全/多氟烷基化合物(perfluoro and polyfluoroalkyl substances，PFASs)在水环境中具有生态毒性、长距离迁移性、能随食物链富集等特点。随着水环境中PFASs的暴露风险不断增加，PFASs检测技术逐渐成为研究人员关注的热点。文章改进了固相萃取法富集水样、超声振荡-提取法提取沉积物样品的前处理条件，优化了液相色谱和三重四极杆质谱分离检定条件，整合建立了适用于测定环境水相与沉积物中19种PFASs的超高效液相色谱-三重四极杆质谱检测方法。试验结果表明，水相中19种PFASs在低、中、高浓度下加标回收率分别为60。2％～120。0％、74。3％～114。2％、65。4％～107。2％，相对标准偏差(RSD)分别为2。1％～12。1％、4。5％～11。7％、4。3％～9。8％。沉积物中19种PFASs低、中、高3个浓度的加标回收率分别为80。3％～124。1％、89。9％～104。3％、95。1％～105。7％，RSD 分别为 5。0％～14。3％、3。1％～10。9％、2。6％～9。9％。水相和沉积物中PFASs在一定线性范围内具有良好线性，方法检出限为0。2～0。5 ng/L和0。1～0。6 ng/g，方法定量限为0。8～2。0 ng/L和0。4～2。5 ng/g。该方法前处理简单，方法学指标好，适用于各类型水质和沉积物中PFASs的高通量检测。
Determination of 19 PFASs Compounds in Environmental Water and Sediments with Ultra-High Performance Liquid Chromatography-Triple Quadrupole Mass Spectrometry
Perfluoro and polyfluoroalkyl substances(PFASs)are known for their ecological toxicity,long-range mobility,and propensity for bioaccumulation through the food chain within aquatic environments.As the exposure risks of PFASs in water environments continue to escalate,the development of PFASs detection techniques has become a focal point for researchers.This study has refined the pre-treatment conditions for the enrichment of water samples using solid-phase extraction and the extraction of sediment samples using an ultrasonic oscillation-extraction method.Additionally,it has optimized the separation and identification conditions for liquid chromatography and triple quadrupole mass spectrometry,integrating an ultra-high-performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)detection method suitable for the quantification of 19 types of PFASs in environmental water and sediment matrices.Experimental results indicated that the recovery rates of 19 PFASs at low,medium,and high concentrations in the aqueous phase and sediment are 60.2％to 120.0％,74.3％to 114.2％,and 65.4％to 107.2％,respectively,with relative standard deviations(RSD)of 2.1％to 12.1％,4.5％to 11.7％,and 4.3％to 9.8％,respectively.In the sediment,the recovery rates of 19 PFASs at the three concentrations of low,medium,and high were 80.3％to 124.1％,89.9％to 104.3％,and 95.1％to 105.7％,with RSD values of 5.0％to 14.3％,3.1％to 10.9％,and 2.6％to 9.9％,respectively.The PFASs in both the aqueous phase and sediment exhibited good linearity within a certain range,with method detection limits of 0.2 ng/L to 0.5 ng/L and 0.1 ng/g to 0.6 ng/g,and method quantification limits of 0.8 to 2.0 ng/L and 0.4 to 2.5 ng/g.This method has a simple pretreatment process,good methodological indicators,and is suitable for high-throughput detection of PFASs in various types of water quality and sediment.
perfluoro and polyfluoroalkyl substances(PFASs)watersedimentpretreatmentanalytical method
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