基质固相分散-高效液相色谱法测定小麦籽粒中吡虫啉和啶虫脒残留
Analysis of Imidacloprid and Acetamiprid Residue in WheatSeeds by Matrix Solid-Phase Dispersion and HighPerformance Liquid Chromatography
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摘要: 建立了以C18键合硅胶作为固相分散剂,高效液相色谱法同时测定小麦籽粒中吡虫啉和啶虫脒残留的分析方法。C18键合硅胶与样品一起研磨均匀制成基质固相分散柱,用乙腈淋洗,浓缩后用高效液相色谱检测。结果表明:吡虫啉在0.05~0.8 mg/L、啶虫脒在0.1~1.0 mg/L的范围内线性良好,相关系数分别为0.999 6、0.999 7。在0.05、0.1、0.5 mg/kg水平时,吡虫啉和啶虫脒的添加回收率分别在88.5%~98.4%和93.2%~98.9%之间,相对标准偏差分别在2.0%~3.8%和3.6%~9.8%之间,仪器最低检出量分别为0.1 ng和0.4 ng,方法最小检出浓度分别为0.04 mg/kg 和 0.1 mg/kg。该方法简便、快速、溶剂消耗少,满足农药残留分析的要求。Abstract: Analytical method using matrix solid-phase dispersion (MSPD) clean-up for the analysis of imidacloprid and acetamiprid in wheat seeds was developed.Wheat seed sample was mixed in a glass mortar with a bonded-phase solid support material.Then the solid support and sample were manually blended together using a glass pestle.The blended material was packed into a column containing activated C18 and eluted with acetonitrile.The eluate was concentrated and analyzed by high-performance liquid chromatography with ultraviolet detection.The linearity of response ranges of imidacloprid and acetamiprid was obtained from 0.05 to 0.8 mg/L and 0.1 to 1.0 mg/L, the correlation coefficient were 0.999 6 and 0.999 7, the recoveries ranged from 88.5% to 98.4% and from 93.2% to 98.9% respectively.At the fortified levels of 0.05, 0.1 and 0.5 μg/g, the relative standard deviations ranged from 2.0% to 3.8% and from 3.6% to 9.8%, the limit of detection were 0.1 ng and 0.4 ng,the limit of quantification were 0.04 mg/kg and 0.1 mg/kg,respectively.