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采用乙腈提取水稻植株、土壤、田水、稻米中的吡虫啉和噻嗪酮,经氟罗里硅土固相萃取小柱和氨基固相萃取小柱净化,分别采用反相HPLC-DAD和GC-μECD检测。结果表明,样本中吡虫啉和噻嗪酮添加回收率均在89.2%～106.4%,变异系数为1.7%～13.2%,吡虫啉最小检出量为5×10-10g,噻嗪酮最小检出量为2×10-11g。吡虫啉在植株、土壤和田水的半衰期分别为1.7～2.2、2.3～2.8和1.3～2.0 d;噻嗪酮在植株、土壤和田水的半衰期分别为2.3～2.9、9.4～12.7和1.8～2.3 d。16%吡虫啉.噻嗪酮可湿性粉剂按照推荐施用剂量,最多施药两次,最后一次施药距采收间隔期为14 d,收获稻米中吡虫啉的最终残留量均低于0.05 mg.kg-1,噻嗪酮的最终残留量均低于0.3mg.kg-1。两种农药的最终残留量均未超过我国规定的最大残留限量值。
Acetonitrile was used to extract imidacloprid and buprofezin from rice plants, soil, field water and rice, purified by flurolidine solid-phase extraction cartridges and amino-solid phase extraction cartridges, reversed-phase HPLC-DAD and GC- μECD test. The results showed that the recoveries of imidacloprid and buprofezin in the samples ranged from 89.2% to 106.4%, the coefficient of variation was 1.7% ~ 13.2%, the minimum detectable amount of imidacloprid was 5 × 10-10g, the minimum detectable amount of buprofezin was 2 × 10-11g. The half-lives of imidacloprid in plant, soil and field water were 1.7-2.2, 2.3-2.8 and 1.3-2.0 d, respectively. The half-lives of buprofezin in plant, soil and field water were 2.3-2.9, 9.4-12.7 and 1.8-2.3 d, respectively. 16% imidacloprid. Buprofezin WP According to the recommended dosage, up to twice application, the last application interval 14 days, the final residues of imidacloprid harvest rice were less than 0.05 mg.kg- 1, the final residues of buprofezin were lower than 0.3mg.kg-1. The final residues of the two pesticides did not exceed the maximum residue limits prescribed by our country.