HPLC-MS/MS法测定猪肌肉、肝脏及肾脏中双氯芬酸钠残留量

建立了HPLC-MS/MS方法检测猪肌肉、肝脏及肾脏3种组织中非甾体抗炎药双氯芬酸钠的残留量。样品处理以萘普生为内标,先经乙酸乙酯液液提取,后经甲醇沉淀,Eclipse Plus C18柱(100 mm×2.1 mm×3.5μm)等度洗脱。在负离子模式下,采用ESI电离源选择性反应监测模式(SRM)对双氯芬酸及萘普生进行检测。结果表明:在0.5~100μg/kg浓度范围内,双氯芬酸钠在猪肌肉、肝脏及肾脏组织中的线性关系均良好,相关系数均大于0.99,各组织中的准确度RE及精密度CV均小于15%。该方法快速、有效、可靠,可应用于市场出售的猪肌肉、肝脏及肾脏中双氯芬酸钠残留量的检测。

Determination of Diclofenac Sodium Residue in Swine Muscle,Liver or Kidney by HPLC-MS/MS

The method for high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) was established for the determination of diclofenac sodium (NSAIDs) in swine muscle, liver or kidney. Naproxen was adapted for internal standard. The samples were pretreated by liquid-liquid extraction, then methanol protein precipitation. Chromatographic separations were performed on an Eclipse Plus C18 column (100 mm×2.1 mm×3.5 μm) with an isocratic elution. Diclofenac and naproxen were ionized with an ESI source operated in negative ion mode, and were measured by selective reactions monitoring mode (SRM). The results show that the relationships of diclofenac sodium in the three tissues are well in the concentration of 0.5-100 μg/kg. The correlation coefficinets are more than 0.99. The RE of accuracy and the CV of precisions are all less than 15%. The method is rapid, specific and reliable, which has been applied to determine the residue of diclofenac sodium in swine muscle, liver or kidney bought from markets.