摘要
本研究基于在线湍流固相萃取-高效液相-串联质谱(on-line TF-SPE-HPLC-MS/MS),建立了一种用于直接检测血清中21种化合物全氟及多氟类化合物(PFASs,13种全氟羧酸,5种全氟磺酸,2种氯化多氟醚基磺酸盐,1种全氟磺酰胺)的全自动检测方法。通过对高效液相相关参数、湍流柱、进样体积、载样流速和时间以及洗脱时间的优化,所有目标化合物在0.1-100 ng/m L范围内呈现良好的线性关系(r2>0.99),检测限在0.008-0.063 ng/m L之间,相对偏差低于10%。本方法在血清样品中0.5ng/m L、5 ng/m L及50 ng/m L的加标回收率在83.8%至119%之间。与传统离线方法相比,本方法极大的减少了人工操作带来的误差,显著地降低了溶剂的使用量;相对于现有文献中的在线方法,本方法血清无需经过任何的前处理而直接进样。此外,与现有文献报导的PFASs检测方法比较,本方法在短链(碳链长度小于6)和长链PFASs(碳链长度大于12)的检测中表现出更低的检出限和更优的回收率。
An automated method for determining 21 per-and polyfluoroalkyl substances(13 PFCAs,5 PFSAs,PFOSA,and 2 Cl-PFESAs) in human serum samples by on-line Turboflow-SPE-HPLC-MS/MS) was developed.Under the optimized condition,the analytical method displayed good linearity(r2 >0.99) for all PFASs over a concentration range of 0.1-100 ng/m L.The limits of detection(LOD) were between 0.008 and 0.063 ng/m L,the matrix spiked recoveries of 21 PFASs were in the range of 83.8 %-119 % at 0.5 ng/m L,5 ng/m L and 50 ng/m L levels.Our on-line SPE method had significant advantages over off-line methods at a minimization of manual handling,significantly decreasing solvent use,time-consuming and costs.Additionally,present method also showed advantages over literature on-line methods in injecting directly without any sample preparation,and lower LODs,more excellent recovery of short(C<6) and long chain(C>12) PFASs than both previous off-line and on-line methods.
引文
[1]Huber,S.&Brox,J.Anal and Bioa Chem.2015.
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