超高效液相色谱-新型串联四极杆质谱法测定环境水体与土壤中的全氟辛酸和全氟辛烷磺酸
Determination of perfluorooctanoic acid and perfluorooctanesulfonates in environmental water and soil matrixes using ultra high performance liquid chromatography coupled with state-of-art tandem quadrupole mass spectrometry
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摘要: 本文建立了基于超高效液相色谱与新型的Ultivo串联四极杆质谱联用技术测定环境水体与土壤中全氟辛酸(PFOA)和全氟辛烷磺酸(PFOS)的方法.水样和土壤样品分别经过过滤和提取后,经弱阴离子交换柱富集净化后,采用同位素稀释法进行定量.在0.5-200 μg·L-1范围内,PFOA和PFOS的线性响应良好,回归系数大于0.997.水样PFOA和PFOS的检出限分别为0.1 ng·L-1和0.3 ng·L-1;土壤检出限分别为4 ng·kg-1和7 ng·kg-1.PFOA和PFOS在纯水、地表水和废水基质中的添加回收率分别介于88.4%-98.8%和88.0%-97.3%之间,相对标准偏差(RSD,n=6)小于14%.二者在空白土、农田土和底泥中的回收率分别介于98.6%-113%和96.8%-111%之间,RSD小于7%.结果表明,该方法灵敏、准确、可靠,可以满足环境水与土壤介质中痕量PFOA和PFOS的监测要求.
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关键词:
- 全氟辛酸(PFOA) /
- 全氟辛烷磺酸(PFOS) /
- 液相色谱串联质谱法 /
- 水 /
- 土壤
Abstract: To establish determination of perfluorooctanoic acid and perfluorooctanesulfonates in environmental water and soil matrixes using ultra high performance liquid chromatography coupled with state-of-art tandem quadrupole mass spectrometry。In the range of 0.5-200 mg·L-1, the linear response of PFOA and PFOS is good, and the regression coefficient is greater than 0.997. The detection limits of water samples PFOA and PFOS were 0.1 and 0.3 ng·L-1, respectively; the soil detection limits were 4 and 7 ng·kg-1, respectively. The recovery rates of PFOA and PFOS in pure water, surface water and wastewater matrix were between 90.7%-98.8% and 88.0%-97.3%, respectively, and the relative standard deviation (RSD, n=6) was less than 14%. The recoveries of the two in blank soil, farm soil and sediment were between 98.6%-113% and 96.8%-111%, respectively, and the RSD was less than 7%. -
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[1] LOOS R, LOCORO G, HUBER T, et al. Analysis of perfluorooctanoate (PFOA) and other perfluorinated compounds (PFCs) in the River Po watershed in N-Italy[J].Chemosphere, 2008, 71(2):306-313. [2] PAN Y Y, SHI Y L, WANG J M, et.al. Evaluation of perfluorinated compounds in seven wastewater treatment plants in Beijing urban areas[J]. Sci. China Chem. 2011, 54(3):552-558. -
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