Key Laboratory for Marine Bioactive Substances and Modern Analytical Technology, The First Institute of Oceanography, Ministry of Natural Resources, Qingdao, 266061, China.
Key Laboratory for Marine Bioactive Substances and Modern Analytical Technology, The First Institute of Oceanography, Ministry of Natural Resources, Qingdao, 266061, China; Laboratory for Marine Ecology and Environmental Science, Pilot National Laboratory for Marine Science and Technology (Qingdao), Qingdao, 266071, China.
Chemosphere. 2019 Nov;234:224-231. doi: 10.1016/j.chemosphere.2019.05.243. Epub 2019 Jun 1.
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 (R ≥ 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.
在过去的十年中，新烟碱类（NEOs）和氟虫腈（FIP）作为环境污染物受到了越来越多的关注，因为这些杀虫剂对非靶标节肢动物的高毒性已被认识到。在这项研究中，开发了一种新的方法，用于使用基于磁盘的固相萃取（SPE）和高效液相色谱-串联质谱（HPLC-MS/MS）同时测定海水中和河水中的七种 NEOs 和 FIP 及其代谢物（FIPs）。研究了基于磁盘的 SPE 萃取和目标分析物 HPLC 分离参数的优化。在最佳条件下，11 种实际水样中目标分析物的低定量限（LOQ）范围为 0.05 ng/L 至 0.50 ng/L。还实现了令人满意的绝对回收率（58.9%-109.9%）、精密度（相对标准偏差，≤13.3%）和线性（R≥0.995），从而表明该方法适用于测定海水中和河水中的目标 NEOs 和 FIPs。最后，该方法应用于测定中国胶州湾及其附近河流采集的真实环境水样中这些杀虫剂的含量。在海水中和河水中检测到了吡虫啉、噻虫嗪、噻虫啉、噻虫胺和乙虫腈以及 FIPs。本研究首次报道了沿海海水中检测到 NEOs 和 FIPs。这些杀虫剂的总浓度范围为≤LOD 至 11.19 ng/L，这表明这些农药最终被排放到海洋环境中。因此，有必要在进一步的研究中调查这些农药在时空分布、迁移转化、环境命运和生物利用度方面的情况。
