A simple, sensitive, and efficient method has been developed for the determination of the seven neonicotinoid insecticides commercially available (imidacloprid, thiacloprid, clothianidin, thiamethoxam, acetamiprid, nitenpyram, and dinotefuran) and the main metabolite 6-chloronicotinic acid. Micellar electrokinetic chromatography (MEKC) mode was applied, using 48.5 cm of total length capillary (50 μm i.d.) with an extended light-path capillary (150 μm). The running electrolyte consisted of 25 mM sodium tetraborate buffer (pH 9.2) containing 120 mM of sodium dodecyl sulfate and 15% of methanol (v/v). A voltage of 27 kV and a temperature of 25 °C were applied. Samples dissolved in deionized water were hydrodynamically injected at 50 mbar for 12 s, achieving the analysis in less than 12 min. Diode array detection (DAD) was performed at 220, 254, and 270 nm, depending on the analyte. Two different methodologies as sample treatments were developed; for water samples, solid-phase extraction was checked using different cartridges (C18, Oasis® HLB, Oasis® HLB Prime, and Strata-X), being the best option Oasis® HLB for preconcentration and cleanup. In the case of soil samples, a simple solid–liquid extraction was applied using a mixture of 1:3 (v/v) acetonitrile/dichloromethane. Satisfactory linearity, trueness, and precision were achieved, with detection limits in the range of 0.1–0.4 μg L⁻¹ for river water and 1.0–2.9 μg kg⁻¹ for soil samples. Recoveries in the range of 80–107% for all of the assayed neonicotinoids in water samples of different origin and 73–92% for soil samples were achieved.

开发了一种简单、灵敏、高效的方法，用于测定市售的七种新烟碱类杀虫剂（吡虫啉、噻虫啉、噻虫胺、噻虫嗪、啶虫脒、烯啶虫胺和呋虫胺）和主要代谢物 6-氯烟酸。应用胶束电动色谱 (MEKC) 模式，使用 48.5 cm 的总长毛细管（50 μm 内径）和延长的光路毛细管（150 μm）。运行的电解质由 25 mM 四硼酸钠缓冲液 (pH 9.2) 组成，其中含有 120 mM 十二烷基硫酸钠和 15% 甲醇 (v/v)。施加了 27 kV 的电压和 25 °C 的温度。溶解在去离子水中的样品在 50 毫巴下以流体动力学方式注入 12 秒，在不到 12 分钟的时间内完成分析。二极管阵列检测 (DAD) 在 220、254、和 270 nm，取决于分析物。开发了两种不同的样品处理方法；对于水样，使用不同的小柱（C18、Oasis® HLB、Oasis® HLB Prime 和 Strata-X）检查固相萃取，这是 Oasis® HLB 预浓缩和净化的最佳选择。在土壤样品的情况下，使用 1:3 (v/v) 乙腈/二氯甲烷的混合物进行简单的固液萃取。获得了令人满意的线性度、正确度和精密度，检测限范围为 0.1–0.4 μg L 在土壤样品的情况下，使用 1:3 (v/v) 乙腈/二氯甲烷的混合物进行简单的固液萃取。获得了令人满意的线性度、正确度和精密度，检测限范围为 0.1–0.4 μg L 在土壤样品的情况下，使用 1:3 (v/v) 乙腈/二氯甲烷的混合物进行简单的固液萃取。获得了令人满意的线性度、正确度和精密度，检测限范围为 0.1–0.4 μg L^-1用于河水，1.0–2.9 μg kg ^-1用于土壤样品。不同来源的水样中所有检测到的新烟碱类物质的回收率为 80-107%，土壤样品的回收率为 73-92%。