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| Determination of Fipronil and Its Metabolites in Rice Fishing Water Samples by SPE/UPLC－MS/MS |
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| DOI： |
| KeyWord:ultra performance liquid chromatography－tandem mass spectrometry solid-phase extraction rice fishing water fipronil and its metabolites |
| Author | Institution |
| MA Li-sha，ZHENG Guang-ming，YIN Yi，XIE Wen-ping，SHAN Qi，LIN Jia-wei，LI Li-chun，LIU Shu-gui，ZHAO Cheng，DAI Xiao-xin，WEI Lin-ting |
Guangdong Provincial Key Laboratory of Aquatic Animal Immunology and Sustainable Aquaculture，Key Laboratory of Prevention and Control for Aquatic Invasive Alien Species，Ministry of Agriculture and Rural Affairs， Pearl River Fisheries Research Institute，Chinese Academy of Fishery Sciences，Guangzhou ，China |
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| Abstract: |
| A solid-phase extraction（SPE）/ultra performance liquid chromatography－tandem mass spectrometry（UPLC－MS/MS） was developed for the determination of residues of fipronil（FIP） and its metabolites（FIPS），i.e．fipronil desulfinyl，fipronil sulfone and fipronil sulfide in rice fishing water．According to the complicated properties of the testing chemicals and the impurities of rice fishing water samples，a new type of filter membrane was selected for the pretreatment of water samples，and the following extraction method was successfully exploited after a series of preliminary experiments．Furthermore，the SPE conditions and nitrogen blowing temperatures were optimized to ensure the high efficiency of extraction and high purification quality of extraction．In brief，rice fishing water samples were firstly filtered by using glass fiber filter paper，then enriched and purified with Supelco ENVI－18 solid-phase extraction column，and finally eluted with acetonitrile．The target compounds were separated on a SB－C18 column（2.1 mm × 100 mm，1.8 μm），and subsequently determined using an electrospray ionization source in the negative ion multiple reaction monitoring（MRM） mode．The calibration curves for target compounds were linear in the range of 0.5－100 ng/mL with correlation coefficients（r2） more than 0.998．The limits of detection（LODs） and quantitation（LOQs） were 0.5 ng/L and 1.5 ng/L，respectively．The average recoveries for target compounds ranged from 81.6% to 105%，with relative standard deviations（RSDs） of 3.5%－7.0%．The proposed method was applied to the determination of FIP and FIPS in thirteen authentic water samples collected from the rice fishing areas，of which one was found containing fipronil and fipronil sulfone．The proposed method is simple，sensitive，cost-effective and efficient，and could provide technical support for the environmental monitoring and risk assessment of FIP and FIPS in rice fishing systems and their food products. |
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