2023年第4期36No.4Jul.2023分析仪器AnalyticalInstrumentation气相色谱-质谱法同时快速测定地表水中33种半挥发性有机物鲁瑞梅李国文*(云南省生态环境厅驻玉溪市生态环境监测站，玉溪653100)摘要：建立了液液萃取结合气相色谱-质谱法同时测定地表水中33种半挥发性有机物（SVOCs）的分析方法。样品以二氯甲烷为萃取剂在先酸性后中性条件下液液萃取2次，合并萃取液经无水硫酸钠脱水、浓缩并定容至1mL，采用气相色谱-质谱联用仪在电子电离源（EI）模式和选择离子监测（SIM）模式检测，内标法定量。对影响目标物萃取效率的关键因素，水样pH值、萃取剂种类与用量及萃取时间进行了优化与考察。在最优萃取条件下，33种SVOCs在5~500μg∙L-1范围内线性良好，平均相对响应因子的相对标准偏差（RRFRSD）小于15.5%，方法检出限为0.01~0.09μg∙L-1，定量限为0.04~0.36μg∙L-1，在2个空白添加高低质量浓度（0.05和0.25μg∙L-1）水平下的平均回收率为67.1%~119.2%，相对标准偏差（n=6）为1.0%~9.3%。该方法具有较高的选择性、灵敏度和准确度，适合地表水中33种SVOCs快速分析检测。关键词：半挥发性有机物同时测定气相色谱-质谱法地表水内标法DOI:10.3969/j.issn.1001‐232x.2023.04.008Simultaneousrapiddeterminationof33semi-volatileorganiccompoundsinsurfacewaterbygaschromatography-massspectrometry.LuRuimei,LiGuowen*（EcologicalandEnvironmentalMonitoringStationofDEEYinYuxi,Yuxi653100,Yunan,China）Abstract:Thesamplewasextractedtwicewithdichloromethaneastheextractantunderacidicandthenneutralconditions,thecombinedextractwasdehydratedandconcentratedwithanhydroussodiumsulfateandthevolumewasfixedto1mL.Thesamplesweredetectedbygaschromatography-massspectrometryinelectronionizationsource(EI)modeandselectiveionmonitoring(SIM)mode,andquantifiedbyinternalstandardmethod.Thekeyfactorsaffectingtheextractionefficiencyofthetargetsubstance,suchasthepHvalueofthewatersample,thetypeandamountofextractant,andtheextractiontime,wereoptimizedandinvestigated.Undertheoptimalextractionconditions,thelinearityofthe33SVOCswasgoodintherangeof5to500μg·L-1withtheaveragerelativestandarddeviationlessthan15.5%,thelimitsofdetectionofthemethodwere0.01to0.09μg·L-1andthelimitsofquantificationwere0.04to0.3...
