稳定同位素标记D4-罗丹明B的合成及表征

doi:10.11944/j.issn.1000-0518.2016.08.150374

摘要/Abstract

摘要：

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。

关键词: 稳定同位素标记, D₄-罗丹明B, 合成, 内标, 食品安全

Abstract:

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.

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

王浩然, 杨维成, 涂亚辉, 杨超, 方超, 李美华, 罗勇, 吴范宏. 稳定同位素标记D₄-罗丹明B的合成及表征[J]. 应用化学, 2016, 33(8): 939-944.

WANG Haoran, YANG Weicheng, TU Yahui, YANG Chao, FANG Chao, LI Meihua, LUO Yong, WU Fanhong. Synthesis and Properties of Stable Isotope Deuterium Labeled D₄-Rhodamine B[J]. Chinese Journal of Applied Chemistry, 2016, 33(8): 939-944.

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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

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