[目的]采用高效液相色谱法,对不同提取、净化及色谱条件进行比较,建立氟铃脲在复杂基质棉叶及棉籽中的提取、净化及检测方法。[方法]对棉叶及棉籽中的组分进行气相色谱-质谱和高效液相色谱分析。[结果]干扰氟铃脲检测的主要物质为软脂酸、硬脂酸以及叶绿醇等色素成分。[结论怫罗里硅土和中性氧化铝混合层析柱能有效去除棉籽中的大部分脂肪酸以及棉叶中的大部分色素,脂肪酸和色素的净化率分别为89%。100%、29%~100%。通过净化后的棉叶及棉籽样品氟铃脲回收率均达到农药残留分析的要求。
[Aims] The extraction, purification and HPLC analysis method was developed for determination of hexaflumuron residues in complex matrix cotton leaf and seed by comparing different extraction, purification and chromatographic conditions. [Methods] The components of cotton leaf and seed were analyzed by GC-MS and HPLC. [Results] The main substances which interfere with the analysis of hexaflumuron were palmitic acid, octadecanoic acid and phytol, etc. [Conclusions] By using the Florisil and Alumina-N mixing chromatographic column, the fatty acid in the cotton seed and pigment in the cotton leaf can be removed, and the purifying rates were 89-100% and 29-100%, respectively. In addition, the recovery of hexaflumuron in cotton leaf and seed met the requirement of pesticide residue analysis.