丁烯氟虫腈在油菜中残留分析方法的研究

在建立油菜中丁烯氟虫腈残留分析方法的实验中,在添加丁烯氟虫腈浓度为0.05、0.10、0.50μg/ml的油菜样品中分别加入60 ml不同提取溶剂,比较不同提取溶剂对丁烯氟虫腈残留添加回收率的影响。结果表明,乙腈提取效果最好。以乙腈为提取剂提取的丁烯氟虫腈残留液,通过柱层析(中性氧化铝与活性炭的混合物为柱填料)净化,气相色谱测定,得出氟虫腈的最小检测量为2×10-13g。油菜中丁烯氟虫腈(0.05~0.50 mg/kg)的添加回收率为91.12%~93.21%,变异系数是6.01%~13.20%。方法的准确性、灵敏度均达到农药残留分析的要求。

Studies on Analysis Method of Butylene Fipronil Residues in Rape

In the experiment of establishing the method of analyzing butylene fipronil residues in rape,the different extraction solvents at 60 ml were added with in the rape samples added with butylene fipronil at 0.05,0.10,0.50 μg/ml and the effect of the different extraction solvents on the recovery rate of adding butylene fipronil residues were compared.Results showed that the extraction effect of acetonitrile was best.The extracts of butylene fipronil residues extracted by acetonitrile were purified by column chromatography(with the mixture of neutral alumina and activated carbon as filling materials) and determined by gas chromatography.The minimum detective amount of fipronil in rape was 2×10-13 g.The recovery rate of adding butylene fipronil(0.05～0.50 mg/kg) residues varied from 91.12% to 93.21% and the coefficient of variation was from 6.01% to 13.2%.The accuracy and sensitivity of the method accorded with the requirements of residue analysis of pesticide.