首页|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

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

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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.
Direct Determination of 15 Kinds of Perfluoroalkyl Substances in Water by Liquid Chromatography-Tandem Mass Spectrometry Coupled with Online Solid Phase Extraction
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.

perfluoroalkyl substances(PFASs)surface watertap wateron-line solid phase extraction(on-line SPE)liquid chromatography tandem mass spectrometry

赵陈晨、陈勇、侯晓玲、李思思、吴佳伦、陈娟、王萍

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四川省成都生态环境监测中心站,四川 成都 610000

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

成都市水环境新污染物监测研究项目

2021CD22

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)
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