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宠物毛发中全氟/多氟化合物的固相萃取/高效液相色谱-串联质谱分析方法研究 被引量:1

Study on Analysis Method of Per-and Polyfluoroalkyl Substances in Pet Fur by High Performance Liquid Chromatography-Tandem Mass Spectrometry Combined with Solid Phase Extraction
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摘要 该研究对宠物毛发中全氟/多氟化合物(PFAS)的萃取方法进行优化,建立了固相萃取/高效液相色谱-串联质谱(SPE/HPLC-MS/MS)同时测定宠物毛发中包括替代品6∶2氯代多氟醚磺酸(6∶2 Cl-PFESA)和全氟壬烯氧基苯磺酸钠(OBS)在内的24种PFAS的分析方法。样品以乙腈为溶剂超声和振荡萃取2次,萃取液用弱阴离子交换(WAX)固相萃取柱进行净化,收集洗脱液氮吹浓缩后进行HPLC-MS/MS分析。在优化条件下,目标化合物的仪器检出限(LOD)和方法检出限(MDL)分别为0.005~0.136 ng/mL和0.009~0.273 ng/g。24种PFAS的加标回收率为66.2%~110%,相对标准偏差(RSD)为1.5%~21%。采用该方法对52个实际宠物毛发样品进行分析,24种PFAS均被检出,检出率为3.8%~98.1%,PFAS总含量为0.89~17.94 ng/g,平均含量为5.02 ng/g。该方法灵敏度高、稳定性好,应用于宠物毛发中PFAS分析可获得满意的结果。 Since pets and humans are in the same environment,analyzing the concentrations of perand polyfluoroalkyl substances(PFAS)in pet fur and evaluating pet exposure to PFAS can reflect hu⁃man exposure to a certain extent,which is important for risk assessment.In this study,extraction conditions in the pretreatment process were optimized,and a high performance liquid chromatogra⁃phy-tandem mass spectrometry combined with solid phase extraction(SPE/HPLC-MS/MS)method was established for the detection of 24 PFAS including the 6∶2 chlorinated polyfluoroalkyl ether sul⁃fonic acid(6∶2 Cl-PFESA)and sodium p-perfluorous nonenoxybenzene sulfonate(OBS)in pet fur.The samples were ultrasonically extracted with acetonitrile two times,and then the extracts were cleaned up by weak anion exchange(WAX)cartridges.Finally,the eluent were collected and con⁃centrated for the detection of PFAS by HPLC-MS/MS.The instrument detection limits(LODs)and method detection limits(MDLs)ranged from 0.005-0.136 ng/mL and 0.009-0.273 ng/g,respec⁃tively.The recoveries of 24 PFAS in pet fur were 66.2%-110%and the relative standard deviations(RSDs)were 1.5%-21%.The optimized method was applied to detect PFAS in 52 pet fur samples.The results showed that 24 PFAS were detected with detection rates ranging from 3.8%to 98.1%.The total contents of 24 PFAS ranged from 0.89-17.94 ng/g,with a mean content of 5.02 ng/g.This method has the advantages of high sensitivity,good stability,and satisfactory results can be obtained when applied to the analysis of PFAS in pet fur.
作者 杨晨 李鹏飞 王媛 史亚利 YANG Chen;LI Peng-fei;WANG Yuan;SHI Ya-li(College of Environmental Science and Engineering,Hebei University of Science and Technology,Shijiazhuang 050018,China;State Key Laboratory of Environmental Chemistry and Ecotoxicology,Research Center for Eco-Environmental Sciences,Chinese Academy of Sciences,Beijing 100085,China)
出处 《分析测试学报》 CAS CSCD 北大核心 2024年第8期1227-1234,共8页 Journal of Instrumental Analysis
基金 国家自然科学基金项目(22320102005,22176198) 河北省高等学校青年拔尖人才项目(BJK2022042)。
关键词 全氟/多氟化合物 宠物毛发 固相萃取 高效液相色谱-串联质谱 per-and polyfluoroalkyl substances pet fur solid phase extraction high perfor⁃mance liquid chromatography-tandem mass spectrometry
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