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搅拌子吸附-热脱附-气相色谱-质谱法分析北京大气中33种多氯联苯
Determination of 33 Polychlorinated Biphenyls in the Atmosphere of Beijing Using Stir Bar Sorptive Extraction-Thermal Desorption Coupled with Gas Chromatography-Mass Spectrometry
投稿时间:2022-10-23  修订日期:2023-12-22
DOI:10.19316/j.issn.1002-6002.2024.02.18
中文关键词:  搅拌子吸附  热脱附  多氯联苯  被动大气采样
英文关键词:stir bar sorptive extraction  thermal desorption  polychlorinated biphenyls  passive air sampling
基金项目:国家自然科学基金资助项目(21307148);中国科学院技术支撑人才项目(2021)
作者单位
李红华 中国科学院生态环境研究中心, 环境化学与生态毒理学国家重点实验室, 北京 100085 
李英明 中国科学院生态环境研究中心, 环境化学与生态毒理学国家重点实验室, 北京 100085 
李晓敏 中国农业科学院农业质量标准与检测技术研究所, 北京 100081 
孙慧中 国家地质实验测试中心, 北京 100037 
夏莎莎 中国科学院生态环境研究中心, 环境化学与生态毒理学国家重点实验室, 北京 100085 
张庆华* 中国科学院生态环境研究中心, 环境化学与生态毒理学国家重点实验室, 北京 100085 
通讯作者:张庆华*  中国科学院生态环境研究中心, 环境化学与生态毒理学国家重点实验室, 北京 100085  
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中文摘要:
      用包覆聚二甲基硅氧烷(PDMS)吸附层的搅拌子作被动大气采样器,建立了搅拌子吸附-热脱附-气相色谱-质谱法(SBSE-TD-GC-MS)分析大气中多氯联苯(PCBs)的方法。优化后的热脱附温度为280℃,热脱附时间为6 min,聚焦冷阱的温度为-40℃,33种PCB单体的热脱附残留比例低于7%。验证了方法的线性、精密度和重复性。标准曲线5个点线性关系良好,33种PCB单体的相关系数r>0.998。方法精密度验证的相对标准偏差(RSD)为0.79%~20.2%(n=8),日内重复性实验的RSD为0.43%~29.8%(n=10),日间重复性实验的RSD为3.20%~29.6%(n=20),方法检出限(LOD)为0.01~2.51 pg,回收率为98%±18%。将建立的方法用于北京大气中PCBs的分析。检出8种PCB单体,质量为2.94~129 pg。在32 d的采样周期内PCB-52、PCB-123、PCB-155一直处于线性吸附阶段,而PCB-1和PCB-3经过了线性吸附阶段、曲线吸附阶段和平衡阶段。研究结果表明,SBSE-TD-GC-MS可以用于大气中PCBs的样品采集和快速分析。
英文摘要:
      A method was developed for the determination of Polychlorinated biphenyls (PCBs) in air by stir bar sorptive extraction-thermal desorption-gas chromatography-mass spectrometry (SBSE-TD-GC-MS) using polydimethylsiloxane (PDMS)-coated stir bar for passive air sampler. The optimized conditions for desorption temperature, desorption time and cryofocusing temperature were found to be 280℃,6 min and -40℃,respectively,along with the carry-over of up to 7% for 33 PCB congeners. Linearity,precision and repeatability of the method were investigated. The proposed method showed excellent linearities for 33 PCB congeners,with the correlation coefficients (r) > 0. 998 for 5 point calibrations. Better precision,intra-day repeatability and inter-day repeatability were obtained with RSDs (relative standard deviation) in the ranges of 0. 79% -20. 2% (n=8),0. 43%-29. 8% (n=10) and 3. 20% -29. 6% (n=20), respectively. Detection limits ranged from 0. 01 to 2. 51 pg, and the average recovery was 98% ± 18%. The developed method was applied to monitor PCBs in the atmosphere of Beijing. Eight PCB congeners were detected and the contents were in the range of 2. 94-129 pg. PCB-52, PCB-123 and PCB-155 were always in the linear uptake phase,whereas PCB-1 and PCB-3 experienced linear uptake phase,curvilinear uptake phase and equilibrium phase during the sampling campaign of 32 days. The results indicated that SBSE-TD-GC-MS could be employed for sampling and quick determination of PCBs in atmosphere.
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