顶空气相色谱法测定丙硫异烟胺中三氯甲烷残留量

Determination of Chloroform Residue in Protionamide by Headspace Gas Chromatography

目的建立丙硫异烟胺中三氯甲烷(CHCl3)残留量的测定方法。方法顶空进样色谱法,采用DM-1毛细管柱(60m×0.32mm,5μm)。结果空白溶剂无干扰,检测限为0.03μg/mL,0.006～0.018mg/mL的范围内线性关系良好(r=0.9992),平均回收率为99.7%(RSD=1.5%,n=9),3批样品三氯甲烷残留量均符合规定。结论经方法学试验,该方法灵敏、准确、可靠,适用于本品三氯甲烷残留量的测定。

Objective To establish a GC method for the determination of chloroform residue in protionamide.Methods A headspace gas chromatography method was developed using a DM-1 capillary column（60m×0.32mm,5μm）.Results The blank solvent was non-interfering.The detection limit was estimated to be 0.03μg/mL.The quality concentration of 0.006-0.018mg/mL show the good linear relationship（r=0.9992）.The average recovery was 99.7%（RSD=1.5%,n=9）.The chloroform residues of the samples were up to specification.Conclusion The method was sensitive,accurate,reliable and applicable to the determination of chloroform residue in protionamide.