1, 3-双[1-(6-氯-3-吡啶基甲基)-N-硝基亚咪唑烷-2-基胺]的合成及高效液相色谱分析

合成了吡虫啉原药中的主要杂质——1,3-双[1-(6-氯-3-吡啶基甲基)-N-硝基亚咪唑烷-2-基胺] (BPMNA),并建立了BPMNA的高效液相色谱定量分析方法。结果表明:在质量浓度为0.5~25 mg/L范围内,BPMNA的质量浓度与峰面积之间呈良好的线性关系,决定系数(R2)为0.999 7,方法检出限(LOD)为0.01 mg/L,定量限(LOQ)为0.1 mg/L,5次平行测定的相对标准偏差(RSD)小于1.0%,在8.24、12.36和16.48 mg/L 3个添加水平下,以吡虫啉标样为基质的添加回收率在99%~101%之间。该方法简单实用,可直接应用于商品化吡虫啉原药和制剂中BPMNA的含量检测。

Synthesis of 1, 3-bis-[(6-chloro-3-pyridylmethyl)-N-nitroimidazolidin-2-ylideneamine] and analysis by high performance liquid chromatography

The major impurity of imidacloprid technical material named 1,3-bis-[(6-chloro-3-pyridylmethyl)-N-nitroimidazolidin-2-ylideneamine](BPMNA) was synthesized and a rapid high performance liquid chromatography (HPLC) analytical method for BPMNA has been established.The results showed that the regression of the peak area of BPMNA on the concentration well fitted a linear relationship(R²=0.999 7) at the concentration levels ranging from 0.5 to 25.0 mg/L.The LOD and LOQ were 0.01 and 0.1 mg/L,respectively.The relative standard deviations (RSD) for 5 parallel determinations were less than 1.0%.Standard additions of BPMNA to imidacloprid standard as matrix lead to excellent recoveries of 99%-101%.The method presented here stands out as simple and easily applicable,which can be applied directly to commercial imidacloprid formulations to provide a rapid and efficient quality control.