Directed synthesis of N1/N3-histidine modified by 2-hydroxyethylthioethyl and identification in sulfur mustard-exposed plasma

Abstract Sulfur mustard (HD) alkylates biomolecules such as proteins, generating specific biomarkers. This study employs steric hindrance, electronic effects, and solvent effects through an occupancy-removal strategy to synthesize regioisomers [N1-HETE]-His and [N3-HETE]-His, overcoming isomer separ...

Full description

Saved in:
Bibliographic Details
Main Authors: Long Wen, Zhibin Shu, Li Pan, Bo Chen, Gang Qu, Shu Geng, Yuntao Yang, Yan Jiang, Shilei Liu
Format: Article
Language:English
Published: Nature Portfolio 2025-03-01
Series:Communications Chemistry
Online Access:https://doi.org/10.1038/s42004-025-01479-1
Tags: Add Tag
No Tags, Be the first to tag this record!
_version_ 1849761664793051136
author Long Wen
Zhibin Shu
Li Pan
Bo Chen
Gang Qu
Shu Geng
Yuntao Yang
Yan Jiang
Shilei Liu
author_facet Long Wen
Zhibin Shu
Li Pan
Bo Chen
Gang Qu
Shu Geng
Yuntao Yang
Yan Jiang
Shilei Liu
author_sort Long Wen
collection DOAJ
description Abstract Sulfur mustard (HD) alkylates biomolecules such as proteins, generating specific biomarkers. This study employs steric hindrance, electronic effects, and solvent effects through an occupancy-removal strategy to synthesize regioisomers [N1-HETE]-His and [N3-HETE]-His, overcoming isomer separation challenges in conventional methods. Density functional theory (DFT) calculations revealed hexafluoroisopropanol (HFIP)’s critical role in directing HD’s regioselective alkylation: HFIP modulates steric and electronic environments to preferentially target N1 or N3 sites of histidine imidazole rings, with predictions validated experimentally. The method further enables selective detection of the isomers in HD-contaminated plasma via standard addition, advancing absolute quantification. This work not only establishes a precision synthesis platform for biomarkers but also elucidates HFIP’s unique role in imidazole regioselectivity, offering insights for medicinal chemistry and HD toxicology. These findings hold implications for HD exposure tracking, mechanism analysis, clinical diagnostics, and antidote development.
format Article
id doaj-art-14302e77dcc24423849a3ffd59460fb4
institution DOAJ
issn 2399-3669
language English
publishDate 2025-03-01
publisher Nature Portfolio
record_format Article
series Communications Chemistry
spelling doaj-art-14302e77dcc24423849a3ffd59460fb42025-08-20T03:05:56ZengNature PortfolioCommunications Chemistry2399-36692025-03-01811910.1038/s42004-025-01479-1Directed synthesis of N1/N3-histidine modified by 2-hydroxyethylthioethyl and identification in sulfur mustard-exposed plasmaLong Wen0Zhibin Shu1Li Pan2Bo Chen3Gang Qu4Shu Geng5Yuntao Yang6Yan Jiang7Shilei Liu8State Key Laboratory of NBC Protection for CivilianState Key Laboratory of NBC Protection for CivilianState Key Laboratory of NBC Protection for CivilianState Key Laboratory of NBC Protection for CivilianState Key Laboratory of NBC Protection for CivilianState Key Laboratory of NBC Protection for CivilianState Key Laboratory of NBC Protection for CivilianCollege of Chemistry and Environmental Engineering, Sichuan University of Science and EngineeringState Key Laboratory of NBC Protection for CivilianAbstract Sulfur mustard (HD) alkylates biomolecules such as proteins, generating specific biomarkers. This study employs steric hindrance, electronic effects, and solvent effects through an occupancy-removal strategy to synthesize regioisomers [N1-HETE]-His and [N3-HETE]-His, overcoming isomer separation challenges in conventional methods. Density functional theory (DFT) calculations revealed hexafluoroisopropanol (HFIP)’s critical role in directing HD’s regioselective alkylation: HFIP modulates steric and electronic environments to preferentially target N1 or N3 sites of histidine imidazole rings, with predictions validated experimentally. The method further enables selective detection of the isomers in HD-contaminated plasma via standard addition, advancing absolute quantification. This work not only establishes a precision synthesis platform for biomarkers but also elucidates HFIP’s unique role in imidazole regioselectivity, offering insights for medicinal chemistry and HD toxicology. These findings hold implications for HD exposure tracking, mechanism analysis, clinical diagnostics, and antidote development.https://doi.org/10.1038/s42004-025-01479-1
spellingShingle Long Wen
Zhibin Shu
Li Pan
Bo Chen
Gang Qu
Shu Geng
Yuntao Yang
Yan Jiang
Shilei Liu
Directed synthesis of N1/N3-histidine modified by 2-hydroxyethylthioethyl and identification in sulfur mustard-exposed plasma
Communications Chemistry
title Directed synthesis of N1/N3-histidine modified by 2-hydroxyethylthioethyl and identification in sulfur mustard-exposed plasma
title_full Directed synthesis of N1/N3-histidine modified by 2-hydroxyethylthioethyl and identification in sulfur mustard-exposed plasma
title_fullStr Directed synthesis of N1/N3-histidine modified by 2-hydroxyethylthioethyl and identification in sulfur mustard-exposed plasma
title_full_unstemmed Directed synthesis of N1/N3-histidine modified by 2-hydroxyethylthioethyl and identification in sulfur mustard-exposed plasma
title_short Directed synthesis of N1/N3-histidine modified by 2-hydroxyethylthioethyl and identification in sulfur mustard-exposed plasma
title_sort directed synthesis of n1 n3 histidine modified by 2 hydroxyethylthioethyl and identification in sulfur mustard exposed plasma
url https://doi.org/10.1038/s42004-025-01479-1
work_keys_str_mv AT longwen directedsynthesisofn1n3histidinemodifiedby2hydroxyethylthioethylandidentificationinsulfurmustardexposedplasma
AT zhibinshu directedsynthesisofn1n3histidinemodifiedby2hydroxyethylthioethylandidentificationinsulfurmustardexposedplasma
AT lipan directedsynthesisofn1n3histidinemodifiedby2hydroxyethylthioethylandidentificationinsulfurmustardexposedplasma
AT bochen directedsynthesisofn1n3histidinemodifiedby2hydroxyethylthioethylandidentificationinsulfurmustardexposedplasma
AT gangqu directedsynthesisofn1n3histidinemodifiedby2hydroxyethylthioethylandidentificationinsulfurmustardexposedplasma
AT shugeng directedsynthesisofn1n3histidinemodifiedby2hydroxyethylthioethylandidentificationinsulfurmustardexposedplasma
AT yuntaoyang directedsynthesisofn1n3histidinemodifiedby2hydroxyethylthioethylandidentificationinsulfurmustardexposedplasma
AT yanjiang directedsynthesisofn1n3histidinemodifiedby2hydroxyethylthioethylandidentificationinsulfurmustardexposedplasma
AT shileiliu directedsynthesisofn1n3histidinemodifiedby2hydroxyethylthioethylandidentificationinsulfurmustardexposedplasma