荧光胺柱前衍生-高效液相色谱法同时测定水产品中8种磺胺的残留量

Simultaneous determination of 8 kinds of sulfonamides residues in aquatic products by high performance liquid chromatography with fluorescence detection after pre-column derivatization

中文关键词:  水产品  磺胺类药物  高效液相色谱法  柱前衍生  荧光检测

英文关键词:aquatic products  sulfonamides  high performance liquid chromatography  pre-column derivatization  fluorescence detection

中文摘要:

      目的 建立荧光胺柱前衍生-高效液相色谱法同时测定水产品中8种磺胺类药物残留量的方法。方法 样品经乙酸乙酯提取, 2 mol/L盐酸反萃取, 正己烷脱脂, 经荧光胺衍生化反应静置20 min后采用3.5 μm反相色谱柱分离。采用荧光检测器进行检测、并选用磺胺-5-甲氧嘧啶为内标物进行内标法定量。结果 8种磺胺完全分离, 线性范围在2.5~200 μg/L内, 8种药物的线性相关系数均大于0.9992, 方法检出限为4.0~8.0 μg/kg; 在5个添加水平范围内, 平均回收率为83.2%~96.3%, 相对标准偏差为3.89%~8.80%(n=5)。结论 本方法重现性良好, 精密度、准确性均能满足水产品中8种磺胺类药物残留分析。

英文摘要:

      Objective To establish a method for the simultaneous determination of the 8 sulfonamide residues in aquatic products by high performance liquid chromatography (HPLC) with fluorescence detection after pre-column derivatization. Methods Samples were extracted with ethyl acetate, back-extracted with 2 mol/L hydrochloric acid, degreased with n-hexane, separated by a fluorescein derivatization reaction for 20 min, and then separated by a 3.5 μm reversed-phase chromatographic column. Fluorescence detector was used for detection and sulfanilamide-5- methoxypyrimidine was used as internal standard for quantitative analysis. Results Eight sulfonamides were completely separated, the linear range was 2.5–200 μg/L, and the correlation coefficients of the 8 drugs were all greater than 0.9992. The limits of detection were 4.0–8.0 μg/kg. The average recovery under the 5 spiked levels was 83.2%–96.3% with the relative standard deviation 3.89%–8.80%(n=5). Conclusion This method has good reproducibility, and the precision and accuracy can meet the analysis of sulfonamides residues in aquatic products.