高等学校化学学报 ›› 2018, Vol. 39 ›› Issue (3): 463-469.doi: 10.7503/cjcu20170323

• 分析化学 • 上一篇    下一篇

耗时短、 通用性强的固体核磁共振交叉极化定量检测方法

顾佳丽1, 张田田1, 赵辉鹏2, 舒婕1(), 李晓虹1   

  1. 1. 苏州大学材料与化学化工学部, 分析测试中心, 苏州 215123
    2. 东华大学分析测试中心, 上海 201620
  • 收稿日期:2017-05-25 出版日期:2018-03-10 发布日期:2018-01-02
  • 作者简介:联系人简介: 舒 婕, 女, 博士, 副教授, 主要从事固体核磁共振方法在材料科学中的应用研究. E-mail:jie_sh@yeah.net
  • 基金资助:
    国家自然科学基金(批准号: 21673148, 21303111, 21305098)资助

Time-saving and Highly Applicable Quantitative Method Based on Solid-state Nuclear Magnetic Resonance Techniques

GU Jiali1, ZHANG Tiantian1, ZHAO Huipeng2, SHU Jie1,*(), LI Xiaohong1,*   

  1. 1. College of Chemistry, Chemical Engineering and Materials Science, Testing and Analysis Center, Soochow University, Suzhou 215123, China
    2.Testing and Analysis Center, Donghua University, Shanghai 201620, China.
  • Received:2017-05-25 Online:2018-03-10 Published:2018-01-02
  • Contact: SHU Jie,LI Xiaohong E-mail:jie_sh@yeah.net
  • Supported by:
    † Supported by the National Natural Science Foundation of China(Nos.21673148, 21303111, 21305098)

摘要:

设计了rCDPz脉冲序列, 结合使用ramp CP技术, 提出了rQCPz/rQCPzRC定量检测方法. 与QCP/QCPRC方法相比, rQCPz/rQCPzRC更适用于高速魔角旋转条件及较长的样品体系. 为了评估rQCPz/rQCPzRC方法的准确性, 选取丙氨酸、 组氨酸及二者的混合物作为检测样品, 分别测定了样品分子基团的相对比例及混合物的组分含量. 通过对DP, CP和rQCPz/rQCPzRC法测定结果进行比较发现, 与CP方法相比, rQCPz/rQCPzRC检测结果的准确度显著提高, 且准确度与传统的DP定量方法相当, 但实验时间大大缩减.

关键词: 固体核磁共振, 定量, 交叉极化, 交叉去极化

Abstract:

For most solid samples, direct polarization(DP) consumes extraordinarily long time. QCP/QCPRC method was capable to provide quantitative information in notably short period of time. However, QCP/QCPRC was not applicable for systems with long or under high MAS frequency condition. To solve aforementioned problems, rCDPz sequence was designed and rQCPz/rQCPzRC method was proposed. L-Alanine, L-histidine and their mixtures were used to evaluate the accuracy of rQCPz/rQCPzRC method. By comparing among three schemes of cross polarization(CP), DP and rQCPz/rQCPzRC, it is demonstrated that rQCPz/rQCPzRC provides accuracy equal to that of DP experiment but consumes markedly shorter experimental time.

Key words: Solid-state NMR, Quantification, Cross polarization, Cross depolarization

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