同时测定尿中反-反式黏糠酸和苯巯基尿酸的在线固相萃取-液相色谱-质谱测定法

职业与健康 ›› 2024, Vol. 40 ›› Issue (13): 1774-1777.

同时测定尿中反-反式黏糠酸和苯巯基尿酸的在线固相萃取-液相色谱-质谱测定法

何宗剑¹, 莫玉茗², 宁攀良¹, 朱定姬¹, 覃利梅¹, 李燕¹

1.广西壮族自治区职业病防治研究院理化检测所,广西南宁 530021;
2.广西医科大学公共卫生学院,广西南宁 530021

收稿日期:2023-10-09 修回日期:2023-10-31 发布日期:2026-03-17
通信作者: 李燕,高级工程师,E-mail：1139659701@qq.com
作者简介:何宗剑,男,工程师,主要从事理化检测工作。
基金资助:
广西壮族自治区卫生健康委员会课题（Z-A20230412）

Simultaneous determination of trans-trans mucofuric acid and phenylthiouric acid in urine by online solid-phase extraction liquid chromatography mass spectrometry

HE Zongjian¹, MO Yuming², NING Panliang¹, ZHU Dingji¹, QIN Limei¹, LI Yan¹

1. Department of Physical and Chemical Testing, Guangxi Zhuang Autonomous Region Academy for Prevention and Treatment of Occupational Diseases, Nanning Guangxi, 530021, China;
2. School of Public Health, Guangxi Medical University, Nanning Guangxi, 530021, China

Received:2023-10-09 Revised:2023-10-31 Published:2026-03-17
Contact: LI Yan,Senior engineer,E-mail：1139659701@qq.com

摘要/Abstract

摘要： 目的建立同时测定尿中反-反式黏糠酸和苯巯基尿酸的在线固相萃取-液相色谱-质谱测定方法。方法尿样离心后上机,经在线固相萃取HLB柱（20 mm×3.9 mm×15 μm）净化、富集,经C18柱（150 mm×4.6 mm×5 μm）分析,线性离子阱质谱检测。结果反-反式黏糠酸和苯巯基尿酸的线性范围为0.0~15.0 mg/L、0.0~500.0 μg/L,相关系数为0.999 8、0.999 9,检出限为3.5、0.1 μg/L,样品加标回收率为103.3%~108.8%,相对标准偏差为2.8%~8.4%。结论该方法样品前处理只需离心,操作简便快捷、结果准确、重现性好、灵敏高,适用于大批量的苯职业接触人群生物监测指标的检测。

关键词: 在线固相萃取, 液相色谱-质谱法, 尿, 反反-粘糠酸, 苯巯基尿酸, 苯代谢物

Abstract: Objective To establish an online solid-phase extraction liquid chromatography-mass spectrometry method for the simultaneous determination of trans-trans mucofuric acid and phenylmercaptouric acid in urine. Methods The urine samples were centrifuged and processed on the machine,purified and enriched by online solid-phase extraction on HLB column（20 mm×3.9 mm×15 μm）,and analysed by C18 column（150 mm×4.6 mm×5 μm）,detected by linear ion trap mass spectrometry. Results The linear range of trans-trans mucofuric acid and phenylmercaptouric acid were 0.0-15.0 mg/L and 0.0-500.0 μg/L,with correlation coefficients of 0.999 8 and 0.999 9,and detection limits of 3.5 and 0.1 μg/L,the recovery rates were 103.3%-108.8%,and the relative standard deviations were 2.8%-8.4%. Conclusion The sample pre-treatment of this method only requires centrifuged,which is simple and fast,with accurate results,good reproducibility and high sensitivity,and it was suitable for the detection of biological monitoring indicators in large quantities of occupational benzene exposure population.

Key words: Online solid-phase extraction, Liquid chromatography-mass spectrometry, Urine, Trans-trans mucofuric acid, Phenylmercaptouric acid, Benzene metabolites

中图分类号:

R115

何宗剑, 莫玉茗, 宁攀良, 朱定姬, 覃利梅, 李燕. 同时测定尿中反-反式黏糠酸和苯巯基尿酸的在线固相萃取-液相色谱-质谱测定法. [J]职业与健康, 2024, 40(13): 1774-1777.

HE Zongjian, MO Yuming, NING Panliang, ZHU Dingji, QIN Limei, LI Yan. Simultaneous determination of trans-trans mucofuric acid and phenylthiouric acid in urine by online solid-phase extraction liquid chromatography mass spectrometry. [J]OCCUPATION AND HEALTH, 2024, 40(13): 1774-1777.

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