多壁碳纳米管-气相色谱/串联质谱法测定杨梅中氟虫腈及其代谢物残留量

Determination of Fipronil and Its Metabolites in Waxberry by Multi-walled Carbon Nanotube Coupled with Gas Chromatography-tandem Quadrupole Mass Spectrometry

建立杨梅中多壁碳纳米管-气相色谱/串联质谱法同时测定氟虫腈及其代谢物(氟甲腈、氟虫腈砜和氟虫腈亚砜)。样品经乙腈提取,多壁碳纳米管净化,气相色谱/串联质谱仪测定,基质外标法定量。氟虫腈及代谢物在10~500μg/L范围内具有良好的线性关系(r>0.99);在3个不同浓度加标水平下,氟虫腈及其代谢物的平均回收率为85.2%~104%之间,RSD为2.7%~8.1%之间,方法的定量限为0.1~0.5μg/kg之间。该方法简便、快速、准确、重现性好、灵敏度高,适用于杨梅中多种氟虫腈及其代谢物的同时检测。

A gas chromatography-tandem quadrupole mass spectrometry( GC-MS/MS) method was developed for the determination of fipronil and its metabolites in waxberry. The sample was extracted with acetonitrile, and then cleaned up using multi-walled carbon nanotube, and detected by GC-MS/MS. Fipronil and its metabolites were detected by multiple reaction monitoring(MRM)mode in the positive ion mode. The linear ranges were from 10 to 500μg/L with the correlation coefficients above 0.99 for both fipronil and its metabolites. The average recoveries of fipronil and its metabolites in waxberry at the three spiked levels were 85.5%~104% with the relative standard deviations of 2.7%~8.1%. The limits of detection were 0.1 ~0.5μg/kg. The method is rapid, accurate, reproducible, sensitive and easy to apply, and suitable for the determination of fipronil and its metabolites in waxberry.