Jiading District of Shanghai Agricultural Techonogy Extension Service Center
标准方法验证是检验检测实验室质量管理过程中的重要一环，是保障检验检测数据准确性的基础。本文建立了超高效液相色谱三重四级杆质谱联用仪测定水体中磺胺类药物残留量的方法，从标准曲线、线性范围、定量限、精密度及方法回收率几方面进行方法验证，并对本方法的实验关键点进行了分析优化。结果表明：17种磺胺类药物在5.0 ng/mL～50 ng/mL浓度范围内线性良好，校准曲线相关系数r2值均大于0.997，该方法的检出限为0.038 ng/mL，3个加标水平的平均回收率在74.6%～105.6%之间，相对标准偏差0.89%～12.89%。该方法的建立，可为监控水产养殖过程中磺胺类药物的使用情况提供技术依据。
Standard method validation is an important part of the quality management process in inspection and testing laboratories, and is the foundation for ensuring the accuracy of inspection and testing data. In this study, a method for determination of sulfonamides residues in water by UPLC-MS/MS was established.Verify the method from standard curve, linear range,quantification limit, precision, and method recovery rate. And the key experimental points of this method were analyzed and optimized. 17 kinds of sulfonamides have good linearity within the concentration range of 5.0 ng/mL-50 ng/mL. The correlation coefficient of calibration curve were more than 0.997. The detection limit of this method was 0.038 ng/mL. The average recovery rates of three spiked levels range from 74.6% to 105.6%, and the relative standard deviations were 0.89%～12.89%. The method could be used for quantitative determination of sulfonamides residues in water from aquaculture environment..