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

作　　者：张磊 李筱翠 纪洁[3] 国振[3] 卢晓华[3] ZHANG Lei;LI Xiao-Cui;JI Jie;GUO Zhen;LU Xiao-Hua(School of Science,Beijing University of Chemical Technology,Beijing 100029,China;Beijing Prevention and Treatment Hospital of Occupational Disease for Chemical Industry,Beijing 100051,China;National Institute of Metrology,Beijing 100029,China)

机构地区：[1]北京化工大学理学院,北京100029 [2]北京市化工职业病防治院,北京100051 [3]中国计量科学研究院,北京100029

出　　处：《食品安全质量检测学报》2018年第15期3922-3926,共5页Journal of Food Safety and Quality

基　　金：国家重点研发计划项目(2017YFF0205804)~~

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。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.

关 键 词：标准物质 稳定性 纯度 冻干 

分 类 号：TQ450.6[化学工程—农药化工]