Detection of three metabolites of xylene in urine samples by solid-phase extraction coupled with liquid chromatography-mass spectrometry
10.3760/cma.j.cn121094-20220902-00440
- VernacularTitle:尿中二甲苯3种代谢产物测定的固相萃取-液质联用法
- Author:
Shengdong PAN
1
;
Xiaohai LI
;
Li WANG
;
Qiaoli QIU
Author Information
1. 宁波市疾病预防控制中心理化检验所，浙江省微量有毒化学物健康风险评估技术研究重点实验室，宁波 315010
- Keywords:
Urine;
Metabolites of xylene;
Ultra-performance liquid chromatography-high resolution mass spectrometry, UPLC-HRMS;
MAX solid-phase extraction
- From:
Chinese Journal of Industrial Hygiene and Occupational Diseases
2023;41(10):854-858
- CountryChina
- Language:Chinese
-
Abstract:
Objective:To establish a method for the rapid determination of the three metabolites of xylene, 2-methylmarmaluronic acid, 3-methylmarmaluronic acid and 4-methylmarmaluronic acid, in urine of occupationally exposed workers by ultra-performance liquid chromatography-high resolution mass spectrometry (UPLC-HRMS) .Methods:In July 2022, urine samples were diluted and extracted with pH=6.86 phosphate cache solution, cleaned up by a MAX solid-phase extraction (SPE) column and separated by an Accucore Ph/Hexyl column (100 mm×2.1 mm, 2.6 μm) with a gradient of 5 mmol/L ammonium formate-0.1% formic acid aqueous solution and methanol as mobile phases. The analysis was carried out in electrospray ionization mode and full mass-data dependent secondary mass spectrometry mode, and quantified by external standard method. The characteristics of each index of this method were analyzed.Results:A good linearity was obtained in the concentration range of 1.0-200.0 μg/L for 2-methylmuramic acid, 3-methylmuramic acid and 4-methylmuramic acid with the correlation coefficients of 0.9979-0.9993. The limits of detection of the method were 0.18-0.24 μg/L. While the spiked recoveries at the three concentrations (1.0 μg/L, 100.0 μg/L, and 180.0 μg/L) were in the range of 83.0%-93.7%, with the relative standard deviations of 2.2%-7.9%.Conclusion:The UPLC-HRMS method is simple, rapid, sensitive and accurate, and is suitable for the simultaneous determination of the three metabolites of xylene in the urine of occupationally exposed workers.
