气相色谱法快速测定蛋中氟虫腈及其代谢物

Determination of fipronil and its metabolites in eggs by gas chromatography

中文关键词:  氟虫腈  代谢物  气相色谱法  蛋  残留

英文关键词:fipronil  metabolites  gas chromatography  eggs  residue

中文摘要:

      目的 建立气相色谱法同时快速测定蛋中氟虫腈及其代谢物残留量的分析方法。方法 鸡蛋中的氟虫腈及其代谢物氟甲腈、氟虫腈硫醚、氟虫腈砜残留经乙腈提取, 盐析, 固相萃取小柱净化, 采用气相色谱电子捕获检测器进行分离和测定, 外标法定量。结果 氟虫腈及其代谢物氟甲腈、氟虫腈硫醚、氟虫腈砜的检出限为0.2 μg/kg, 在0.2~200 μg/kg范围内, 线性相关系数大于0.9995。 在所添加3个质量浓度水平下, 方法的回收率在75.1%~102.0%, 相对标准偏差为4.3%~6.4%。结论 该方法简便、准确、重现性好, 适合对蛋中氟虫腈及其代谢物进行有效监测。

英文摘要:

      Objective To establish a rapid method for simultaneous determination of fipronil and its metabolites by gas chromatography. Methods The fipronil and its metabolites (fipronil-desulfinyl, fipronil-sulfide, fipronil-sulfon) in eggs were extracted by acetonitrile, salted out and cleaned up by solid phase extraction column, respectively, separated and determined by gas chromatography-electron capture detector and quantified by the external standard method. Results The limits of detection of fipronil and its metabolites were 0.2 μg/kg. The calibration curves were good linear between area and the concentration in range of 0.2-200 μg/kg with the correlation coefficient more than 0.9995. The average recoveries were 75.1%-102.0% at 3 spiked levels with relative standard deviation of 4.3%-6.4%. Conclusions This method is simple, accurate, and well reproducible, which can be effectively applied to the monitoring of fipronil and its metabolites in eggs.