分析化学2024，Vol.52Issue(2)：286-295,后插1-后插5,15.DOI:10.19756/j.issn.0253-3820.231167
在线固相萃取净化-液相色谱-串联质谱法直接测定植物粗提物中的23种全氟化合物
Direct Determination of 23 Kinds of Per-and Polyfluoroalkyl Substances in Crude Plant Extracts by Liquid Chromatography-Tandem Mass Spectrometry Coupled with Online Solid Phase Extraction
摘要
Abstract
A new method for simultaneous determination of 23 kinds of per-and polyfluoroalkyl substances(PFASs)(13 kinds of perfluoro carboxylic acids,4 kinds of perfluoro sulfonic acids,and 6 kinds of new substitutes)in plant leaf tissue by ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)using automatic online solid phase extraction(SPE)to remove the matrix interference components in plant crude extracts was developed.The plant leaf samples were extracted twice with 1%formic acid-methanol solution,then evaporated to dry,redissolved with 70%methanol solution,and directly injected for analysis.After 23 kinds of target PFASs were purified automatically by online SPE with a WAX column,the six-way valve was switched to rinse PFASs onto an alkaline mobile phase system-compatible C18 analytical column.Then,the 23 kinds of target PFASs were separated within 16 min by gradient elution using a binary mobile phase system of methanol/water(Containing 0.4%ammonium hydroxide).Tandem mass spectrometry was performed in multiple reaction monitoring(MRM)mode for online detection of various PFASs,and quantification was carried out by internal standard method.The results of the method validation showed that satisfactory average recoveries of 23 kinds of PFASs in plant leaf samples(64.2%-125.5%),precision(relative standard deviations(RSDs)of 0.7%-12.8%),linearity(R2＞0.990),and sensitivity(the detection limits(S/N=3)were in the range of 0.02-0.50 μg/kg)were achieved.Finally,this method was used to detect PFASs in the marine green tide algae(Enteromorpha prolifera)and several tree leaves,and a total of 6 kinds of PFASs were detected,in which PFBA was the main contaminant.Compared with the reported offline SPE methods,the proposed online SPE technique significantly simplified the sample pretreatment process and provided an automatic,simple,and environment-friendly method for the routine monitoring of legacy and emerging PFASs in plant tissues.关键词
在线固相萃取/植物叶片/全氟化合物/超高效液相色谱-串联质谱Key words
Online solid phase extraction/Plant leaves/Per-and polyfluoroalkyl substances/Ultra-performance liquid chromatography-tandem mass spectrometry引用本文复制引用
申楠,韩同竹,盛璨璨,何秀平,陈军辉,刘晨光,李先国..在线固相萃取净化-液相色谱-串联质谱法直接测定植物粗提物中的23种全氟化合物[J].分析化学,2024,52(2):286-295,后插1-后插5,15.基金项目
浙江省污染暴露与健康干预重点实验室开放基金项目(No.20220104)和国家自然科学基金委-山东省联合基金项目(No.U1706217)资助.Supported by the Key Laboratory of Pollution Exposure and Health Intervention of Zhejiang Province,China(No.20220104)and the National Natural Science Foundation of China-Shandong Joint Fund(No.U1706217). （No.20220104）
