Research Progress on Detection and Screening Techniques for Perfluoroalkyl and Polyfluoroalkyl Substances

LIU Xuesong; ZHANG Tao; TAO Yanqiu; LYU Yonggao

doi:10.15898/j.ykcs.202408120172

Rock and Mineral Analysis > 2025 > In Press, Accepted Manuscript > DOI: 10.15898/j.ykcs.202408120172

LIU Xuesong，ZHANG Tao，TAO Yanqiu，et al. Research Progress on Detection and Screening Techniques for Perfluoroalkyl and Polyfluoroalkyl Substances[J]. Rock and Mineral Analysis，2025，44（3）：1−16. DOI: 10.15898/j.ykcs.202408120172

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Research Progress on Detection and Screening Techniques for Perfluoroalkyl and Polyfluoroalkyl Substances

Center for Hydrogeology and Environmental Geology Survey, China Geology Survey, Tianjin 300304, China

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Received Date: August 11, 2024
Revised Date: October 16, 2024
Accepted Date: November 21, 2024
Available Online: December 20, 2024

Abstract

HIGHLIGHTS
(1) PFAS pre-processing technology is becoming increasingly mature, but there is still room for improvement in eliminating impurity interference and reducing analyte loss。

(2) The current detection standards can only accurately quantify dozens of known PFAS, and for a large number of unknown PFAS, it is difficult to be quantified accurately. It is necessary to increase research on detection technology and the development of standard reference materials.

(3) Non targeted screening is an important method for identifying unknown PFAS, and developing a comprehensive automated technology that can characterize known and unknown PFAS in tandem HRMS data is the future direction of non targeted screening development.

ABSTRACT

Perfluoroalkyl and polyfluoroalkyl substances (PFAS) are synthetic chemicals widely present in water and soil media with industrial and commercial applications. PFAS has attracted global attention due to its toxicity and bioaccumulation, and its precise identification and quantitative detection are of great significance for pollution prevention and control. This article reviews the latest research progress on pre-treatment methods, detection techniques, and screening methods for PFAS in different media. Analyzed the advantages, disadvantages, and development directions of mainstream extraction techniques and detection methods for PFAS. The system summarizes quantifiable detection standards and key indicator characteristics at home and abroad, explores the advantages, disadvantages, and applicable scenarios of targeted and non targeted screening methods, and focuses on analyzing the characteristics and development prospects of two non targeted screening technologies, high-resolution mass spectrometry (HRMS) and total PFAS analysis. It is recommended to develop a rapid screening tool for total organic fluorine, develop pre-treatment techniques suitable for different sample matrices, and enrich the PFAS database to provide reference for accurate identification and rapid quantification of PFAS in diverse environments in the future.
- PFAS,
- Detection standard,
- HPLC-MS/MS,
- HRMS,
- Non-targeted screening
BRIEF REPORT
Perfluoroalkyl and polyfluoroalkyl substances (PFAS) are synthetic chemicals with wide industrial and commercial applications. They enter environmental media such as water，soil，and gas through food packaging，textiles，cosmetics，and fire-fighting equipment containing PFAS，and are commonly present in surface water，groundwater，soil，and sediments. PFAS has strong chemical inertness and high temperature resistance. In addition，PFAS has also received global attention due to its toxicity and bioaccumulation. The above characteristics determine that once PFAS enters the environment，it is difficult to eliminate naturally and exists in soil，water bodies，and atmosphere for a long time，causing great harm to the ecological environment and posing a long-term threat to the ecosystem.
　　This article starts with the pre-treatment technology，detection technology，screening methods，and standards of PFAS from the perspectives of identification，quantification，and standardization. It tracks and understands the development level and research progress of PFAS detection and analysis technology at home and abroad，comprehensively analyzes and compares the advantages and disadvantages of sample pre-treatment technology，analysis and detection technology，and screening methods，provides method reference and technical reference for the accurate quantification and rapid identification of PFAS，and provides technical support and data basis for its pollution prevention and harmless treatment.
1. PFAS analysis sample pretreatment technology
The pre-treatment stage of PFAS samples mainly uses solvent extraction technology and solid-phase extraction technology. Solvent extraction techniques include Soxhlet extraction，pressurized liquid extraction (PLE)，liquid-liquid extraction (LLE)，dispersed liquid-liquid microextraction (DLLME)，and ion pair extraction (IPE). Solid phase extraction techniques mainly include SPE column extraction，solid-phase microextraction (SPME)，and dispersed solid-phase extraction (DSPE). Different extraction techniques have different principles，and their applicability and recovery rates also vary. By comprehensively utilizing different extraction techniques，FPAS substances can be extracted and separated from samples in different media such as water，soil，and gas，with recovery rates generally ranging from 80% to 145%. In addition to the traditional pretreatment techniques mentioned above，this article also introduces some other simple and effective pretreatment methods for enriching PFAS.
2. PFAS analysis sample analysis and detection technology
　　PFAS mainly uses separation and physical analysis methods，among which gas chromatography-mass spectrometry and liquid chromatography-mass spectrometry are the most commonly used techniques for separation and fractionation in PFAS analysis. Generally speaking，PFAS can be determined by GC-MS using electron ionization (EI)，negative ion chemical ionization (NICI)，or chemical ionization (CI) under selected ion monitoring modes. The determination of PFAS by gas chromatography-mass spectrometry has the characteristics of easy operation，high sensitivity，and good precision，which can meet the determination needs of perfluorinated compounds in various media. Liquid chromatography tandem mass spectrometry combines the advantages of chromatography and mass spectrometry，and can effectively perform qualitative and quantitative analysis on various substances with high boiling points and poor thermal stability. The main methods of liquid chromatography-mass spectrometry include liquid chromatography-mass spectrometry (LC-MS)，high-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS)，ultra-high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS)，etc. Among them，HPLC-MS/MS and UPLC-MS/MS have been extensively studied for the application of PFAS，with high sensitivity and a detection limit as low as 0.01ng/L. In addition to the traditional detection methods mentioned above，matrix assisted laser desorption/ionization imaging mass spectrometry (MALDI-IMS) is mainly used for in-situ detection and imaging of perfluorooctane sulfonic acid，without involving several complex preparation procedures or introducing contamination. Dielectric barrier discharge ionization mass spectrometry (DBDI-MS) is used to analyze PFOA in water samples without the need for sample preparation and chromatography.
3. PFAS screening method
　　PFAS belongs to a vast chemical category，comprising over 4700 different compounds with various chemical compositions，molecular weights，functional groups，and fluorine contents，but most quantitative studies only focus on a small subset of them. The PFAS testing standards released by European and American countries and organizations are targeted screening methods that have been validated by multiple laboratories to accurately quantify some PFAS. Targeted screening methods mainly focus on a few PFAS such as PFOA and PFOS (usually with far less than 50 analytes). For unknown PFAS with uncertain standard curves，non targeted screening methods are more important. Currently，non targeted screening methods mainly include PFAS total analysis and high-resolution mass spectrometry chromatography. The PFAS total amount analysis method uses combustion ion chromatography (CIC) and total oxidizable precursor (TOP) determination to quantitatively analyze the total amount of PFAS in the sample，in order to determine the degree of contamination of the sample and its impact on the environment and human health; High resolution mass spectrometry chromatography is mainly used for screening and identifying suspicious or unknown organic fluorine compounds to guide the development of new detection technology standards for quantitative detection of unknown PFAS.
4. Conclusion and Prospect
　　The advancement of pre-treatment methods and detection technologies for PFAS，especially the development and comprehensive application of non targeted screening techniques，suspected screening techniques，and high-resolution mass spectrometry detection techniques，has promoted the quantification and identification of more peak values in PFAS spectra. The detection range of PFAS types is becoming wider and wider，providing data basis and technical support for more PFAS to enter the list of quantitative detection standards. While PFAS detection technology has made progress，it still faces the following challenges: (1) There are many types of PFAS with similar structures but significant differences in physical and chemical properties，which increases the difficulty of accurate identification and quantitative detection. (2) PFAS is at a trace level in the medium，and improving pre-treatment and analytical detection techniques to identify and quantify lower levels of PFAS will be the key to future technological advancements. (3) Lack of PFAS detection methods and equipment that can be used for rapid on-site identification.

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