研究论文

dDNP溶融系统的自动化设计与研究

  • 曾祥政 ,
  • 陈俊飞 ,
  • 黄重阳 ,
  • 皮海亚 ,
  • 曹丽 ,
  • 黄臻 ,
  • 郭文龙 ,
  • 冯继文 ,
  • 刘朝阳
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  • 1.武汉轻工大学电气与电子工程学院,湖北 武汉 430023
    2.波谱与原子分子物理国家重点实验室,武汉磁共振中心,中国科学院精密测量科学与技术创新研究院,湖北 武汉 430071
    3.中国科学院大学,北京 100049
* Tel: 027-87199686, E-mail: chyliu@apm.ac.cn.

收稿日期: 2024-03-18

  网络出版日期: 2024-04-16

基金资助

国家自然科学基金重大科研仪器研制项目(22327901);国家重点研发计划项目(2022YFF0707001);国家自然科学基金青年项目(22204168);国家自然科学基金青年项目(12205352);曙光计划项目(2022010801020130);中国科学院B类先导专项(XDB0540301)

Design and Research of the dDNP Automated Dissolution System

  • ZENG Xiangzheng ,
  • CHEN Junfei ,
  • HUANG Chongyang ,
  • PI Haiya ,
  • CAO Li ,
  • HUANG Zhen ,
  • GUO Wenlong ,
  • FENG Jiwen ,
  • LIU Chaoyang
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  • 1. School of Electrical and Electronic Engineering, Wuhan Polytechnic University, Wuhan 430023, China
    2. State Key Laboratory of Magnetic Resonance and Atomic and Molecular Physics, Wuhan Center for Magnetic Resonance, Innovation Academy for Precision Measurement Science and Technology, Chinese Academy of Sciences, Wuhan 430071, China
    3. University of Chinese Academy of Sciences, Beijing 100049, China

Received date: 2024-03-18

  Online published: 2024-04-16

摘要

溶融动态核极化(dDNP)是一种将分子样品在超低温、强磁场以及微波照射下高度极化,然后经高温高压溶剂快速溶解后立即转移至NMR/MRI系统进行检测的灵敏度增强技术.溶融系统是实现这一过程的关键部分,其性能直接影响样品的溶融、转移效率以及样品极化度的保留程度.本文提出了基于双闭环PID控制算法的自动化溶融系统的控制方案,可在9 min以后达到目标压强1.7 MPa左右并使内部压强被动控制在1.5%以内.将研制的自动化溶融系统集成于自主开发的5 T dDNP仪器系统,可将-271℃的低温样品快速溶融,并于4 s内将其转移到距离11.2 m处的7 T NMR系统进行检测,获得了[1-13C]-丙酮酸钠在溶融态下13C NMR信号9 050倍的增强.自动化溶融系统简化了操作步骤,提高了实验的安全性和一致性.

本文引用格式

曾祥政 , 陈俊飞 , 黄重阳 , 皮海亚 , 曹丽 , 黄臻 , 郭文龙 , 冯继文 , 刘朝阳 . dDNP溶融系统的自动化设计与研究[J]. 波谱学杂志, 2024 , 41(4) : 382 -392 . DOI: 10.11938/cjmr20243101

Abstract

Dissolution dynamic nuclear polarization (dDNP) involves polarizing the sample under microwave irradiation at a low-temperature and strong-magnetic field, dissolving it by solvent of high-temperature and high-pressure, then injecting it rapidly into an NMR/MRI for detection. The dissolution system serves as a pivotal component in the dissolving and injecting process, with its performance directly affecting the melting and transfer efficiency and the high polarization retention. We present an automated dissolution system using a dual-loop proportional-integral-derivative (PID) control algorithm that can reach the target pressure of ~1.7 MPa after 9 min and control the internal pressure within 1.5%. The system can dissolve a solid sample of -271 ℃ in the self-developed 5 T dDNP polarizer and transfer it to the 7 T NMR system at a distance of 11.2 m for detection in 4 s, yielding a 9050-fold enhancement of 13C NMR signal of sodium [1-13C]-pyruvate at the solvated state. In summary, this work developed an automated dissolution system that simplifies the operation steps, ensures detection consistency, and improves experimental safety.

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