Quantitative analysis of ethylene glycol in human serum by liquid chromatography-tandem mass spectrometry with p-toluenesulfonyl isocyanate derivatization.

IF 2.8 4区医学 Q2 TOXICOLOGY

Forensic Toxicology Pub Date : 2025-06-24 DOI:10.1007/s11419-025-00729-0

Shin Ogawa, Ryosuke Shiraki, Kengo Wakigawa, Hidehiko Okazaki, Akira Tsujita, Akinaga Gohda, Toshiro Matsui

{"title":"Quantitative analysis of ethylene glycol in human serum by liquid chromatography-tandem mass spectrometry with p-toluenesulfonyl isocyanate derivatization.","authors":"Shin Ogawa, Ryosuke Shiraki, Kengo Wakigawa, Hidehiko Okazaki, Akira Tsujita, Akinaga Gohda, Toshiro Matsui","doi":"10.1007/s11419-025-00729-0","DOIUrl":null,"url":null,"abstract":"Purpose: Ethylene glycol (EG) is a typical antifreeze compound and a significant analyte in forensic toxicology. Current EG analytical method for biological samples in forensic toxicology employ liquid chromatography-tandem mass spectrometry (LC-MS/MS), however, they exhibit low sensitivity and reliability. Therefore, in this study, we aimed to establish a highly sensitive, selective, and reliable EG assay system for human serum analysis using a hydroxyl derivatization-aided LC-MS/MS technique.Methods: p-Toluenesulfonyl isocyanate (PTSI) was applied for precolumn derivatization of EG in human serum, to enhance the sensitivity of LC-MS/MS for EG detection.Results: The optimal derivatization conditions were 200 µL/mL PTSI in acetonitrile at 25 °C for 10 min. A highly sensitive and reliable LC-MS/MS detection of EG in human serum was achieved, with the calibration curve exhibiting a good linearity (r > 0.999, 10-1000 µg/mL of EG). The proposed PTSI-derivatization-LC-MS/MS method exhibited high reliability (1.4-1.8%) for the intra-day and inter-day repeatability (%RSD), and accuracy (96.7-102.4%), with the limits of detection and quantification in human serum being 0.023 µg/mL (S/N = 3) and 0.077 µg/mL (S/N = 10), respectively.Conclusions: A novel PTSI derivatization-aided LC-MS/MS method was developed, offering a highly sensitive, selective, and reliable analytical tool for EG quantification in human serum for forensic toxicology applications.","PeriodicalId":12329,"journal":{"name":"Forensic Toxicology","volume":" ","pages":""},"PeriodicalIF":2.8000,"publicationDate":"2025-06-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Forensic Toxicology","FirstCategoryId":"3","ListUrlMain":"https://doi.org/10.1007/s11419-025-00729-0","RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q2","JCRName":"TOXICOLOGY","Score":null,"Total":0}

引用次数: 0

Abstract

Purpose: Ethylene glycol (EG) is a typical antifreeze compound and a significant analyte in forensic toxicology. Current EG analytical method for biological samples in forensic toxicology employ liquid chromatography-tandem mass spectrometry (LC-MS/MS), however, they exhibit low sensitivity and reliability. Therefore, in this study, we aimed to establish a highly sensitive, selective, and reliable EG assay system for human serum analysis using a hydroxyl derivatization-aided LC-MS/MS technique.

Methods: p-Toluenesulfonyl isocyanate (PTSI) was applied for precolumn derivatization of EG in human serum, to enhance the sensitivity of LC-MS/MS for EG detection.

Results: The optimal derivatization conditions were 200 µL/mL PTSI in acetonitrile at 25 °C for 10 min. A highly sensitive and reliable LC-MS/MS detection of EG in human serum was achieved, with the calibration curve exhibiting a good linearity (r > 0.999, 10-1000 µg/mL of EG). The proposed PTSI-derivatization-LC-MS/MS method exhibited high reliability (1.4-1.8%) for the intra-day and inter-day repeatability (%RSD), and accuracy (96.7-102.4%), with the limits of detection and quantification in human serum being 0.023 µg/mL (S/N = 3) and 0.077 µg/mL (S/N = 10), respectively.

Conclusions: A novel PTSI derivatization-aided LC-MS/MS method was developed, offering a highly sensitive, selective, and reliable analytical tool for EG quantification in human serum for forensic toxicology applications.

查看原文本刊更多论文

对甲苯磺酰异氰酸酯衍生化液相色谱-串联质谱法定量分析人血清中乙二醇。

目的：乙二醇是一种典型的防冻化合物，是法医毒理学研究中的重要分析物。目前法医毒理学中生物样品的EG分析方法采用液相色谱-串联质谱法（LC-MS/MS），但灵敏度和可靠性较低。因此，在本研究中，我们旨在利用羟基衍生辅助LC-MS/MS技术建立一个高灵敏度、高选择性和高可靠性的EG分析系统，用于人血清分析。方法：采用对甲苯磺酰异氰酸酯（PTSI）进行柱前衍生化，提高LC-MS/MS检测EG的灵敏度。结果：最佳衍生化条件为200µL/mL PTSI在乙腈中，在25°C条件下，反应10 min，实现了对人血清中EG的高灵敏度、高可靠性的LC-MS/MS检测，校准曲线线性良好（r = 0.999, 10-1000µg/mL EG）。所建立的ptsi衍生化- lc -MS/MS方法具有较高的可靠性（1.4 ~ 1.8%），日内重复性（%RSD）和准确度（96.7 ~ 102.4%），在人血清中的检测限和定量限分别为0.023µg/mL （S/N = 3）和0.077µg/mL （S/N = 10）。结论：建立了一种新的PTSI衍生辅助LC-MS/MS方法，为法医毒理学应用提供了一种高灵敏度、高选择性和高可靠性的人血清EG定量分析工具。

本文章由计算机程序翻译，如有差异，请以英文原文为准。

求助全文

约1分钟内获得全文求助全文

来源期刊

Forensic Toxicology TOXICOLOGY-

CiteScore

5.80

自引率

9.10%

发文量

审稿时长

3 months

期刊介绍： The journal Forensic Toxicology provides an international forum for publication of studies on toxic substances, drugs of abuse, doping agents, chemical warfare agents, and their metabolisms and analyses, which are related to laws and ethics. It includes original articles, reviews, mini-reviews, short communications, and case reports. Although a major focus of the journal is on the development or improvement of analytical methods for the above-mentioned chemicals in human matrices, appropriate studies with animal experiments are also published. Forensic Toxicology is the official publication of the Japanese Association of Forensic Toxicology (JAFT) and is the continuation of the Japanese Journal of Forensic Toxicology (ISSN 0915-9606).