稳定同位素标记D<sub>4</sub>-罗丹明B的合成及表征

应用化学, 2016, 33(8): 939-944. doi: 10.11944/j.issn.1000-0518.2016.08.150374

稳定同位素标记D₄-罗丹明B的合成及表征

王浩然 ^a,b, , 杨维成 ^b,c, , 涂亚辉 ^b, , 杨超 ^b, , 方超 ^b, , 李美华 ^b,c, , 罗勇 ^b,c,*,, , 吴范宏 ^a,

a.上海应用技术学院上海 201418

b.上海化工研究院上海 200062

c.国家同位素工程技术研究中心-上海分中心上海 200062

通讯作者: 罗勇, real-luoyong@hotmail.com

录用日期: 2016-04-25

关键词：稳定同位素标记 , D₄-罗丹明B , 合成 , 内标 , 食品安全

Synthesis and Properties of Stable Isotope Deuterium Labeled D₄-Rhodamine B

Haoran WANG ^a,b, , Weicheng YANG ^b,c, , Yahui TU ^b, , Chao YANG ^b, , Chao FANG ^b, , Meihua LI ^b,c, , Yong LUO ^b,c,*,, , Fanhong WU ^a,

a.School of Chemical and Environmental Engineering, Shanghai Institute of Technology, Shanghai 201418, China

b.Shanghai Research Institute of Chemical Industry, Shanghai 200062, China

c.National Isotope Engineering Technology Research Center-Shanghai Sub-Center, Shanghai 200062, China

Correspondence author: Yong LUO, real-luoyong@hotmail.com

Keywords： stable isotope-labeling , D₄-rhodamine B , synthesis , internal standard , food safety

以全氘代邻二甲苯为同位素标记前体，经氧化得到的D₄-邻苯二甲酸与3-羟基-N,N-二乙基苯胺反应生成稳定同位素标记的D₄-罗丹明B，总收率36.9%。目标产物的结构经质谱（MS）、核磁（NMR）等技术手段表征确认，通过高效液相色谱确定化学纯度高于98.0%，同位素氘丰度大于98.0%。将其作为同位素内标试剂用于果汁中罗丹明B的残留检测，在0.05~50 mg/L范围内呈良好的线性关系，其检出限为5 μg/kg，回收率为96.4%~103.4%，相对标准偏差（RSD）为1.0%~1.2%，具有很高的灵敏度和准确性。为食品安全领域违禁色素的检测提供了一种可靠实用的方法。

This paper presents an efficient synthesis of stable isotope labeled D₄-rhodamine B from deuterated orthoxylene through oxidation and its reaction with 3-diethylaminophenol in 36.9% total yield. The deuterated product was confirmed by mass spectrometry(MS) and nuclear magnetic resonance(NMR). Its chemical purity is higher than 98.0% by high performance liquid chromatography(HPLC), and isotopic enrichment is higher than 98.0%(atom D). D₄-rhodamine B was used as internal standard for the determination of rhodamine B in orange juice with linear calibration curve of 0.05~50 mg/L, limit for determination of 5 μg/kg, recovery of 96.4%~103.4% and relative standard deviation(RSD) of 1.0%~1.2%. This method is proved to be accurate and sensitive for the determination of rhodamine in food safety.

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材料期刊网

稳定同位素标记D4-罗丹明B的合成及表征

Synthesis and Properties of Stable Isotope Deuterium Labeled D4-Rhodamine B

参考文献

稳定同位素标记D₄-罗丹明B的合成及表征

Synthesis and Properties of Stable Isotope Deuterium Labeled D₄-Rhodamine B