稳定同位素氘标记D_6-结晶紫的合成及表征  

Synthesis and Characterization of Stabe Isotope Deuterium-labeled D_6-Crystal Violet

作　　者：杨维成[1] 齐庆瑞[2] 李美华[1] 杨超[1] 罗勇[1] 

机构地区：[1]上海化工研究院技术开发中心,上海200062 [2]新疆教育学院职业技术分院,乌鲁木齐830063

出　　处：《应用化学》2014年第3期262-267,共6页Chinese Journal of Applied Chemistry

基　　金：科技部转制院所专项(2012EG116257);长三角科技联合攻关项目(10595812100);质检公益性行业科研专项项目计划(201310140)~~

摘　　要：以D4-甲醇为原料,通过酯化、N-甲基化、缩合等过程合成得到稳定同位素标记D6-结晶紫,利用均匀设计法,研究了投料比、三氯氧磷用量、反应温度和反应时间对合成结晶紫的影响。实验数据通过多元回归分析,得出了优化的工艺条件。目标产物的结构经质谱(MS)、核磁(NMR)和高效液相色谱(HPLC)等表征,化学纯度高于98.0%,同位素丰度高于99.5%(atom D),可作为食品安全领域检测用同位素内标试剂。An efficient synthesis of deuterium labeled crystal violet [ D6 ] with CD30D as the common substrate was developed via esterification, N-methylation and condensation. Taking advantage of the uniform design method, the effects of feed ratio, the amount of phosphorus oxychloride, reaction temperature and reaction time on the yield of crystal violet were investigated. The optimized reaction parameters were found by using quadratic polynomial regression analysis based on the data obtained from experiments. The target product was characterized by MS, NMR and higher than 99.5 % （atom D）. HPLC. Its chemical purities is higher than 98.0% and isotopic enrichment is This product could be used as an internal standard in the field of food safety.

关 键 词：稳定同位素标记 结晶紫 均匀设计 表征 

分 类 号：O628.2[理学—有机化学] TQ421.6[理学—化学]