Simultaneous Determination of 6 Neonicotinoid Residues in Soil Using DLLME-HPLC and UV
SUN Bao-li, SHAN Hong, LI Yan-hua, ZENG Ya-ling, SHEN Xiu-li, TONG Cheng-feng
Institute of Environment and Sustainable Development in Agriculture, Chinese Academy of Agricultural Sciences; Key Laboratory of Agro-environment and Climate Change of Ministy of Agriculture, Beijing 100081, China
Abstract：A simple, cheap and rugged method was developed for simultaneous deter mination of 6 neonicotinoid residues in soil, including imidacloprid, acetamiprid, thiamethoxam, thiacloprid, clothianidin and nitenpyram. The soil sample was produced by dispersive liquid-liquid micro-extraction (DLLME) after extracted by the mixed solution of acetonitrile and CH2Cl2 (2∶1, φ). The analytes were separated by HPLC with Alltima TMC18 column (4.6 mm×250 mm，5 μm) and detected by PDA at 260 nm. External standard method was used for quantification. The results showed that good linearity was obtained with correlation coefficients between 0.998 2 and 0.999 9 in the range of 0.5～200 μg·L-1. The limits of detection (LODs) were in the range between 0.000 5 and 0.003 μg· mL-1(S/N=3). The method was validated with five soil samples spiked at three fortification levels (0.05, 0.1, 1.0 mg·kg-1) and recoveries were in the range of 55.3%～95.6% with RSD of 1.4%～7.0%. The effect of clean-up was evaluated by UV spectra and demonstrated that the method established is effective. In conclusion, this method is competent for the simultaneous analysis of 6 neonicotinoid residues in soil.
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