Determination of Fipronil and Its Metabolites in Paddy fish Soil Using High Performance Liquid Chromatography Tandem Mass Spectrometry

Abstract

Residues of fipronil and its metabolites in paddy fish soil were detected using high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS). Samples were extracted with oscillation and acetonitrile in constant temperature, and subsequently purified by solid phase extraction using ENVI 18 column and 10 mg GCB. The target compounds were separated on an Agilent ZORBAX Extend C18 column (2.1 mm× 100 mm×1.8 μm), and determined using electrospray ionization (ESI) source at negative mode with multiple reation monitoring (MRM). The analytes were quantified with external standard using the matrix matched standard calibration curve method. The results indicated that the average spiked recoveries of fipronil, fipronil desulfinyl, fipronilsulfone and fipronilsulfide in paddyfish soil were 83.5%~110.3% with the relative standard deviations (RSDs) of 1.9%~11.5%. Good linearities were obtained in the range of 0.5~100 μg/L, and the correlation coefficients were greater than 0.998, the limits of detection (LODs) were 1.0 μg/kg, and the limits of quantification (LOQs) were 3.0 μg/kg. This method is simple, accurate and reliable, which can meet the detection requirements of fipronil and its metabolites in paddy fish soil.

Keywords

• high performance liquid chromatography tandem mass spectrometry (hplc-ms/ms)
• constant temperature oscillation extraction
• paddy fish soil
• fipronil
• fipronildesulfinyl
• fipronil sulfone
• fipronil sulfide