retention effect” of the Hypercarb chromatographic column. HPLC-MS/MS was performed in multiple reaction monitoring (MRM) mode for simultaneous qualitative and quantitative analyses (using matrix external standard) of gentamicin C components in fish tissues. Good linearity was obtained for the target analytes within the concentration range from 0.0100 to 0.500 mg/L. The limits of quantification (LOQ) of this method were 10.0, 20.0, and 20.0 μg/kg for C1, C1a, and sum of C2 + C2a, respectively. The average recoveries of gentamicin C components were 80.0%–110% when spiked at three levels with the blank carp (Cyprinus carpio) matrix, and the relative standard deviations (RSD) were all less than 15% (n = 6). In addition, for the features of simple operation, high sensitivity and good reproducibility, the proposed method has been successfully applied for detection of gentamicin residues in fish tissues during actual breeding.

在这项工作中，基于强阳离子交换固相萃取（SPE）纯化与Hypercarb色谱柱在分离模式下的结合，开发了一种用于测定鱼组织中庆大霉素C成分的HPLC / MS / MS方法。使用含有EDTA的三氯乙酸水溶液萃取样品。由于Hypercarb色谱柱具有“石墨极性保留作用”，因此不需要离子对试剂。HPLC-MS / MS在多反应监测（MRM）模式下进行，用于鱼组织中庆大霉素C组分的同时定性和定量分析（使用基质外标）。在0.0100至0.500 mg / L的浓度范围内，目标分析物具有良好的线性。该方法的定量限（LOQ）为10.0、20.0和20。C1，C1a和C2 + C2a的总和分别为0μg/ kg。当空白鲤鱼加标成三个浓度时，庆大霉素C成分的平均回收率为80.0％–110％（鲤（Cyprinus carpio）矩阵和相对标准偏差（RSD）均小于15％（n  = 6）。此外，该方法操作简便，灵敏度高，重现性好，已成功应用于实际养殖过程中鱼组织中庆大霉素残留的检测。