摘要
为了快速准确地检测甜蜜素的含量,采用稳定同位素内标试剂与同位素稀释质谱法结合的检测技术,可以在保证高灵敏度的同时,又具有抗干扰能力强、快捷高效等优点。其中,稳定同位素标记甜蜜素作为内标试剂,是该方法的关键。本文以重水(D2O)和环己酮为起始原料,经过碱催化的氢-氘同位素交换、还原胺化、磺酰化等关键反应步骤,得到四氘代环己基氨基磺酸钠。该产物经核磁共振(1H NMR)和质谱(MS)表征确认,氘同位素丰度大于99%。该合成方法简单成熟,原料廉价易得,副反应少,产物同位素丰度高,适合作为内标试剂用于甜蜜素的定性定量分析。
Stable isotope labeled internal standards combined with isotope dilution mass spectrometry can offer an analytical method with good accuracy and precision for the detection of sodium cyclamate.A novel deuterium-labeled sodium cyclamate was synthesized from cyclohexanone using heavy water(D2O)as deuterium source.The synthesis procedure featured key steps such as hydrogen-deuterium exchange,reductive amination,and sulfonylation reaction,and had the advantages of cheap and easily available starting materials,less side reactions and high isotope abundance.The deuterated product was confirmed by nuclear magnetic resonance(1H NMR)and tandem mass spectrometry(MS)characterization with more than 99 atom%deuterium isotope abundance,which can be used as stable isotope-labeled MS internal standards for qualitative and quantitative analysis.
作者
邱婷
张曙盛
朱苏珍
郭寅龙
QIU Ting;ZHANG Shusheng;ZHU Suzhen;GUO Yinlong(Shanghai Institute of Organic Chemistry,Chinese Academy of Sciences,Shanghai 200032,China;Innovation Research Institute of Traditional Chinese Medicine,Shanghai University of Traditional Chinese Medicine,Shanghai 201203,China)
出处
《同位素》
CAS
2020年第5期273-278,共6页
Journal of Isotopes
关键词
稳定同位素标记
甜蜜素
氢-氘交换反应
质谱内标试剂
stable isotope labeling
sodium cyclamate
H-D exchange reaction
MS internal standards
