高压液相色谱法测定水产品中呋喃苯烯酸钠残留

Determination of residues of sodium nifurstylenate in aquatic products by high pressure liquid chromatography

中文关键词:  呋喃苯烯酸钠  水产品  高压液相色谱法

英文关键词:sodium nifurstylenate  aquatic products  high pressure liquid chromatography

中文摘要:

      目的 建立高效液相色谱法测定水产品中呋喃苯烯酸钠残留量的分析方法。方法 水产品样品经0.5%甲酸乙腈（v/v）提取后，氨水、正己烷液-液萃取去除杂质，Zorbax SB-C18为分析柱，0.1%甲酸∶乙腈（58:42，v/v）为流动相，经DAD检测器（λ=398 nm）测定，基质标准溶液外标法定量。结果 方法的线性范围为50～1000 μg/L，相关系数r＞0.998，检出限5 μg/kg，定量限10 μg/kg，在10 ~ 100 μg/kg添加水平下平均回收率为87.1% ~ 102%，相对标准偏差（relative standard deviation，RSD）为4.3% ~ 8.4%。结论 该方法能满足水产品中呋喃苯烯酸钠残留量测定的需要。

英文摘要:

      Objective To establish an analytical method for the determination of sodium nifurstylenate in aquatic products by high performance liquid chromatography method. Method Samples were extracted by 0.5% formic acid-acetonitrile（v/v）, followed by clean-up by liquid-liquid extraction with ammonium hydroxide and n-hexane. A Zorbax SB-C18 column was adopted with the mobile phase of 0.1% formic acid- acetonitrile（58:42，v/v）. Sodium nifurstylenate was detected by DAD detector at 398 nm, and quantitively analysed by external standard. Results The method showed a good linearity in the range of 50-1000 μg/L with the correlation coefficients over 0.998. The limit of detection（LOD） was 5 μg/kg, and the limit of quantitation(LOQ) was 10 μg/kg. The average recoveries were 87.1%-102% at the spiked level of 10-100 μg/kg with the relative standard deviation (RSD) of 4.3%-8.4%. Conclusion This method can meet the requirement of fast and accurate determination of sodium nifurstylenate in aquatic products.