| 摘要: |
| 采用微波萃取方式，结合全自动固相萃取和超高效液相色谱-串联质谱技术，开发了一种高效的可以同步测定土壤中26种全氟及多氟烷基化合物（PFAS）的分析方法。采用0.5%氨水-甲醇作为提取溶剂，通过混合型反相弱阴离子交换柱（WAX柱）富集后，用1%氨水-甲醇洗脱。以BEH C18色谱柱分离，采用负离子模式的电喷雾电离源，在靶向质谱采集模式（MRM）下进行质谱分析，内标法进行定量。实验结果显示，土壤中26种目标PFAS的加标回收率为63.5%～112.3%，相对标准偏差为0.4%～18.8%，方法的线性关系较好，相关系数均＞0.995，检出限为0.02～0.13 μg/kg。该方法为土壤中PFAS的准确测定提供了有效手段。 |
| 关键词: 全自动固相萃取 土壤 全氟/多氟烷基化合物 超高效液相色谱-串联质谱 |
| DOI：DOI：10.3969/j.issn.1674-6732.2025.02.010 |
| 分类号:X833 |
| 基金项目:江苏省生态环境监测科研基金项目（2315） |
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| Determination of 26 Perfluoroalkyl and Polyfluoroalkyl Substances（PFAS） in Soil by Automatic Solid-Phase Extraction Purification， Ultra-High-Performance Liquid Chromatography-Tandem Mass Spectrometry |
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CAI Ye， YIN Yanmin， XU Zhenqiu， SUN Xinyang
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Jiangsu Suzhou Enviromental Monitoring Center， Suzhou， Jiangsu 215000， China
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| Abstract: |
| An efficient method for simultaneous determination of 26 different perfluorinated and polyfluoroalkyl compounds（PFAS） in soil was developed by microwave extraction， automatic solid-phase extraction and ultra-high performance liquid chromatography-tandem mass spectrometry（ASPE-UPLC-MS/MS）. 0.5% ammonia-methanol solution was used as the extraction solvent， enriched through a mixed-mode reversed-phase weak anion exchange column（WAX column）， and eluted with 1% ammonia-methanol. Separation was achieved using a BEH C18 chromatographic column， with ionization in the electrospray negative ion mode， and mass spectrometric detection under multiple reaction monitoring mode， quantified using an internal standard method. The experimental results showed that the spiked recovery rates of 26 target PFAS in soil ranged from 63.5% to 112.3%， with relative standard deviations of 0.4% to 18.8%. The established method demonstrated good linearity， with correlation coefficients greater than 0.995， and detection limits ranging from 0.02 to 0.13 μg/kg， providing an effective means for the accurate determination of PFAS in soil. |
| Key words: Automatic solid-phase extraction Soil Perfluoroalkyl and polyfluoroalkyl substances Ultra performance liquid chromatography-tandem mass spectrometry |
