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Multi-residue analysis of systemic insecticides and their transformation products in environmental matrixes: Method
Junwu Xiong1, Youzhen Wang2, Yuqian Wu2
1School of Environmental Studies, China University of Geosciences, Wuhan 430078, China; MOE Key Laboratory of Groundwater Quality and Health, China University of Geosciences, Wuhan 430078, China; Hubei Key Laboratory of Yangtze Catchment Environmental Aquatic Science, China University of Geosciences, Wuhan 430078, China; State Key Laboratory of Geomicrobiology and Environmental Changes, China University of Geosciences, Wuhan 430078, China.
None:
A robust and sensitive analytical method was developed and validated for simultaneous determination of 38 systemic insecticides and their transformation products (TPs), including neonicotinoid insecticides (NNIs), fipronil (FIP) and their typical TPs in six environmental matrices, namely surface water, groundwater, wastewater, soil, sediment and sludge. The method integrated optimized extraction procedures for solid samples and solid-phase extraction (SPE) cleanup/enrichment with liquid chromatography-tandem mass spectrometry (LC-MS/MS), aiming to support the investigation of the occurrence and environmental behaviour of these systemic insecticides and their TPs in multimedia environment. The pre-treatment including the selection of SPE cartridges, sample pH, extraction reagents and procedures were optimized, and acceptable recoveries (> 60% for 35 target compounds), low method detection limits (surface water and groundwater: 0.003-0.319 ng/L, wastewater: 0.007-0.637 ng/L, soil and sediment: 0.42-82.1 ng/kg, and sludge: 0.38-205 ng/kg) and excellent precision (intra-day repeatability: RSDs < 5% for all analytes; inter-day reproducibility: RSDs < 10% for > 90% of analytes) were achieved. Optimised methods were applied to analyse NNIs, FIP and TPs in surface water, sediment and soil from the Dawen River Basin, groundwater in karst springs from Zigui, and wastewater and sludge from wastewater treatment plants in Wuhan, China. The results revealed that TPs had comparable or even higher concentrations and detection frequencies than their parents in all tested matrices, with the concentrations of certain NNI-TPs (e.g., Desnitro-imidacloprid: 2368 ng/L and Thiamethoxam-urea: 1882 ng/L) being among the highest reported in surface water worldwide. The developed method provides a tool to comprehensively investigate NNIs, FIP and their TPs in common environmental matrices, and the preliminary findings in the characterization of environmental samples emphasise the importance of incorporating TPs into investigations in future environmental studies.
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