纯度标准物质定量分装冻干制备技术评估研究

Research and evaluation of quantitative packaging lyophilization preparation technique for purity reference materials

中文关键词:  标准物质  稳定性  纯度  冻干

英文关键词:reference material  stability  purity  lyophilization

中文摘要:

      目的 选取代表性农药品种, 建立和评估一种新型纯度标准物质定量分装冻干制备技术。方法 通过溶液制备与定量分装、冻干、复溶及色谱法检测, 评估样品冻干复溶回收率、瓶间均匀性与稳定性。结果 丙硫克百威及毒死蜱2种农药品种的应用效果良好, 冻干复溶回收完全, 样品均匀性良好。通过40 ℃下加速稳定性实验, 与溶液样品比较, 样品稳定性显著改善。毒死蜱和甲基嘧啶磷2种农药品种则出现冻干复溶回收不完全现象。结论 该技术对于低蒸汽压和高沸点的有机纯度标准物质具有较高应用价值, 可降低纯品标准物质的分装量至1 mg以下并在使用环节通过复溶实现完全移取, 避免纯物质原料浪费。在保证均匀性的同时, 可提高标准物质稳定性。

英文摘要:

      Objective To establish and evaluate a new quantitative packaging lyophilization preparation technique for purity reference materials by selecting typical pesticides as research objects. Methods Following by solution preparation, quantitative packaging, lyophilization and re-dissolution, the recovery, between-unit homogeneity and stability were evaluated. Results The method could be well applied for pesticides of benfuracarb and chlorpyrifos with satisfactory recovery and homogeneity. Compared with solution samples, the stability was significantly improved under 40 ℃ accelerating stability assessment condition. Poor recoveries were observed for two other pesticides of pirimiphos-methyl and dichlorvos. Conclusion This technique is valuable for purity reference materials with low vapor pressure and high boiling point. The packaging amount can be reduced to less than 1 mg and completely transferred through re-dissolution during use, to avoid waste of pure materials. The stability of reference materials can be enhanced with homogeneity guarantee.