超声波-微波辅助提取-高效液相色谱法同时检测羊肉组织中4种非甾体抗炎药物残留

建立了超声波-微波辅助提取-高效液相色谱同时检测羊肉组织中氟尼辛葡甲胺、美洛昔康、双氯芬酸钠和酮洛芬4种非甾体抗炎药残留量的分析方法。样品前处理以酸化后的乙醇为提取剂,采用超声波-微波辅助提取,硅藻土柱净化。采用的色谱条件: 色谱柱为Hypersil C18柱(250 mm×4.6 mm, 5 μm),柱温为30 ℃,流动相为乙腈-0.2%三乙胺水溶液(40:60, v/v,用磷酸调节pH 3.5),流速为0.8 mL/min,检测波长为255 nm。4种非甾体抗炎药能够在20 min内得到很好的分离,各药物线性回归方程的线性相关系数为0.9993～0.9998,检出限(信噪比(S/N)=3)为5～10 μg/kg,定量限(S/N=10)为15～30 μg/kg,添加回收率为65.3%～99.6%(n=5),相对标准偏差小于15%。该方法操作简单、快速、灵敏度高,满足定性定量分析的要求。

Simultaneous analysis of 4 non-steroidal anti-inflammatory drug residues in mutton muscle using high performance liquid chromatography assisted by ultrasonic-microwave extraction

A method for the simultaneous determination of 4 non-steroidal anti-inflammatory drug (NSAID) residues, including flunixin meglumine, meloxicam, diclofenac sodium and ketoprofen, in mutton muscle was developed using high performance liquid chromatography assisted by ultrasonic-microwave extraction. The NSAIDs were extracted with acidified ethanol and purified by a diatomite column. The subsequent analysis of NSAIDs was achieved on a Hypersil C18 column (250 mm×4.6 mm, 5 μm) with the mobile phase of acetonitrile-0.2% triethylamine (40:60, v/v, pH 3.5 adjusted by phosphoric acid) at a flow rate of 0.8 mL/min at 30 ℃. The detection wavelength was set at 255 nm. The 4 NSAIDs were well separated within 20 min. The correlation coefficients for 4 NSAIDs were from 0.9993 to 0.9998 with the limits of detection (LOD, S/N=3) of 5~10 μg/kg and the limits of quantification (LOQ, S/N=10) of 15~30 μg/kg. The recoveries were in the range of 65.3%~99.6% with the relative standard deviations (RSDs) less than 15%. This method is simple, rapid and highly sensitive, and can meet the requirement for the qualitative and quantitative analysis.