色谱2025，Vol.43Issue(8)：950-958,9.DOI:10.3724/SP.J.1123.2025.01030
超声辅助气液微萃取-气相色谱-质谱法测定海带中16种多环芳烃
Determination of 16 polycyclic aromatic hydrocarbons in seaweed by ultrasound-assisted gas-liquid microextraction coupled with gas chromatography-mass spectrometry
摘要
Abstract
The increasing demand for the detection of polycyclic aromatic hydrocarbons(PAHs)in the complex matrices of the marine environment requires overcoming the limitations of traditional detection methods,particularly in terms of sensitivity and accuracy.Analyzing PAHs in seaweed matrices is often hindered by significant interference owing to the complex compositions of these matrices,which compromises both qualitative identification and quantitative determination.To address these challenges,this study developed an innovative and efficient method for detecting PAHs based on ultrasound-assisted gas-liquid microextraction(UA-GLME)coupled with gas chromatography-mass spectrometry(GC-MS).The developed method involves extracting a seaweed sample with dichloromethane-hexane(DCM-HEX)(1:1,v/v),followed by further GLME.The separated sample is then analyzed using a DB-5MS capillary column(30 m×0.25 mm×0.25 µm)in SCAN and selective ion monitoring(SIM)modes.PAH extraction efficiencies were enhanced while significantly minimizing the co-extraction of interfering compounds by exploiting the cavitation effects of ul-trasound.This optimization procedure improves both PAH-detection sensitivity and accuracy while reducing matrix effects.Under optimal conditions,the PAHs showed excellent linearity in the range of 5.0-2 000 ng/mL,with correlation coefficients(R2)exceeding 0.999.Limits of detection(LODs)ranged between 0.001 and 0.01 μg/mL,while method detection limits(MDLs)of 0.004-0.04 mg/kg were recorded.The recovery rates at high,medium,and low concentration levels were 62.32％-91.64％,with relative standard deviations(RSDs)between 2.94％and 9.15％.The developed method significantly reduces interference from lipophilic and low-volatility co-extractives,while removing co-extractives,such as long-chain alkanes,fatty acids,and sterols,at rates of up to 100％.Chromatographic comparisons revealed that the UA-GLME method delivers superior peak shapes for the target PAHs,enhanced signal-to-noise ratios,high quantitative accuracies,and remarkable resistance to seaweed-matrix interference.The method was used to detect PAHs in seaweed samples from the East China Sea,Bohai Sea,Yellow Sea,and South China Sea,with the 16 PAHs detected at varying levels.Both low-molecular-weight PAHs(such as naphthalene,phenanthrene,and fluorene)and high-molecular-weight PAHs(such as benzo[a]pyrene and benzo[k]fluoranthene)were detected at high rates.This method offers a reliable approach for the qualitative and quantitative analysis of PAHs in seaweed,thereby providing valuable technical support for assessing marine environmental pollution and evaluating risks.The developed method can be extended to other complex matrices by optimizing the ultrasound conditions and solvent system,thereby offering new strategies for environmental monitoring and pollutant-source tracing.关键词
超声辅助/气液微萃取/气相色谱-质谱法/多环芳烃/海带Key words
ultrasound-assisted(UA)/gas-liquid microextraction(GLME)/gas chromatography-mass spectrometry(GC-MS)/polycyclic aromatic hydrocarbons(PAHs)/seaweed分类
化学化工引用本文复制引用
牟志国,王译旋,郭炎琳,金香子,李东浩,赵锦花..超声辅助气液微萃取-气相色谱-质谱法测定海带中16种多环芳烃[J].色谱,2025,43(8):950-958,9.基金项目
国家自然科学基金项目(22206171,22176164) （22206171,22176164）
吉林省科技发展计划项目(YDZJ202501ZYTS410).National Natural Science Foundation of China(Nos.22206171,22176164) （YDZJ202501ZYTS410）
Jilin Foundation for Program of Science and Technology Research(No.YDZJ202501ZYTS410). （No.YDZJ202501ZYTS410）
