首页|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

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

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  • 国家科技期刊平台
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  • NSTL
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采用全自动在线固相萃取净化技术去除植物粗提物中的基质干扰组分,建立了一种超高效液相色谱-串联质谱(UHPLC-MS/MS)同步测定植物叶片组织中23种全氟化合物(Per-and polyfluoroalkyl substances,PFASs)(13种全氟羧酸类、4种全氟磺酸类和6种新型替代品)的新方法.植物样品经1%甲酸-甲醇溶液提取两次再旋蒸至干,用70%甲醇溶液复溶后直接进样分析.通过WAX在线固相萃取柱对PFASs进行自动化净化后,切换六通阀,将PFASs冲洗至适用于碱性流动相体系的C18 分析柱上,采用含0.4%氨水的甲醇/水二元流动相体系进行梯度洗脱,在16 min内即可实现各目标化合物的色谱分离.采用串联质谱在多重反应监测(MRM)模式下进行PFASs的在线检测,并用内标法进行定量分析.方法学考察结果表明,植物叶片样品中23种目标PFASs的平均加标回收率为64.2%～125.5%,相对标准偏差(RSD)为0.7%～12.8%,各目标PFASs在相应的质量浓度范围内线性关系良好,相关系数(R2)大于0.990,检出限(LOD,S/N=3)在0.02～0.50 μg/kg之间.采用本方法对海洋绿潮藻浒苔和4种树叶实际样品中的PFASs进行检测,共检出6种PFASs,其中PFBA为主要污染物.与文献报道的离线固相萃取法相比,本方法简化了样品前处理过程,为植物组织中典型PFASs及其新型替代品的日常监测提供了一种简便、快捷和准确的方法.
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
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.

Online solid phase extractionPlant leavesPer-and polyfluoroalkyl substancesUltra-performance liquid chromatography-tandem mass spectrometry

申楠、韩同竹、盛璨璨、何秀平、陈军辉、刘晨光、李先国

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中国海洋大学,海洋化学理论与工程技术教育部重点实验室,青岛 266100

自然资源部第一海洋研究所,自然资源部海洋生态环境科学与技术重点实验室,青岛 266061

青岛市现代分析与近海生态环境安全保障重点实验室,青岛 266061

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

浙江省污染暴露与健康干预重点实验室开放基金项目国家自然科学基金委-山东省联合基金项目

20220104U1706217

2024

10.19756/j.issn.0253-3820.231167

分析化学
中国化学会 中国科学院长春应用化学研究所

分析化学

CSTPCD北大核心
影响因子：1.423
ISSN：0253-3820
年,卷(期)：2024.52(2)
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