首页|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

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

扫码查看
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.
Determination of 33 Polychlorinated Biphenyls in the Atmosphere of Beijing Using Stir Bar Sorptive Extraction-Thermal Desorption Coupled with Gas Chromatography-Mass Spectrometry
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.

stir bar sorptive extractionthermal desorptionpolychlorinated biphenylspassive air sampling

李红华、李英明、李晓敏、孙慧中、夏莎莎、张庆华

展开 >

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

中国农业科学院农业质量标准与检测技术研究所,北京 100081

国家地质实验测试中心,北京 100037

搅拌子吸附 热脱附 多氯联苯 被动大气采样

国家自然科学基金中国科学院技术支撑人才项目(2021)

21307148

2024

中国环境监测
中国环境监测总站

中国环境监测

CSTPCD北大核心
影响因子:1.761
ISSN:1002-6002
年,卷(期):2024.40(2)
  • 29