高效液相色谱法和高效液相色谱-串联质谱法测定水产品中的四环素类残留量

Determination of tetracyclines residues in aquatic products by high performance liquid chromatography and high performance liquid chromatography-tandem mass spectrometry

中文关键词:  高效液相色谱法  高效液相色谱-串联质谱法  四环素  水产品

英文关键词:high performance liquid chromatography  high performance liquid chromatography-tandem mass spectrometry  tetracycline  aquatic products

中文摘要:

      目的 建立高效液相色谱法(high-performance liquid chromatography, HPLC)定量测定水产品中四环素类残留量, 同时采用高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)进行定性确证和定量检测。方法 优化缓冲提取液浓度、固相萃取柱类型、色谱条件选择等测定环节。样品经柠檬酸缓冲液提取, 固相萃取柱净化后, 以液相色谱-紫外检测器进行定量检测, 同时通过高效液相色谱-串联质谱仪进行定性和定量检测。结果 四环素类目标物在10~200 ng/mL范围内线性良好(r>0.999), 在10、50、100 μg/kg 3个水平上进行加标回收实验, 回收率为76.0%~94.5%, 相对标准偏差为3.9%~7.4%, 高效液相色谱法检出限为5 μg/kg, 高效液相色谱-串联质谱法检出限为1 μg/kg。结论 该方法简便、稳定、准确, 适合测定水产品中的四环素类残留量。

英文摘要:

      Objective To establish a method for the determination of tetracycline’s residues in aquatic products by high performance liquid chromatography (HPLC) and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The concentration of buffer extract, solid phase extraction column type and chromatographic condition selection were optimized. The samples were extracted with citric acid buffer, purified with solid phase extraction column, quantitatively detected by liquid chromatography-ultraviolet detector, and qualitatively and quantitatively detected by high performance liquid chromatography-tandem mass spectrometry. Results Tetracycline targets had good linearity in the range of 10-200 ng/mL (r>0.999). With 3 spiked concentrations of 10, 50 and 100 μg/kg, the average recoveries were 76.0%-94.5%, the relative standard deviation were 3.9%-7.4%, the detection limit of HPLC was 5 g/kg, and the detection limit of HPLC-MS/MS was 1 g/kg. Conclusion The method is simple, stable and accurate, suitable for the determination of tetracycline residues in aquatic products.