HPLC-MS/MS法测定猪肌肉、肝脏及肾脏中双氯芬酸钠残留量  

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

作　　者：王莉[1] 倪莹莹[1] 王慧[1] 王文艳[1] 

机构地区：[1]烟台大学药学院,山东烟台264005

出　　处：《质谱学报》2015年第3期237-242,共6页Journal of Chinese Mass Spectrometry Society

摘　　要：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×3.5 μm）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0.5～100 μg/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.The method for high performance liquid chromatography tandem mass spec- trometry （HPLC-MS/MS） was established for the determination of diclofenac sodium （NSAIDs） in swine muscle, liver or kidney. Naproxen was adapted for internal stand- ard. The samples were pretreated by liquid-liquid extraction, then methanol protein pre- cipitation. Chromatographic separations were performed on an Eclipse Plus C18 column （100 min×2.1 min×3.5 μm） with an isocratic elution. Diclofenae and naproxen were ionized with an ESI source operated in negative ion mode, and were measured by selec- tive 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 eoefficinets are more than 0.99. The RE of accuracy and the CV of pre- cisions 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 kidneybought from markets.

关 键 词：双氯芬酸钠 残留量 肌肉 肝脏 肾脏 高效液相色谱-串联质谱(HPLC—MS/MS) 

分 类 号：O657.63[理学—分析化学]