顶空固相微萃取/气相色谱法快速萃取-解吸土壤中7种芳香族化合物  

Rapid Extraction-Desorption of 7 Aromatic Compounds in Soil by Headspace Solid Phase Micro-extraction and Gas Chromatography

作　　者：李丙阳 王钊 陈佳[2] 邱洪灯[2] LI Bing-yang;WANG Zhao;CHEN Jia;QIU Hong-deng(College of Chemistry and Chemical Engineering,Xinjiang Normal University,Urumqi 830000,China;Key Laboratory for Natural Medicine of Gansu Province,Lanzhou Institute of Chemical Physics,Chinese Academy of Sciences,Lanzhou 730000,China)

机构地区：[1]新疆师范大学化学化工学院,新疆乌鲁木齐830000 [2]中国科学院兰州化学物理研究所,甘肃省天然药物重点实验室,甘肃兰州730000

出　　处：《分析测试学报》2025年第1期172-179,共8页Journal of Instrumental Analysis

基　　金：国家重点研发计划课题(2019YFC1905501)。

摘　　要：利用氧化石墨烯功能化修饰固相微萃取(GO@SPME)针,结合气相色谱(GC)-氢火焰离子化检测器(FID)建立了检测土壤中7种挥发性芳香烃及其衍生物(包括甲苯、氯苯、乙苯、对二甲苯、邻二甲苯、硝基苯和萘)的快速萃取和解吸策略。考察了萃取液体积、搅拌速率、萃取温度、加盐量、解吸温度、萃取时间和解吸时间对目标物萃取效果的影响,确定在土壤样品中加入内标物质(氘代甲苯),经甲醇提取,顶空固相微萃取快速富集,再结合GC-FID进行检测,基质匹配内标法定量分析。在优化的实验条件下,该方法在15 s内可实现对目标物的快速萃取与解吸(萃取时间12 s,解吸时间3 s)。土壤样品中7种挥发性芳香烃及其衍生物的线性关系良好,相关系数(r^(2))均不小于0.9989,方法检出限(LOD,S/N=3)为1.71~11.60μg/g,定量下限(LOQ,S/N=10)为5.70~38.67μg/g;在3个不同加标水平(60、120、180μg/g)下的平均回收率为87.3%~109%,相对标准偏差(RSD)不大于12%。该方法前处理简单快速,成本较低,数据稳定可靠,适用于土壤样品中芳香族类化合物的快速检测。A rapid extraction and desorption strategy for the detection of seven volatile aromatic hy⁃drocarbons and their derivatives in soil has been developed utilizing a graphene oxide modified solid phase micro-extraction(GO@SPME)needle,in conjunction with gas chromatography(GC)coupled with a hydrogen flame ionization detector(FID).The target compounds include toluene,chloroben⁃zene,ethylbenzene,paraxylene,orthoxylene,nitrobenzene and naphthalene.The influence of seven factors(extraction liquid volume,stirring rate,extraction temperature,salt addition,desorp⁃tion temperature,extraction time and desorption time)on the extraction efficiency was systematically investigated to determine optimal experimental conditions.In the experimental process,we initially introduced deuterated toluene,which serves as an internal standard,to the soil sample to calibrate the systematic errors inherent in the analytical process.In addition,the organic compounds from the soil samples were extracted through methanol soaking,a step designed to separate the target com⁃pounds from the complex soil sample.Under optimal conditions,the target analytes were rapidly en⁃riched using headspace solid phase micro-extraction technology.Finally,the enriched samples were analyzed using GC-FID and internal standard quantification was achieved by constructing a calibra⁃tion curve,ensuring the precision and reliability of the analytical results.The findings indicate that rapid extraction and desorption are feasible within 15 seconds,with extraction taking 12 seconds and desorption requiring just 3 seconds.The linear relation of seven volatile aromatic hydrocarbons and their derivatives was good,with correlation coefficients(r^(2))not less than 0.9989.The limits of de⁃tection(LODs,S/N=3)ranged from 1.71 to 11.60μg/g,while the limits of quantification(LOQs,S/N=10)were from 5.70 to 38.67μg/g.The average recoveries of the seven volatile aromatic hydro⁃carbons and their derivatives at three spiked levels of 60,120 and 180μg/g,ranged from 87.3%to

关 键 词：芳香烃及其衍生物 氧化石墨烯 顶空固相微萃取 气相色谱法 快速萃取-解吸策略 土壤 

分 类 号：O657.7[理学—分析化学] X132[理学—化学]