稳定同位素氘标记D6-结晶紫的合成及表征

doi:10.3724/SP.J.1095.2014.30218

摘要/Abstract

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。

关键词: 稳定同位素标记, 结晶紫, 均匀设计, 表征

Abstract: An efficient synthesis of deuterium labeled crystal violet[D6] with CD3OD 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 HPLC. Its chemical purities is higher than 98.0% and isotopic enrichment is higher than 99.5%（atom D）. This product could be used as an internal standard in the field of food safety.

Key words: stabe isotope-labelling, crystal violet, uniform design, characterization

中图分类号:

杨维成, 齐庆瑞, 李美华, 杨超, 罗勇. 稳定同位素氘标记D₆-结晶紫的合成及表征[J]. 应用化学, DOI: 10.3724/SP.J.1095.2014.30218.

YANG Weicheng1, QI Qingrui2, LI Meihua1, YANG Chao1, LUO Yong1*. Synthesis and Characterization of Deuterium-labeled D₆-Crystal Violet[J]. Chinese Journal of Applied Chemistry, DOI: 10.3724/SP.J.1095.2014.30218.

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稳定同位素氘标记D₆-结晶紫的合成及表征

Synthesis and Characterization of Deuterium-labeled D₆-Crystal Violet

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