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蔬菜中全氟/多氟化合物的固相萃取-超高效液相色谱-串联质谱分析方法研究
Method of per-and polyfluoroalkyl substances(PFAS) in vegetables by solid phase extraction combined with ultra-high performance liquid chromatography-tandem mass spectrometry
【摘要】 食用蔬菜已被确认为人类接触全氟/多氟化合物(PFAS)的一个重要途径,蔬菜可以通过土壤和灌溉水等途径吸收PFAS,从而在其组织中积累,威胁人类健康.因此监测蔬菜中PFAS含量,对于评估其潜在风险具有重要意义.本文基于有机溶剂提取固相萃取净化的前处理方法,通过优化提取溶剂和固相萃取柱填料,建立了一种固相萃取-超高效液相色谱-串联质谱(SPE-UPLC-MS/MS)测定小青菜、卷心菜和空心菜等叶菜类蔬菜中24种PFAS的分析方法.以碱性甲醇作为提取溶剂,通过涡旋振荡提取蔬菜中的PFAS,并使用ENVI-18固相萃取柱对提取液进行净化,采用串联质谱在多重反应监测模式下进行PFAS的检测,并用内标法进行定量分析.在优化的分析条件下,当加标水平为2 ng时,加标回收率和相对标准偏差(RSD)分别为50.0%—120.8%和1.0%—26%,各目标PFAS在相应的质量浓度范围内线性关系良好,相关系数(r)大于0.99,检出限(LOD,S/N=3)在0.002—0.103 ng·g-1之间,定量限(LOQ,S/N=10)在0.007—0.343 ng·g-1之间.采用本方法对实际样品中的PFAS进行检测,共检出20种PFAS,其中10种PFAS的检出率为100%,PFAS总浓度范围为2.92—6.83 ng·g-1干重(dw).全氟丁酸(PFBA)为主要污染物,浓度范围为1.18—3.74 ng·g-1dw.本方法展示了良好的灵敏度和准确性,能够有效地识别和定量多种PFAS,从而为蔬菜中PFAS的监测提供可靠的技术支持.
【Abstract】 Vegetable consumption is a well-established pathway for human exposure to per-and polyfluoroalkyl substances(PFAS). These contaminants are absorbed by vegetables through uptake from soil and irrigation water, leading to bioaccumulation within plant tissues and posing potential risks to human health. Therefore, the monitoring of PFAS concentrations in vegetables is critical for assessing dietary exposure and associated health risks. In this study, a solid-phase extraction(SPE)followed by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method was developed for the determination of 24 PFAS compounds in leafy vegetables, including Shanghai Bok Choy, Cabbage and Water Spinach. The analytical method, incorporating organic solvent extraction followed by SPE cleanup, was optimized with respect to both extraction solvent and SPE sorbent. In this method, alkaline methanol was used as the extraction solvent, and PFAS in vegetables were extracted via vortex-assisted extraction. Tandem mass spectrometry was used for the detection of the PFAS in multiple reaction monitoring mode, and the quantitative analysis was performed by internal standard method. Under the optimized analytical conditions, the recoveries and relative standard deviation(RSD) were in the range of 50.0% —120.8% and 1.0% —26%,respectively, when the spiked level was 2 ng. The linearity of each target PFAS was good in the corresponding mass concentration range with the correlation coefficients(r) greater than 0.99, and the limits of detection(LOD, S/N=3) ranged from 0.002 ng·g-1 to 0.103 ng·g-1, and the limits of quantification(LOQ, S/N=10) ranged from 0.007 ng·g-1 to 0.343 ng·g-1. The method was applied to the determination of PFAS in real samples, and 20 PFAS were detectable, among which 10 PFAS were detected with 100%, and the total concentration range of PFAS was 2.92 —6.83 ng·g-1 dw.PFBA was the main PFAS with the concentration range at 1.18 —3.74 ng·g-1 dw. The method demonstrated good sensitivity and accuracy, and was able to effectively quantify a variety of PFAS,thus providing a reliable technical support for the monitoring of PFAS in vegetables.
【Key words】 PFAS; solid phase extraction; ultra-high performance liquid chromatography-tandem mass spectrometry; vegetables;
- 【文献出处】 环境化学 ,Environmental Chemistry , 编辑部邮箱 ,2026年04期
- 【分类号】O657.63;TS255.7
- 【下载频次】25