分析测试学报2026，Vol.45Issue(1)：88-96,9.DOI:10.12452/j.fxcsxb.25061601
固相支撑液液萃取/超高效液相色谱-串联质谱法测定尿液中30种内分泌干扰物
Determination of 30 Endocrine Disrupting Chemicals in Urine by Solid Supported Liquid-Liquid Extraction Coupled with Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry
摘要
Abstract
A method was developed for simultaneous determination of 30 endocrine disrupting chemi-cals(EDCs)in urine.The target compounds detected included 9 parabens,9 bisphenols,10 benzo-phenones,and 2 antimicrobials.The method was based on solid supported liquid-liquid extraction(SLE)and ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Urine sample was first treated with enzyme,then purified on a SLE column.The chromatographic separation was performed on an Acquity UPLC BEH C18(2.1 mm×100 mm,1.7 μm)column with 0.05％acetic acid aqueous solution and methanol as the mobile phase.The electrospray ion source(ESI)was operated in positive and negative ion switching scan.The detection was performed in multi-ple reaction monitoring(MRM)mode.Internal standard method was applied for quantitative analysis.The method yielded good linearity in the range level of 0.10-80 μg/L.The spiked recoveries of target compounds ranged from 86.9％to 127％.The relative standard deviations(RSDs)of intra-day and in-ter-day were 1.0％-8.7％and 1.1％-8.2％,respectively.The detection limits(LOD)and quantifica-tion limits(LOQ)of the method were 0.003-0.094 μg/L and 0.009-0.313 μg/L,respectively.The proposed method was applied to detect the target EDCs in 150 urine samples,and a total of 23 EDCs were detected,with a detection rate ranging from 0.7％to 100％.Among them,the detection rate of methylparaben(MeP)was the highest(100％),followed by 4-hydroxybenzophenone(4-OHBP,96.7％)and bisphenol A(BPA,94.7％).The developed method is easy to operate,sensitive,and accurate,and is suitable for high-throughput screening and quantitative analysis of EDCs in human urine.关键词
内分泌干扰物/超高效液相色谱-串联质谱/尿液/固相支撑液液萃取Key words
endocrine disrupting chemicals/ultra-high performance liquid chromatography-tan-dem mass spectrometry(UPLC-MS/MS)/urine/solid supported liquid-liquid extraction(SLE)分类
化学化工引用本文复制引用
张艳,曲良娇,凌莉,梁素丹,吴和岩,黄文燕..固相支撑液液萃取/超高效液相色谱-串联质谱法测定尿液中30种内分泌干扰物[J].分析测试学报,2026,45(1):88-96,9.基金项目
珠海市社会发展领域科技计划项目(2220004000115) （2220004000115）
