水产品中四环素类药物残留的超高效液相色谱-串联质谱测定

建立同时测定水产品中6 种四环素类药物残留的超高效液相色谱- 串联质谱(UPLC-MS/MS)分析方法。用0.01mol/L Na2EDTA-Mcllvaine 磷酸盐缓冲溶液提取，样液过滤后正己烷除脂，经Oasis HLB 固相萃取柱净化，甲醇洗脱，氮气吹干缓冲液定容后，用反相液相色谱分离，电喷雾正离子模式离子化，用多反应监测模式(MRM)监测，三重四级杆质谱测定，外标法定量。该法对四环素类药物在5.0～50.0μg/kg 范围内呈线性关系，相关系数r 在0.9969～0.9999 之间，在5.0、10.0、25.0、50.0μg/kg 添加水平，回收率为61%～97%，相对标准偏差(RSD)为1.3%～5.7%，其检出限达2.5μg/kg，方法操作简便，稳定性好，选择性好，灵敏度高。

Determination of Tetracycline Residues in Aquatic Products by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established for the simultaneous determination of six tetracylines in aquatic products. Samples were extracted with 0.01 mol/L Na2EDTA/ Mcllvaine buffer solution. After filtrated and degreased by n-hexane, the extract was passed through Oasis HLB solid phase extraction column and eluted with methanol, and the eluate was then pooled together and evaporated until dryness under nitrogen and redissolved in 1.0 mL of dissolving solution. The solution was separated on a RP-UPLC column and detected by triplequadrupole MS. The electrospraying was operated in the positive ionization mode and the identification of analytes was achieved using multiple reaction monitoring (MRM) mode. Quantitation was carried out using the external standard method. The standard curves for all the compounds were linear over the concentration range of 5.0 to 50.0μg/kg with correlation coefficients between 0.9969 and 0.9999. The spike recoveries at four levels of 5.0, 10.0, 25.0, 50.0μg/kg ranged form 61% to 97%, and the relatives standard deviations (RSD) were in the range of 1.3% to 5.7%. The limits of detection of the method for the analytes were all 2.5μg/kg. Owing to the merits of simplicity, selectivity and sensitivity, the proposed method has been successfully applied to the determination of tetracyclines in aquatic products.