定量核磁共振氢谱测定氘代碘甲烷的氘代率

doi:10.3976/j.issn.1002-4026.2021.05.017

山东科学 ›› 2021, Vol. 34 ›› Issue (5): 136-142.doi: 10.3976/j.issn.1002-4026.2021.05.017

• 其他研究论文 • 上一篇

定量核磁共振氢谱测定氘代碘甲烷的氘代率

王瑜亮¹，万新焕²，张云云¹，肖童³，李福伟¹，高红梅¹，刘桂娟¹，林云良^1*

1.齐鲁工业大学（山东省科学院）山东省分析测试中心，山东济南 250014；2.山东中医药大学药学院，山东济南 250355；3.济南美高生物医药科技有限公司，山东济南 250119

收稿日期:2020-12-16 出版日期:2021-10-14 发布日期:2021-10-19
通信作者: 林云良，男，高级实验师，研究方向为药物分析。Tel: 13370523069，E-mail:wodekafei@126．com
作者简介:王瑜亮（1988—），男，硕士研究生，助理实验师，研究方向为药物分析。E-mail:wangyuliang123@163.com
基金资助:
山东省重大科技创新工程项目（2017CXGC1209；2017CXGC1308）

Determination of deuteration rate of iodomethane-d₃ using quantitative proton nuclear magnetic resonance

WANG Yu-liang¹，WAN Xin-huan²，ZHANG Yun-yun¹，XIAO Tong³，LI Fu-wei¹，GAO Hong-Mei¹，LIU Gui-juan¹，LIN Yun-liang^1*

1. Shandong Analysis and Test Center， Qilu University of Technology (Shandong Academy of Sciences)，Jinan 250014，China；2. College of Pharmacy，Shandong University of Traditional Chinese Medicine，Jinan 250355，China；3.Jinan Meigao Biopharmatech Co.， Ltd.， Jinan 250119， China

Received:2020-12-16 Online:2021-10-14 Published:2021-10-19

摘要/Abstract

摘要： 建立了测定氘代碘甲烷氘代率的定量核磁共振氢谱方法。实验以氘代二甲基亚砜（DMSO-d₆）为氘代溶剂、对苯二甲酸二甲酯为内标物，在400 MHz光谱仪上进行测定。选择谱宽4807.69 Hz，激发偏置为2000.65 Hz，弛豫延迟时间为65 s，扫描次数为16次，以二氘碘甲烷氢（δ2.16）为定量峰，对苯二甲酸二甲酯的苯环氢（δ8.07）为内标峰。对线性关系、精密度、重复性、稳定性及耐用性等进行了方法学评价，结果良好。表明定量氢核磁共振法可用于氘代碘甲烷的氘代率测定，该方法准确可靠，简便快捷，且无需自身对照品，能够满足实验室中氘代碘甲烷氘代率的检测。

关键词: 氘代碘甲烷, 氘代率, 定量核磁共振氢谱

Abstract: In this study, a quantitative proton nuclear magnetic resonance (qHNMR) method was proposed to determine the deuteration rate of iodomethane-d3.An experiment was conducted on a 400 MHz spectrometer using dimethyl terephthalate (DMT) and dimethyl sulfoxide (DMSO-d₆) as the internal standard reference and deuterated solvent, respectively. The following parameters were set: spectral width 4807.69 Hz, transmitter frequency offset 2000.65 Hz, relaxation delay time 65 s, and number of scans 16 times. The peak of δ2.16 in iodomethane-d2 and that of δ8.07 in dimethyl terephthalate were considered as the quantitative and internal standard peaks, respectively. The methodological assessment of linearity, precision, repeatability, stability, and durability was performed, and good results were achieved. The proposed qHNMR method can be used for determining the deuteration rate of iodomethane-d3. This method is accurate, reliable, simple, and fast and does not require its own reference substance. Thus, it can meet the test requirements of iodomethane-d3 deuteration rate in the laboratory.

Key words: iodomethane-d₃, deuteration rate, quantitative proton nuclear magnetic resonance

中图分类号:

O657.61

王瑜亮, 万新焕, 张云云, 肖童, 李福伟, 高红梅, 刘桂娟, 林云良. 定量核磁共振氢谱测定氘代碘甲烷的氘代率[J]. 山东科学, 2021, 34(5): 136-142.

WANG Yu-liang, WAN Xin-huan, ZHANG Yun-yun, XIAO Tong, LI Fu-wei, GAO Hong-Mei, LIU Gui-juan, LIN Yun-liang. Determination of deuteration rate of iodomethane-d₃ using quantitative proton nuclear magnetic resonance[J]. Shandong Science, 2021, 34(5): 136-142.

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定量核磁共振氢谱测定氘代碘甲烷的氘代率

Determination of deuteration rate of iodomethane-d₃ using quantitative proton nuclear magnetic resonance

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定量核磁共振氢谱测定氘代碘甲烷的氘代率

Determination of deuteration rate of iodomethane-d3 using quantitative proton nuclear magnetic resonance

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Determination of deuteration rate of iodomethane-d₃ using quantitative proton nuclear magnetic resonance