固相萃取-高效液相色谱检测鸡蛋中氟虫腈及其代谢物

Determination of fipronil and its main metabolites in eggs by solid phase extraction-high performance liquid chromatography

中文关键词:  固相萃取  氟虫腈及其代谢物  高效液相色谱法  鸡蛋

英文关键词:solid phase extraction  fipronil and its metabolites  high performance liquid chromatography  egg

中文摘要:

      目的 建立固相萃取-高效液相色谱法测定鸡蛋中氟虫腈农药及其主要的代谢物氟虫腈砜、氟虫腈亚砜、氟甲腈的分析方法。方法 选用含1%甲酸的乙腈溶液(V:V)为提取溶剂, 用石墨化碳黑/氨基固相萃取小柱萃取净化, 用乙腈作洗脱剂, 并在以甲醇-水(67:33, V:V))为流动相的条件下进行高效液相色谱检测。结果 该方法的线性范围为0.3~10.0 μg/g, 4种目标物的检测限均在0.05~0.10 μg/g之间。通过对实际鸡蛋样品加标检测, 得到加标回收率在80.9%~115.8%之间, 相对标准偏差均小于6.2%。结论 该方法精密度较高、稳定性良好、操作简便, 可用于鸡蛋样品中氟虫腈及其3种代谢物的测定。

英文摘要:

      Objective To establish a method for the determination of fipronil and its main metabolites residue involving fipronil sulfone, fipronil sulfide and fipronil desulfinyl in eggs by solid-phase extraction combined with high-performance liquid chromatography. Methods The target chemicals were extracted from the eggs by acetonitrile containing 1% (V:V)formic acid, and then cleaned by a PestiCarb/NH2 solid phase extraction cartridge using acetonitrile as eluent. Subsequently, high performance liquid chromatography equiped with a photo-diode array detecter was performed for the residue determination with methanol-water (67:33, V:V) as mobile phase. Results The linear range of the method was 0.310.0 μg/g. The detection limits of the 4 targets were between 0.05 and 0.10 μg/g. The established method was successfully used to determine the 4 targets in egg samples, and the recoveries ranged from 80.9% to 115.8% with the relative standard deviations less than 6.2%. Conclusion This method has high precision, good stability and is easy to operate. It can be applied for the determination of fipronil and its 3 kinds of metabolites in actual egg samples.