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在线固相萃取-液相色谱-串联质谱法直接测定水中15种全氟烷基化合物
Direct Determination of 15 Kinds of Perfluoroalkyl Substances in Water by Liquid Chromatography-Tandem Mass Spectrometry Coupled with Online Solid Phase Extraction
投稿时间:2022-09-17  修订日期:2023-11-15
DOI:10.19316/j.issn.1002-6002.2024.02.21
中文关键词:  全氟烷基化合物  地表水  末梢水  在线固相萃取  液相色谱-串联质谱
英文关键词:perfluoroalkyl substances (PFASs)  surface water  tap water  on-line solid phase extraction (on-line SPE)  liquid chromatography tandem mass spectrometry
基金项目:成都市水环境新污染物监测研究项目(2021CD22)
作者单位
赵陈晨 四川省成都生态环境监测中心站, 四川 成都 610000 
陈勇 四川省成都生态环境监测中心站, 四川 成都 610000 
侯晓玲 四川省成都生态环境监测中心站, 四川 成都 610000 
李思思 四川省成都生态环境监测中心站, 四川 成都 610000 
吴佳伦 四川省成都生态环境监测中心站, 四川 成都 610000 
陈娟 四川省成都生态环境监测中心站, 四川 成都 610000 
王萍* 四川省成都生态环境监测中心站, 四川 成都 610000 
通讯作者:王萍*  四川省成都生态环境监测中心站, 四川 成都 610000  
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中文摘要:
      通过优化样品保存、前处理、分析条件,建立了水中15种典型全氟烷基化合物(PFASs)在线固相萃取-液相色谱-串联质谱分析方法,并对饮用水水源地和末梢水中PFASs进行定量检测。水样过膜后,准确移取700 μL水样、300 μL甲醇至1.5 mL聚丙烯进样瓶,并加入同位素内标后直接进样800 μL至在线固相萃取流路,进行萃取富集,再通过十通阀切换将洗脱的PFASs转移至分析流路进行分离,质谱检测,内标法定量。方法分析总时长22 min,15种全氟烷基化合物的方法检出限为0.31~1.20 ng/L,纯水高、中、低浓度加标样品回收率为70%~115%,相对标准偏差为0.2%~14.0%(n=6)。经实际样品验证,该方法与传统手动固相萃取方法分析结果基本一致。结果表明,该方法操作简单、自动化程度高、有机试剂用量少、灵敏度高、方法稳定,可满足地表水和末梢水中PFASs的快速测定。
英文摘要:
      A method of automated on-line solid phase extraction-liquid chromatography-tandem mass spectrometry (on-line SPE LC-MS/MS) to analyze 15 kinds of perfluoroalkyl substances (PFASs) in water was developed by optimizing the conditions of sample saving, pre-treatment and analysis, and the PFASs in drinking water source and peripheral water were quantitatively detected. After passing through the membrane filter,a 700 μl sample was moved into a 1. 5 mL autosampler vials with 300 μL methanol. A 800 μl sample was directly injected into the online SPE flow path. Online purification and enrichment of the samples were carried out on the SPE column (Bio WAX NP3,4 mm×10 mm,3 μm). The PFASs were eluted from the SPE column and then transferred to the analytical flow path by valve switching. PFASs were separated on HPH-C18 column (2. 1 mm×50 mm,2. 7 μm),and further analyzed by mass spectrometer detector, and quantified by using isotope internal standard method. The total analysis time of the method was 22 min. The detection limits of PFASs were in 0. 31-1. 20 ng/L. The average recoveries for 15 PFASs at low,medium and high spiked levels ranged from 70% to 115%,with relative standard deviations (RSD,n=6) of 0. 2%-14. 0%. PFASs concentrations in the real samples analyzed by this method and conventional method were close to each other,but the proposed method was simple,rapid,high automation and solvent-saving. The established method was sensitive and accurate, and suitable for detection of 15 kinds of PFASs in surface water.
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