[ Objective ] To develop a novel method for the determination of four kinds of NSAIDs ( non-steroidal anti-inflammatory drugs) residues including flunixin meglumine, meloxicam, ketoprofen and diclofenac sodium in the crucian by HPLC, assisting by microwave and ultrasound. [ Method ] The NSAIDs were extracted with the acidificated ethanol and purified by diatomite column, the compounds were eluted by methanol. [ Result ] The subsequent analysis of NSAIDs was achieved using acetonitrile -0. 1％ triethlamine (adjusted pH value to 3.5 with phosphate) (60∶40,by volume) as mobile phase with a flow rate of 0.8 mL/min at 30 ℃. The detection wavelength was set at 255 nm. The detection limit of four kinds of NSAIDs were 5 - 10 μg/kg (S/N = 3 ) and the limits of quantitation (LOQ) were 15 -30 μg/kg (S/N = 10).The adding recovery rates were at the range of 72.5％ -93.8％ with RSD below 15％. [Conclusion] The method was simple, rapid, high sensitivity and specificity, and it could meet the qualitative and quantitative analysis requirements.%[目的]建立一种微波超声波辅助提取-高效液相色谱法同时检测鲫鱼中氟尼辛葡甲胺、美洛昔康、酮洛芬和双氯芬酸钠4种非甾体抗炎药残留的分析方法.[方法]样品前处理采用磷酸酸化的乙醇为提取溶剂,微波超声波辅助提取,硅藻土层析柱净化,甲醇洗脱.[结果]采用的流动相为乙腈-0.1%三乙胺水溶液(磷酸调节pH值为3.5),流动相体积比乙腈∶0.1%三乙胺水溶液=60∶40,流速0.8 ml/min,检测波长为255 nm.4种非甾体抗炎药的检出限为5～10 μg/kg(S/N=3),定量限15～30 μg/kg(S/N=10).添加回收率为72.5%～93.8%(n=5),相对标准偏差(RSD)小于15%.[结论]该方法操作简单、快速、灵敏度高、特异性强,能满足定性定量分析要求.
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