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作 者:时若寒 刘洪斌[2] 叶子煜 雷春娟[2] 韩雪[1] 蔡英华[2] SHI Ruohan;LIU Hongbin;YE Ziyu;LEI Chunjuan;HAN Xue;CAI Yinghua(School of Food and Biology,Hebei University of Science and Technology,Shijiazhuang 050018,China;China Animal Disease Prevention and Control Center,Beijing 102618,China)
机构地区:[1]河北科技大学食品与生物学院,石家庄050018 [2]中国动物疫病预防控制中心,北京102618
出 处:《分析试验室》2023年第6期760-766,共7页Chinese Journal of Analysis Laboratory
基 金:兽药残留检测标准物质研制(2013FY113300-1)项目资助。
摘 要:制备和纯化了4-氯-2-甲基苯胺标准品。通过高效液相色谱、红外光谱、紫外光谱、质谱、核磁共振谱图的测定,确认了其化学结构。使用质量平衡法和定量核磁共振方法联合定值,并进行了均匀性、短期和长期稳定性的评估和特征值的表征。定值结果为99.8%±0.09%(k=2, P=0.95)。该标准品量值具有溯源性和准确性,可以为监测杀虫脒提供可靠的标样支撑。A preparation and purification process was established for the new reference material of 4-chloro-2-methylaniline with high purity.The structure of the compound was determined by high performance efficiency liquid chromatography,infra-red spectrum,ultraviolet spectrum,mass spectrum and nuclear magnetic resonance spectrum.The purity of this compound was detected by combining the mass balance method and the quantitative NMR and evaluated by homogeneity,short-term and long-term stability.The purity value of 4-chloro-2-methylaniline was determined as 99.8%±0.09%(k=2,P=0.95).The value of this reference material was traceable and accurate,which can provide reliable standard sample support for the detection of chlordimeform residue.
关 键 词:4-氯-2-甲基苯胺 标准品 均匀性 稳定性 不确定度
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