relative standard

tandem mass

flow injection

pesticides

pesticide residues

organochlorine pesticides

surface waters

Chemosphere

In the previous decade, neonicotinoids (NEOs) and fipronil (FIP) have received increasing attention as environmental pollutants because the high toxicity of these insecticides to nontarget arthropods has been recognized. In this study, a new method was developed for the simultaneous determination of seven NEOs and FIP and its metabolites (FIPs) in seawater and river water samples using disk-based solid-phase extraction (SPE) and high-performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS). The optimization of disk-based SPE extraction and HPLC separation parameters of target analytes was investigated. Under optimal conditions, the low limit of quantitation (LOQ) of 11 target analytes in actual water samples ranged from 0.05 ng/L to 0.50 ng/L. Satisfactory absolute recoveries (58.9%–109.9%), precision (relative standard deviations, ≤13.3%), and linearity (R2 ≥ 0.995) were also achieved, thereby indicating that the developed method would be suitable to determine the target NEOs and FIPs in seawater and river water. Finally, the proposed method was applied to determine the amounts of these insecticides in authentic environmental water samples collected from Jiaozhou Bay, China, and its adjacent rivers. Nitenpyram, thiamethoxam, imidacloprid, clothianidin, and acetamiprid were detected, as well as FIPs in seawater and river water samples. This study is the first to report that NEOs and FIPs are detected in the coastal seawater. The total concentration of these insecticides ranged from ≤LOD to 11.19 ng/L, which indicates that these pesticides are eventually discharged into the marine environment. Therefore, it is necessary to investigate the temporal spatial distribution, migration and transformation, environmental fate, and bioavailability of these pesticides in further studies.

Simultaneous determination of neonicotinoids and fipronil and its metabolites in environmental water from coastal bay using disk-based solid-phase extraction and high-performance liquid chromatography–tandem mass spectrometry