超高效液相色谱-串联质谱法测定水体中磺胺类药物残留量方法验证  

Determination of Sulfonamides Residues in water by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：余海芬[1] 徐桦[1] 陶军[1] 吴真善 包蔚[1] 朱晓芸[1] YU Haifen;XU Hua;TAO Jun;WU Zhenshan;BAO Wei;ZHU Xiaoyun(Jiading District of Shanghai Agricultural Technology Extension Service Center,Shanghai 201800,China)

机构地区：[1]上海市嘉定区农业技术推广服务中心,上海201800

出　　处：《中国渔业质量与标准》2024年第2期7-13,共7页Chinese Fishery Quality and Standards

基　　金：上海市嘉定区自然科学研究课题(JDKW-2021-0010)。

摘　　要：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。本研究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5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5.0~50.0 ng/mL浓度范围内线性良好,校准曲线相关系数r 2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%。应用该方法测定了上海市嘉定区内河流和养殖场池塘水样中的磺胺类药物的残留量,该方法的建立可为监控河流和水产养殖用水中磺胺类药物的残留情况提供技术依据。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 had good linearity within the concentration range of 5.0~50.0 ng/mL.The correlation coefficient of calibration curve was more than 0.997.The detection limit of this method was 0.038 ng/mL.The average recovery rates of three spiked levels ranged from 74.6%to 105.6%,and the relative standard deviations were 0.89%~12.89%.This method was applied to detect the residues of sulfonamide drugs in water samples and aquaculture pond water samples in Jiading District,Shanghai.The establishment of this method can provide technical basis for monitoring the residues of sulfonamide drugs in rivers and aquaculture water.

关 键 词：水体 磺胺类抗生素 超高效液相色谱—串联质谱 残留检测 

分 类 号：O657.63[理学—分析化学] X52[理学—化学]