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

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

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).

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.
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