分析化学2026，Vol.54Issue(2)：262-271,中插18-中插21,14.DOI:10.19756/j.issn.0253-3820.251327
液液萃取-固相萃取/气相色谱-串联质谱法测定人血清中21种氟代液晶单体
Determination of 21 Kinds of Fluorinated Liquid Crystal Monomers in Human Serum by Combining Liquid-Liquid Extraction and Solid-phase Extraction with Gas Chromatography-Tandem Mass Spectrometry
摘要
Abstract
An analytical method based on liquid-liquid extraction combined with solid-phase extraction(LLE-SPE)and gas chromatography-tandem mass spectrometry(GC-MS/MS)was developed for simultaneous determination of 21 kinds of fluorinated liquid crystal monomers(FLCMs)in human serum.Quantitative internal standards were selected based on retention time and structural similarity.Instrumental conditions,extraction solvents,SPE cartridges,and elution system were systematically optimized.The optimized sample preparation procedure involved processing 250 μL of serum with concentrated sulfuric acid and methanol,followed by two sequential LLE usingn-hexane and methyl tert-butyl ether.The combined extracts were concentrated under a nitrogen stream,purified on a silica gel SPE cartridge,and eluted with dichloromethane.The eluate was concentrated to near dryness with nitrogen,reconstituted in 20 μL of toluene,and analyzed by GC-MS/MS in selected reaction monitoring(SRM)mode with internal standard calibration.Method validation confirmed good linearity for the 21 kinds of FLCMs within the range of 0.5–100 μg/L(r≥0.999).The method achieved limits of detection(LODs)between 0.045 and 0.272 μg/L,with limits of quantification(LOQs)ranging from 0.150 to 0.908 μg/L.The matrix effect was 86.7%–127.8%,with a mean spiked recoveries of 92.7%–134.2%.The intra-day and inter-day precisions(RSD)were 2.45%–8.62%and 2.01%–13.15%,respectively.The method was applied to 122 human serum samples,resulting in the detection of 20 kinds of FLCMs.Five of these target compounds exhibited a detection frequency greater than 50%,with median concentration range of 0.126–5.812 μg/L.This method was suitable for monitoring FLCMs in human serum from the general population,demonstrating controllable matrix effects,high accuracy,stable reproducibility,and adequate sensitivity.关键词
氟代液晶单体/液液萃取/固相萃取/人血清/气相色谱-串联质谱Key words
Fluorinated liquid crystal monomers/Liquid-liquid extraction/Solid-phase extraction/Human serum/Gas chromatography-tandem mass spectrometry引用本文复制引用
白雪,蒋宇晨,鲍珊,骆青青,陆一夫,施小明..液液萃取-固相萃取/气相色谱-串联质谱法测定人血清中21种氟代液晶单体[J].分析化学,2026,54(2):262-271,中插18-中插21,14.基金项目
国家自然科学基金项目(Nos.82388102,82530104)和中国疾病预防控制中心青年科学基金项目(No.2023A201)资助. Supported by the National Natural Science Foundation of China(Nos.82388102,82530104)and the Young Scientific Research Fund of Chinese Center for Disease Control and Prevention(No.2023A201). （Nos.82388102,82530104）
