引用本文:宋晓娟, 杨维英, 李婷婷.QuEChERS-气相色谱-串联质谱法测定海洋沉积物中的多氯联苯[J].环境监控与预警,2024,(3):16-22
SONG Xiaojuan, YANG Weiying, LI Tingting.Determination of 18 PCBs in Marine Sediment by QuEChERS-Gas Chromatography-Tandem Mass Spectrometry[J].Environmental Monitoring and Forewarning,2024,(3):16-22
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QuEChERS-气相色谱-串联质谱法测定海洋沉积物中的多氯联苯
宋晓娟, 杨维英, 李婷婷*
江苏省连云港环境监测中心,江苏 连云港 222001
摘要:
采用QuEChERS-气相色谱-串联质谱法,建立了海洋沉积物中18种多氯联苯的分析方法。样品加入乙腈及QuEChERS萃取盐振荡提取后,通过PSA和C18净化包进行净化,采用动态多级反应监测模式进行检测。结果表明,18种多氯联苯标准溶液线性关系良好,相关系数为0.999 2~0.999 9。对连云港近岸海域表层沉积物样品进行低、中、高3个不同质量分数的加标实验,回收率为70.6%~96.5%,相对标准偏差为6.5%~14.8%,符合质控要求。方法检出限为0.02~0.08 μg/kg,能够满足痕量分析要求。该方法能够避免使用大量溶剂,操作简便、稳定可靠、灵敏度较高,适用于海洋沉积物中多氯联苯的分析检测。
关键词:  多氯联苯  QuEChERS  气相色谱-串联质谱  海洋沉积物
DOI:DOI:10.3969/j.issn.1674-6732.2024.03.003
分类号:X834;O657
基金项目:江苏省环境监测科研基金项目(2120)
Determination of 18 PCBs in Marine Sediment by QuEChERS-Gas Chromatography-Tandem Mass Spectrometry
SONG Xiaojuan, YANG Weiying, LI Tingting*
Lianyungang Environmental Monitoring Center of Jiangsu Province, Lianyungang, Jiangsu 222001,China
Abstract:
A method for the determination of 18 polychlorinated biphenyls (PCBs) in marine sediment was developed by QuEChERS coupled with gas chromatography tandem mass spectrometry. Sediment samples were extracted with acetonitrile and cleaned up with PSA and C18 adsorbent powder. The analytes were then detected by multiple reaction monitoring (MRM) modes. The results showed that, the linear relationships of the 18 PCBs were good with the correlation coefficients ranged from 0.999 2 to 0.999 9. The average recoveries of the target compounds in marine sediments collected from adjacent sea of Lianyungang spiked at three different concentrations ranged from 70.6% to 96.5%, and the relative standard deviations ranged from 6.5% to 14.8%. The limits of detections for the target compounds were in the range of 0.02~0.08 μg/kg. It proved that, the developed method can avoid the use of large amounts of solvents, and is simple,stable,reliable and sensitive. It has been successfully applied to the analysis of trace PCBs in marine sediments.
Key words:  Polychlorinated biphenyls (PCBs)  QuEChERS  Gas chromatography tandem mass spectrometry  Marine sediment