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0.5~25mg/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(R。)为0.9997,方法检出限(LOD)为0.01mg/L,定量限(LOQ)为0.1mg/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16.48mg/L3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。
The major impurity of imidacloprid technical material named 1, 3-bis-[ (6-chloro-3- pyridylmethyl)-N-nitroimidazolidin-2-ylideneamine3 (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( RE --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.