QuCHERS-UHPLC-MS/MS法测定畜中双氯芬酸钠残留量

Determination of Diclofenac Sodium in Pork,Beef and Mutton by QuEChERS-based Extraction with UHPLC-MS/MS

建立了超高效液相色谱-串联质谱法快速测定畜肉中双氯芬酸钠残留量的检测方法。样品用乙腈提取,经Qu ECh ERS试剂化,通过超高效液相色谱C18反向色谱柱分离,在正离子多反应监测模式下分析,外标法定量。结果显示,在0.25~10.00μg/L质量浓度范围内,双氯芬酸钠在猪肉、牛肉、羊肉中呈现出良好的线性关系,相关系数均大于0.996,检出限均为0.5μg/kg。在0.5,1和2μg/kg 3个添加水平下的平均回收率在86.9%~99.0%之间,日内(n=6)变异系数和日间(n=3)变异系数均小于10%。该方法简单、快速、可靠,具有良好的灵敏度、回收率和精密度,适用于猪肉、牛肉、羊肉中双氯芬酸钠残留量的大批量快速检测。

The method for Ultrahigh performance liquid chromatography tandem mass spectrometry(UHPLC-MS/MS)was established for the determination of diclofenac sodium(NSAIDs)in pork,beef and mutton.The samples were pretreated by acetonitrile,purified with Qu ECh ERS reagent,separated by super high performance liquid chromatography(HPLC)with C18 reverse chromatographic column,analyzed under the multi-reaction monitoring mode of positive ions,and quantified by external standard method.The relationships of diclofenac sodium in the three kinds of meat storages were well in the concentration of 0.25-10.00μg/L,the correlation coefficients were more than 0.996,the limits of detection(LOD)were 0.5μg/kg,the average recovery of the three addition levels of 0.5,1 and 2μg/kg was 86.9%-99.0%,the variation coefficient of the intra-batch(n=6)and the variation coefficient of the inter-batch(n=3)was all less than 10%.The method was simple,fast and reliable,and had good sensitivity,recovery and precision,which had been applied to rapid detection of diclofenac residue in pork,beef and mutton.