真空辅助顶空固相微萃取/气相色谱-质谱法测定地下水中9种多氯联苯OA
Determination of 9 Polychlorinated Biphenyls in Groundwater by Vacuum-assisted Headspace Solid-phase Microextraction/Gas Chromatography-Mass Spectrometry
针对水质监测中部分多氯联苯(PCBs)项目的缺失,采用真空辅助顶空固相微萃取(Vac-HS-SPME)富集、气相色谱-质谱(GC-MS)检测,建立了地下水中9种多氯联苯(PCBs)环保、高效且灵敏的分析新方法.通过优化萃取纤维、萃取温度、萃取时间和搅拌速度等实验条件,确定了最佳萃取条件:选用65 µm PDMS/DVB萃取纤维,于70℃以500 r/min的搅拌速度提取40 min.在0.02~2.0 µg/L质量浓度范围内,9种PCBs表现出良好的线性关系,线性相关系数(r)为0.998 1~0.999 4,方法检出限为0.002~0.016 µg/L.9种PCBs的加标回收率为78.9%~115%,相对标准偏差(n=6)为2.8%~12%.与传统顶空固相微萃取(HS-SPME)相比,Vac-HS-SPME展现出更高的方法灵敏度和提取效率.该方法操作简便、环境友好、灵敏度高,已成功应用于实际地下水样品的测定,为环境水样中PCBs的定性和定量分析提供了新的技术手段.
To compensate the absence of some polychlorinated biphenyls(PCBs)items in water qual-ity monitoring,a new environmentally friendly,efficient and sensitive analytical method for 9 PCBs in groundwater was established by using vacuum-assisted headspace solid-phase microextraction tech-nology(Vac-HS-SPME)for enrichment and gas chromatography-mass spectrometry(GC-MS)for de-tection.Experimental conditions including extraction fiber type,extraction temperature,extraction time,and stirring speed were optimized as 65 µm PDMS/DVB extraction fiber at 70℃with a stirring speed of 500 r/min for a duration of 40 min.9 target PCBs exhibited excellent linearities within the range of 0.02-2.0 µg/L with correlation coefficients(r)between 0.998 1-0.999 4.Method detec-tion limits varied from 0.002 to 0.016 µg/L.The spiked recoveries of the 9 PCBs ranged from 78.9%to 115%,with relative standard deviations(n=6)between 2.8%-12%.In comparison to traditional headspace solid-phase microextraction(HS-SPME)techniques,Vac-HS-SPME offers enhanced sensitivity and extraction efficiency-particularly for PCBs with higher chlorination levels.This meth-od is simple to operate,environmentally friendly and highly sensitive and has been successfully ap-plied to the determination of actual groundwater samples,providing a new technical means for the qualitative and quantitative analysis of PCBs in environmental water samples.
周旭平;何媛媛;刘君;殷伟庆
江苏省镇江环境监测中心,江苏 镇江 212000江苏省镇江环境监测中心,江苏 镇江 212000江苏省镇江环境监测中心,江苏 镇江 212000江苏省镇江环境监测中心,江苏 镇江 212000
化学化工
真空辅助顶空固相微萃取气相色谱-质谱地下水多氯联苯
vacuum-assisted headspace solid-phase microextractiongas chromatography-mass spectrometrygroundwaterpolychlorinated biphenyls
《分析测试学报》 2026 (3)
524-530,7
江苏省镇江环境监测中心监测科研基金(E1)镇江市社发重点项目(SH2024107)
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