| 摘要: |
| 建立了固相萃取-超高效液相色谱串联质谱法（UPLC- MS/MS）检测土壤和沉积物中11种全氟羧酸和7种全氟磺酸的分析方法。称取土壤和沉积物样品3.0g左右，以10mL 50%甲醇水为萃取溶剂，常温振荡萃取10min后离心，萃取液经WAX固相萃取柱净化，浓缩后50%甲醇水定容至1mL，经UPLC- MS/MS检测，内标法定量。结果显示，18种 PFCs 在?1~100μg/L范围内线性关系良好，相关系数均>0.995，检出限（LOD）在0.06~0.91μg/kg之间，定量限（LOQ）在0.24~3.63μg/kg之间。对土壤和沉积物实际样品分别进行3个浓度水平的加标回收实验，土壤样品的加标回收范围为92.4%~134%，精密度为1.37%~18.8%。沉积物样品加标回收范围为76.8%~129%，精密度为5.66%-24.9%。该方法操作简便，灵敏度高、准确性和重现性良好，可满足土壤和沉积物中11种全氟羧酸和7种全氟磺酸的检测需要。 |
| 关键词: 高效液相色谱串联质谱，全氟羧酸，全氟磺酸，土壤，沉积物，固相萃取 |
| DOI： |
| 分类号:R15 |
| 基金项目:上海市2021年度“科技创新行动计划”科学仪器领域项目 |
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| Determination of 11 Perfluorocarboxylic Acids And 7 Perfluorosulfonic Acids In Soil And Sediment by Solid phase extraction-UPLC- MS/MS |
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| Abstract: |
| A solid-phase extraction ultra high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method was established to detect 11 perfluorocarboxylic acids and 7 perfluorosulfonic acids in soil and sediment. Weigh about 3.0g of soil and sediment samples, extract with 50% methanol water as the extraction solvent, shake at room temperature for 30 minutes, centrifuge, purify the extract with a Wax solid-phase extraction column, concentrate to 1mL with 50% methanol water, detect by UPLC-MS/MS, and quantify by internal standard method. The results showed that there was a good linear relationship among 18 PFCs in the range of 1-100 μ g/L, with correlation coefficients>0.995. The detection limit (LOD) was between 0.06 and 0.91 μ g/kg, and the quantification limit (LOQ) was between 0.24 and 3.63 μ g/kg. Three concentration levels of spiked recovery experiments were conducted on actual soil and sediment samples, with a spiked recovery range of 92.4% ~134% and a precision of 1.37% ~18.8%. The range of spiked recovery for sediment samples is 76.8%~129%, with a precision of 5.66%~24.9%. This method is easy to operate, highly sensitive, accurate, and reproducible, and can meet the detection needs of 11 perfluorocarboxylic acids and 7 perfluorosulfonic acids in soil and sediment. |
| Key words: UPLC-MS/MS, perfluorocarboxylic acid, perfluorosulfonic acid, soil, sediment, solid-phase extraction |
