一种用于混合物分析的一维双选择性全相关谱核磁共振方法

引用本文: 王栋, 夏俊美, 黄帅, 袁铃, 黄桂兰. 一种用于混合物分析的一维双选择性全相关谱核磁共振方法[J]. 分析化学, 2022, 50(8): 1224-1232,1251. doi: 10.19756/j.issn.0253-3820.221026 shu

Citation: WANG Dong, XIA Jun-Mei, HUANG Shuai, YUAN Ling, HUANG Gui-Lan. A Nuclear Magnetic Resonance Method for Mixture Analysis Based on One-Dimensional Doubly Selective Excitation Total Correlation Spectroscopy[J]. Chinese Journal of Analytical Chemistry, 2022, 50(8): 1224-1232,1251. doi: 10.19756/j.issn.0253-3820.221026 shu

一种用于混合物分析的一维双选择性全相关谱核磁共振方法

王栋 ^1, ,
夏俊美 ^1, ,
黄帅 ^2, ,
袁铃 ^{1,
,} ,
黄桂兰 ^{1,
,}

1.
军事科学院防化研究院,国民核生化灾害防护国家重点实验室, 北京 102205;
2.
西南交通大学生命科学与工程学院, 成都 610031

通讯作者: 袁铃,E-mail:hglhdm@163.com; 黄桂兰,E-mail:1789802010@qq.com

基金项目:
四川省应用基础研究项目(No.2020YJ0288)资助。

摘要: 以一维同核全相关谱(1D TOCSY)技术为编辑模块,构建了一维双选择性全相关谱激发(1D TOCSY-TOCSY)核磁共振(NMR)方法。以监控化学品硫二甘醇(Thiodiglycol,TDG)为模型化合物,将1D TOCSY-TOCSY方法应用于复杂混合样品中TDG的筛查与鉴定。在TDG的¹H谱信号被300~2000倍的背景完全掩盖的样品条件下,1D TOCSY-TOCSY谱完全去除了背景信号,只显示TDG信号。在20 min采集时间内累加256次,TDG的检出限为5 μg/mL;12 h采集时间内累加8000次的检出限可达到100 ng/mL。与传统的1D TOCSY、1D NOESY选择性激发以及化学位移选择性滤波(CSSF)技术相比,1D TOCSY-TOCSY方法显示突出的选择性检测能力,检测灵敏度比现有的1D STEP-NOESY技术提高了20倍。本方法为复杂基质样品中痕量监控化学品的筛查鉴定提供了一种新的分析手段,并可应用于其它类型的混合物分析。

关键词:

English

A Nuclear Magnetic Resonance Method for Mixture Analysis Based on One-Dimensional Doubly Selective Excitation Total Correlation Spectroscopy

WANG Dong ^1, ,
XIA Jun-Mei ^1, ,
HUANG Shuai ^2, ,
YUAN Ling ^{1,
,} ,
HUANG Gui-Lan ^{1,
,}

1.
State Key Laboratory of NBC Protection for Civilian, Institute of Chemical Defense, AMS, PLS, Beijing 102205, China;
2.
School of Life Science and Engineering, Southwest Jiaotong University, Chengdu 610031, China

Corresponding author: YUAN Ling, ; HUANG Gui-Lan,

Received Date: 15 January 2022
Revised Date: 27 May 2022
Fund Project:
Supported by the Science and Technology Support Programs of Sichuan Province, China (No.2020YJ0288).

Abstract: One-dimensional doubly selective total correlation spectroscopy (1D TOCSY-TOCSY) nuclear magnetic resonance (NMR) method was constructed using 1D TOCSY as editing module. 1D TOCSY-TOCSY was applied to screen and identify thiodiglycol (TDG) in the complex mixtures, where TDG was a chemical subject to supervision and control and was used as the model compound.In the sample condition that the ¹H signal of TDG was completely covered by 300-2000 times of background, only TDG was visible without any background in 1D TOCSY-TOCSY spectra. The limit of detection for TDG was 5 μg/mL when 256 scans were completed within 20 min. The limit of detection for TDG could reach 100 ng/mL when 8000 scans were acquired in 12 h. Compared with the traditional 1D TOCSY, 1D NOESY selective excitation and chemical shift selective filtering (CSSF) techniques, 1D TOCSY-TOCSY method showed outstanding selective detection capability. It was 20 times more sensitive than the existing 1D STEP-NOESY doubly selective excitation technique. This study provided a new analytical method for screening and identification of the trace chemicals subject to supervision and control in complex matrix samples and could be applied to other mixture analysis.

Key words:

One-dimensional doubly selective excitation total correlation spectroscopy
/ Nuclear magnetic resonance
/ Mixture analysis
/ Thiodiglycol
/ Chemicals subject to supervision and control

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

一种用于混合物分析的一维双选择性全相关谱核磁共振方法

通讯作者: 袁铃,E-mail:hglhdm@163.com; 黄桂兰,E-mail:1789802010@qq.com

English

A Nuclear Magnetic Resonance Method for Mixture Analysis Based on One-Dimensional Doubly Selective Excitation Total Correlation Spectroscopy

Corresponding author: YUAN Ling, ; HUANG Gui-Lan,

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

一种用于混合物分析的一维双选择性全相关谱核磁共振方法

通讯作者: 袁铃,E-mail:hglhdm@163.com; 黄桂兰,E-mail:1789802010@qq.com

English

A Nuclear Magnetic Resonance Method for Mixture Analysis Based on One-Dimensional Doubly Selective Excitation Total Correlation Spectroscopy

Corresponding author: YUAN Ling, ; HUANG Gui-Lan,

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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