摘要
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HypersilC18柱(250mm×4.6mm,5μm),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pH3.5),流速为0.8mL/min,检测波长为255nm。4种非甾体抗炎药能够在20min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5～10μg/kg,定量限(S/N=10)为15～30μg/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。
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 C18column（250 mm×4.6 mm,5μm）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 from0.999 3 to 0.999 8 with the limits of detection（LOD,S/N=3）of 5-10 μg/kg and the limits of quantification（LOQ,S/N=10）of 15-30μg/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.
出处
《色谱》
CAS
CSCD
北大核心
2010年第11期1056-1060,共5页
Chinese Journal of Chromatography
基金
上海市教育委员会重点学科建设项目(项目编号:J50704)
关键词
超声波-微波辅助提取
高效液相色谱
非甾体抗炎药
羊肉
ultrasonic-microwave assistant extraction
high performance liquid chromatography（HPLC）
non-steroidal anti-inflammatory drugs
mutton muscle
