Simultaneous determination of perfluoroalkyl phosphonates, carboxylates, and sulfonates in drinking water
Simultaneous determination of perfluoroalkyl phosphonates, carboxylates, and sulfonates in drinking water
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DOI：
10.1016/j.chroma.2011.07.005
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发表时间：
2011-09-16
影响因子：
4.1
通讯作者：
Berger, Urs
中科院分区：
文献类型：
--
作者：
Ullah, Shahid;Alsberg, Tomas;Berger, Urs
建立了高效液相色谱-四极杆飞行时间高分辨质谱法同时测定全氟烷基膦酸酯（PFPAs，碳链长度C6，8，10）和全氟烷基羧酸酯（PFCAs）的痕量分析方法。C5-12）和全氟烷基磺酸盐（PFSA）。C4、6、8、10）。使用固相萃取将分析物富集在混合模式共聚物吸附剂（C8 +季胺）上。在Zorbax Extend C18反相柱上，使用由水、甲醇和乙腈（含2 mM乙酸铵和5 mM 1-甲基哌啶）组成的移动的相梯度进行色谱分离。质谱仪以电喷雾负离子模式操作。在移动的相中使用1-甲基哌啶，通过改善色谱分辨率、背景抑制和提高电离效率，使PFPA的仪器灵敏度显著增加。方法的检出限为0.095-0.17 ng/L、0.027-0.17 ng/L和0.014-0.052 ng/L。PFCA和PFSA。在加标水平为0.5 ng/L至500 mL HPLC级水中时，PFPAs和PFCAs的整个方法回收率分别为40- 56%、56- 97%和55-77%。和PFSA。在检测自来水提取物中的PFPA时观察到基质效应（信号增强），导致在0.5 ng/L加标水平下计算的回收率为249-297%。该效应导致PFPA方法灵敏度的额外提高。以补偿母体效应。使用基质匹配和提取的校准标准品定量自来水中的PFPAs。该方法已成功应用于从六个欧洲国家收集的饮用水的分析。在荷兰阿姆斯特丹的两个水样中，除了全氟辛基膦酸盐（PFOPA）接近0.095纳克/升的检测限外，没有检测到全氟磷酸盐。阿姆斯特丹的样本中发现全氟丁磺酸盐（PFBS，18.8纳克/升）和全氟辛酸盐（PFOA，8.6纳克/升）含量最高，瑞典斯德哥尔摩的自来水中也发现全氟辛烷磺酸盐（PFOS，8.8纳克/升）含量最高。(C)2011 Elsevier B. V.保留所有权利。
A trace analytical method based on high performance liquid chromatography coupled to quadrupole time-of-flight high resolution mass spectrometry was developed for simultaneous determination of perfluoroalkyl phosphonates (PFPAs, carbon chain lengths C6,8,10), perfluoroalkyl carboxylates (PFCAs. C5-12), and perfluoroalkyl sulfonates (PFSAs. C4,6,8,10) in drinking water (tap water). Analytes were enriched on a mixed mode co-polymeric sorbent (C8 + quaternary amine) using solid phase extraction. Chromatographic separation was achieved on a Zorbax Extend C18 reversed phase column using a mobile phase gradient consisting of water, methanol, and acetonitrile containing 2 mM ammonium acetate and 5 mM 1-methyl piperidine. The mass spectrometer was operated in electrospray negative ion mode. Use of 1-methyl piperidine in the mobile phase resulted in a significant increase in instrument sensitivity for PFPAs through improved chromatographic resolution, background suppression, and increased ionization efficiency. Method detection limits for extraction of 500 mL tap water were in the ranges of 0.095-0.17 ng/L, 0.027-0.17 ng/L, and 0.014-0.052 ng/L for PFPAs. PFCAs, and PFSAs, respectively. Whole method recoveries at a spiking level of 0.5 ng/L to 500 mL HPLC grade water were 40-56%, 56-97%, and 55-77% for PFPAs, PFCAs. and PFSAs, respectively. A matrix effect (signal enhancement) was observed in the detection of PFPAs in tap water extracts, leading to calculated recoveries of 249-297% at a 0.5 ng/L spiking level. This effect resulted in an additional improvement of method sensitivity for PFPAs. To compensate for the matrix effect. PFPAs in tap water were quantified using matrix-matched and extracted calibration standards. The method was successfully applied to the analysis of drinking water collected from six European countries. PFPAs were not detected except for perfluorooctyl phosphonate (PFOPA) at close to the detection limit of 0.095 ng/L in two water samples from Amsterdam, the Netherlands. Highest levels were found for perfluorobutane sulfonate (PFBS, 18.8 ng/L) and perfluorooctanoate (PFOA, 8.6 ng/L) in samples from Amsterdam as well as for perfluorooctane sulfonate (PFOS, 8.8 ng/L) in tap water from Stockholm, Sweden. (C) 2011 Elsevier B.V. All rights reserved.