| 大体积直接进样-超高效液相色谱-串联质谱法测定水中20种全氟化合物方法研究 |
| Study on the Determination of 20 Perfluorinated Compounds in Water by Large Volume Direct Injection-Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry |
| 投稿时间：2025-02-26 修订日期：2025-05-26 |
| DOI：10.19316/j.issn.1002-6002.2026.01.04 |
| 中文关键词: 直接进样 超高效液相色谱-串联质谱法 地表水 地下水 海水 全氟化合物 |
| 英文关键词:direct injection ultra-high performance liquid chromatography-tandem mass spectrometry surface water groundwater seawater perfluorinated compounds |
| 基金项目:济南市科技计划民生专项项目(201913015);山东省重点研发计划(重大科技创新工程)(2019JZZY020705) |
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| 中文摘要: |
| 目前,采用大体积直接进样方法分析全氟化合物的相关研究还鲜有报道,且现行标准中还未有对该方法的规定。对大体积直接进样方法的各影响因素进行了分析测试和优化,建立了采用大体积直接进样-超高效液相色谱-串联质谱法测定水中20种全氟化合物的高通量方法,并对实际样品进行了检测。该方法在1~100 ng/L范围内线性良好,测定结果相关系数均大于0.995,检出限为0.1~0.6 ng/L,测定下限为0.4~2.4 ng/L,地表水样品加标回收率为71.8%~119%,地下水样品加标回收率为72.8%~123%,海水样品加标回收率为71.4%~121%(全氟戊烷磺酸除外),不同浓度纯水加标样品测定结果的相对标准偏差为0.4%~10.4%。该方法操作简便、精密度好、灵敏度高,具有广阔的应用前景,已成功应用于济南市地表水、地下水及莱州湾海水样品分析测试,可为我国环境水体全氟化合物监管提供技术支撑。 |
| 英文摘要: |
| Currently,there are few reports on the analysis of perfluorinated compounds using the large-volume direct injection method,and no existing standards specify procedures for this method.Various influencing factors of the large-volume injection method were analyzed,tested,and optimized in this study,and a high-throughput detection method for determining 20 perfluorinated compounds in water using direct injection coupled with ultra-high performance liquid chromatography-tandem mass spectrometry was established.The method was applied to actual surface water and groundwater samples.The method showed good linearity within the range of 1-100 ng/L,with correlation coefficients for the determination results all greater than 0.995.The detection limit ranged from 0.1 to 0.6 ng/L,and the lower limit of determination ranged from 0.4 and 2.4 ng/L.Spiked recovery rates for surface water samples spanned from 71.8% to 119%,groundwater samples from 72.8% to 123%,and seawater samples from 71.4% to 121% (excluding perfluoropentanesulfonic acid).The relative standard deviations for the determination results of spiked pure water samples was between 0.4% and 10.4%.This method is simple to operate,has good precision and high sensitivity,with broad application prospects.It has been successfully applied to the analysis and testing of surface water,groundwater samples from Jinan City,and seawater samples from Laizhou Bay,providing technical support for the regulation of perfluorinated compounds in environmental water bodies in China. |
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