摘要
[目的]建立大豆中抑菌灵的毛细管柱气相色谱法。[方法]试样用丙酮提取。分别选用1:48、3:47、5:45的3种乙醚-正己烷体系,制备3支层析柱,用10 ml正己烷活化,各加入0.2 ml,2.5 mg/L的抑菌灵标准溶液,再分别用45 ml上述3种淋洗液体系淋洗,每5 ml收集1次,分别进样测回收率,以淋洗液体积(V)为横坐标,回收率(%)为纵坐标绘制淋洗曲线。比较后选择3:47乙醚-正己烷淋洗体系,淋洗体积为25 ml。经正己烷液液萃取后,用弗罗里硅土柱净化,经毛细管气相色谱柱分离(柱温采用程序升温方式,初始温度50℃,保持1 min;以25℃/min的速度升至125℃后,再以10℃/min的速度升至300℃,保持3 min。采用恒流条件下无分流进样),用ECD检测器测定。[结果]抑菌灵含量在0.05、0.25、0.5、1.0 mg/L范围内,峰面积与抑菌灵的浓度呈良好线性关系,线性方程为s=12 346C+63(r2=0.999 6)。以信噪比(S/N)为3计算抑菌灵的定性检出限为0.005 mg/kg;以信噪比(S/N)为10计算抑菌灵的定量检出限为为0.05 mg/kg。精密度测定表明,该方法具有较好的准确度和精密度。[结论]建立了大豆中抑菌灵的毛细管柱气相色谱法。该方法简单快速,灵敏度高,可满足粮谷中抑菌灵含量的测定要求,可在实际中应用和推广。
A method for the determination of dichlofluanid residue by Capillary Collumns Gas Chromatography was established in this study.Samples were extracted with acetone and subjected to through liquid-liquid extraction with N-hexane,and then they were cleanup with column that filled with florisil,subsequently separated by Capillary Column Gas Chromatography,and the electron capture detector （ECD） was used for detection.The detection limit of this method was 0.005 mg/kg （S/N=3）,and this method was rapid,sensitive and accurate,and was applied in the determination of dichlofluanid residue in soybean.
关键词
抑菌灵
毛细管柱
气相色谱
大豆
Dichlofluanid
Capillary Collumns
Gas Chromatography
Soybean
