利用2,2 ' -二硫代二吡啶和高效液相色谱同时分析人血清中总硫醇和低分子量游离硫醇的综合非碱性衍生化策略

IF 5.7 2区化学 Q1 CHEMISTRY, ANALYTICAL

Analytica Chimica Acta Pub Date : 2025-04-15 DOI:10.1016/j.aca.2025.344078

Zhiyu Shao, Jie Zeng, Jun Dong, Fusui Ji, Hongxia Li, Ruiyue Yang, Wenxiang Chen, Wenyu Li, Siming Wang

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引用次数: 0

摘要

背景氧化应激是衰老和健康损害的主要机制，它与血清游离硫醇水平降低有关。监测血清游离硫醇水平为评估机体健康状况提供了有价值的参考。然而，在临床分析中，同时监测血清总游离硫醇和特定的低分子质量游离硫醇化合物是一个关键的挑战。由于游离硫醇在碱性衍生化环境中的高反应活性，传统的方法往往难以避免副反应的干扰。结果利用2,2′-二硫代二吡啶和高效液相色谱建立了一套完整的非碱性衍生化策略。2,2′-二硫代二吡啶在酸性或中性环境下与游离硫醇快速反应，所有衍生物均表现出与底物相似的吸光度特性。利用这些特性，该方法结合了可靠的衍生化和高效的色谱分离，能够在一个注射周期内同时分析总游离硫醇和五种主要的低分子质量硫醇化合物。在14分钟的分析过程中，观察到8个色谱峰，包括游离硫醇衍生物、衍生化试剂和内标。2-硫代吡啶酮对应的峰表示游离硫醇的总浓度，而特定的吡啶二硫酮衍生物峰表示低分子质量的游离硫醇的个别水平。在一项涉及260名志愿者的研究中，使用开发的方法观察到游离硫醇水平与年龄和健康风险因素之间存在显著的负相关。本研究提出了一种同时测定游离硫醇总量和低分子质量游离硫醇的简便方法，为群体分析和研究游离硫醇与人体健康之间的关系提供了一种简便的技术。

本文章由计算机程序翻译，如有差异，请以英文原文为准。

An integrated non-alkaline derivatization strategy using 2,2′-dithiodipyridine and HPLC for simultaneous analysis of total and low-molecular-weight free thiols in human serum

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An integrated non-alkaline derivatization strategy using 2,2′-dithiodipyridine and HPLC for simultaneous analysis of total and low-molecular-weight free thiols in human serum

Background

Oxidative stress is a major mechanism underlying aging and health damage, and it is associated with decreased serum free thiol levels. Monitoring serum free thiol levels provides a valuable reference for assessing the body's health status. However, it is a key challenge in clinical analysis to simultaneously monitor serum total free thiols and specific low-molecular-mass free thiol compounds in a single run. Traditional methods often struggle to avoid interference from side reactions due to the high reactivity of free thiols in alkaline derivatization environments.

Results

In this study, we developed an integrated non-alkaline derivatization strategy using 2,2′-dithiodipyridine and high-performance liquid chromatography. 2,2′-Dithiodipyridine can react rapidly with free thiols under acidic to neutral environments, and all derivatives exhibit similar absorbance characteristics to the substrates. Taking advantage of these properties, this method combines reliable derivatization with efficient chromatographic separation, enabling the simultaneous analysis of total free thiols and five main specific low-molecular-mass thiol compounds within a single injection cycle. Eight chromatographic peaks including free thiol derivatives, the derivatization reagent, and internal standard were observed during a 14-min analysis. The peak corresponding to 2-thiopyridone indicates the total concentration of free thiols while specific pyridyldithio derivative peaks represent the individual levels of low-molecular-mass free thiols. Using the developed method, a significant negative correlation was observed between free thiol levels and both age and health risk factors in a study involving 260 volunteers.

Significance

This study presents a robust and simple method for the simultaneous measurement of total free and low-molecular-mass free thiols, providing a facile technique for population analysis and for investigating the relationship between free thiols and human health.

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来源期刊

Analytica Chimica Acta 化学-分析化学

CiteScore

10.40

自引率

6.50%

发文量

1081

审稿时长

38 days

期刊介绍： Analytica Chimica Acta has an open access mirror journal Analytica Chimica Acta: X, sharing the same aims and scope, editorial team, submission system and rigorous peer review. Analytica Chimica Acta provides a forum for the rapid publication of original research, and critical, comprehensive reviews dealing with all aspects of fundamental and applied modern analytical chemistry. The journal welcomes the submission of research papers which report studies concerning the development of new and significant analytical methodologies. In determining the suitability of submitted articles for publication, particular scrutiny will be placed on the degree of novelty and impact of the research and the extent to which it adds to the existing body of knowledge in analytical chemistry.