烯啶虫胺在棉花和土壤环境中的残留及.docVIP

烯啶虫胺在棉花和土壤环境中的残留及消解动态研究 李增梅, 邓立刚*, 赵善仓, 张树秋, 郭长英, 梁京芸, 董燕婕 (山东省农业科学院农业质量标准与检测技术研究所, 山东省食品质量与安全检测技术重点实验室, 济南 250100) 摘 要: 目的 建立操作简单、回收率较高的净化方法, 并应用该净化方法, 建立烯啶虫胺的高效液相色谱(HPLC)检测方法, 研究其在棉叶和土壤中的代谢残留及最终残留。方法 样品经甲醇/水(v:v, 60:40)提取, PCX固相萃取柱净化后, 经Waters Atlantis C18(3.6 mm×250 mm, 5 μm)色谱柱分离。结果 棉叶、棉籽、土壤中烯啶虫胺的最低检出浓度(LOQ)均为0.01 mg/kg; 在0.02~10 μg/mL范围内烯啶虫胺的锋面积与质量浓度的线性关系良好, R=0.9999。在棉叶、棉籽和土壤样品中三个不同浓度水平的添加回收率在71.5%~94.5%之间, RSD为2.9%~6.5%。代谢结果表明, 烯啶虫胺在棉叶和土壤中的消解半衰期分别为山东2.8~5.1天, 浙江2.1~4.3天; 最终残留结果表明, 烯啶虫胺在棉籽和土壤中的最终残留量均未检出。结论 该方法简便、准确可靠, 适用于棉叶和土壤中烯啶虫胺含量测定, 并且烯啶虫胺属于易降解农药。 关键词: 液相色谱法; 烯啶虫胺; 棉花; 土壤; 残留 Residue decline study of nitenpyram in cotton and soil LI Zeng-Mei, DENG Li-Gang,*, ZhAO Shan-Cang, ZHANG Shou-Qiu,GUO Chang-Ying, LIANG Jing-Yun, DONG Yan-Jie (Key Laboratory of Test Technology on Food Quality and Safety of Shandong Province, Institute of Agricultural Quality Standards and Testing Technology Research, Shandong Academy of Agricultural Sciences, Jinan 250100, China) ABSTRACT: Objective To establish a method for the determination of nitenpyram in cotton leaves and soil by high performance liquid chromatography (HPLC). Degradation of nitenpyramin cotton and soil using this HPLC method was studied. Methods Samples were extracted by methanol/water (60:40, v:v), and then purified by PCX extraction column. The analysis were separated on a Waters Atlantis C18(3.6 mm×250mm, 5μm)and detected by HPLC. Results This method provided a high linearity of the working curve for calibration as well as repeatability and reproducibility. The limits of quantification (LOQ) were 0.01 mg/kg in cotton and soil. The correlation coefficient of the working curve for calibration was 0.9999 for the nitenpyram in the concentration range from 0.02 to 10 μg/mL. The recoveries of nitenpyram in cotton, seed and soil were 71.5%~94.5%, and RSD were 2.9%~6.5%. The results showed the half-lives of nitenpyram were 2.8~5.1 d at cotton, and 2.1~4.3 d in soil. The final residues of nitenpyram were