固相萃取-高效液相色谱法检测上海青(Brassica chinensis L.)中鱼藤酮的残留动态  

Residual Dynamics of Rotenone in Greengrocery by Solid-phase Extraction-High Performance Liquid Chromatography-UV Detection

作　　者：王苏宁[1] 李冠华[1] 李有志[1,2] 王平 陈银[1] 

机构地区：[1]湖南农业大学生物安全科技学院植物病虫害生物学与防控湖南省重点实验室,长沙410128 [2]湖南农业大学国家植物功能成分利用工程技术研究中心,长沙410128 [3]安徽芜湖市产品质量监督检验所,安徽芜湖241007

出　　处：《农药》2012年第4期278-280,286,共4页Agrochemicals

基　　金：国家自然科学基金(31071715);湖南省教育厅青年基金(09B048);湖南省烟草专卖局科技项目(09-11Aa03)

摘　　要：[目的]建立固相萃取-高效液相色谱-紫外（SPE-HPLC-UV）检测上海青中鱼藤酮的分析方法,对上海青中鱼藤酮的含量进行动态分析。[方法]样品先经乙腈提取,随后在乙腈提取液中加入氯化钠,盐析后过Florisil固相萃取柱富集净化,再用正己烷-乙醚（体积比3∶7）洗脱,最后以乙腈-水（体积比6∶4）为流动相,在290 nm下用高效液相色谱检测分析上海青中鱼藤酮的含量。[结果]该方法稳定可靠,检测物在0.05－10 mg/L范围内线性关系良好。在0.5－5 mg/kg范围内,平均加标回收率为85.9%－86.3%,检出限为0.05 mg/kg。田间推荐剂量和2倍推荐剂量分别施药,鱼藤酮在上海青中的原始沉积量分别为6.26、18.34 mg/kg。[结论]该化合物在田间降解速率快,在上海青中的半衰期分别为11.2、11.1 h。[Aims] An analytical method for residual dynamics of rotenone in greengrocery by solid-phase extraction （SPE） and high performance liquid chromatography （HPLC）-UV detection was described. [Methods] The sample was extracted by acetonitrile, salted out by adding sodium chloride, and cleaned with Florisil SPE using n-hexane-ethyl ether （3 ： 7, by vol） as eluents to provide adequate recovery of rotenone. The detection of rotenone was then carried out by HPLC-UV at 290 nm with acetonitrile and water （6 ： 4, by vol） as the mobile phase. [Results] The method was accurate, specific and sensitive, and had good linear correlations at the concentration range of 0.05-10 mg/L. The average recoveries and the relative standard deviation ranged from 85.9-86.3% at concentration range of 0.5-5 mg/kg. The limits of detection （LOD） of rotenone were 0.05 mg/kg. When greengrocery was treated with rotenone 2.5% EC at recommended dose and 2 times recommended dose, the original residues rotenone in greengrocery were 6.26 and 18.34 mg/kg. [Conclusions] The compound degraded fast in the field. The half-life of rotenone in greengrocery was 11.2 and 11.1 h.

关 键 词：鱼藤酮 固相萃取 高效液相色谱 紫外检测 上海青 残留动态 

分 类 号：S481.8[农业科学—农药学]