Determination of fipronil and its metabolites in eggs by UPLC-QqLIT-MS/MS with multistage mass spectrometry mode

AbstractA fast, sensitive, and reliable method for the determination of fipronil and its metabolites (fipronil-sulfone, fipronil sulfide, and fipronil-desulfynil) in eggs was developed by a modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) pretreatment method and ultra-performance liquid chromatography-quadrupole-linear ion trap mass spectrometry (UPLC-QqLIT-MS/MS). The proposed multistage mass spectrometry (MS3) method provides sufficient sensitivity and excellent reproducibility. The four analytes were separated by a Waters ACQUITY UPLC® BEH C18 column and detected by AB Sciex QTRAP® 5500. The mean recoveries for the four analytes ranged from 90.7% to 105% with relative standard deviations (RSDs) of 0.7% to 4.9%. The calibration curve showed a good linearity within the concentration range of 0.05 to 20 ng/mL. The correlation coefficients (R2) were higher than 0.999. The limits of detection (LODs) obtained from the experimental results for fipronil, fipronil-sulfone, fipronil-sulfide, a...