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Determination of 51 per- and polyfluoroalkyl substances in raw water and drinking water by online solid-phase extraction coupled with ultra performance liquid chromatography- tandem mass spectrometry
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Yongyan CHEN, Jia LYU, Bixiong YE, Lan ZHANG*, Yuanyuan WANG, Ning JIN
Chinese Journal of Chromatography | 2025, 43(11) : 1222 - 1234
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Chinese Journal of Chromatography | 2025, 43(11): 1222-1234
• Articles •
Determination of 51 per- and polyfluoroalkyl substances in raw water and drinking water by online solid-phase extraction coupled with ultra performance liquid chromatography- tandem mass spectrometry
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Yongyan CHEN, Jia LYU, Bixiong YE, Lan ZHANG*, Yuanyuan WANG, Ning JIN
Affiliations
  • China CDC Key Laboratory of Environment and Population Health,National Institute of Environmental Health,Chinese Center for Disease Control and Prevention,Beijing 100050,China
Published: 2025-11-08 doi: 10.3724/SP.J.1123.2024.12020
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In this study, an online solid-phase extraction-ultra performance liquid chromatography-tandem mass spectrometry (online SPE-UPLC-MS/MS) method was established to rapidly screen and determine 51 per- and polyfluoroalkyl substances (PFASs) in raw and drinking water. Ammonium formate and 24 PFAS internal standards were added to each sample. The ammonium formate concentration in the sample was 2 mmol/L after mixing, and the contents of the PFAS internal standards ranged between 2.5 and 50 ng/L. Each sample was filtered through a 0.22-μm cellulose acetate filter, and a 5-mL aliquot was injected and adsorbed using an HLB online solid-phase extraction column and rinsed with 2 mmol/L ammonium formate. Acetonitrile and 2 mmol/L aqueous ammonium formate were used as mobile phases. Separation was performed on a BEH C18 chromatographic column with gradient elution. Electrospray ionization source negative ion mode and multiple reaction monitoring mode were used for detection, with quantification performed using the internal standard method. The method was validated by determining accuracies and precisions for the 51 PFASs using raw water and drinking water as matrices. Excellent linear relationships within their respective ranges were observed, with correlation coefficients (r2)>0.995. The method exhibited limits of detection (LODs, S/N=3) and quantification (LOQs, S/N=10) of 0.03–1.5 and 0.1–5.0 ng/L, respectively. The PFASs were spiked at levels of 1, 10 and 50 ng/L, with spiked recoveries of 60.2%–126.9% and 60.4%–122.6% obtained for raw- and drinking-water samples, respectively, along with corresponding relative standard deviations (RSDs, n=6) of 0.3%-17.9% and 0.4%-17.7%, respectively. The developed method was used to determine PFAS residues in raw and drinking water, with perfluoroalkyl carboxylic acids, perfluoroalkyl sulfonic acids, and perfluoroalkyl ether acids detected at relatively high rates with contents of 0.1–209.7 and 0.1–63.6 ng/L in raw water and drinking water, respectively. Compared to offline solid-phase extraction methods, the developed method requires fewer samples, is more convenient from a sample-collection perspective, and uses lower quantities of internal standards. It also analyzes rapidly and is highly sensitive and reproducible. Only 20 min was required to determine the 51 PFASs at the ng/L level, from online enrichment to detection. The developed method is suitable for the trace determination of various types of PFAS, such as perfluoroalkyl carboxylic acids, perfluoroalkyl sulfonic acids, perfluoroalkyl ether acids, fluorotelomers, and fluoroalkyl sulfonamides, in raw and drinking water, thereby effectively boosting the detection efficiency for perfluoroalkyl substances in water in a manner that has substantial practical applications value.

online solid-phase extraction (online SPE)  /  ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)  /  per- and polyfluoroalkyl substances (PFASs)  /  raw water  /  drinking water
陈永艳, 吕佳, 叶必雄, 张岚, 王园媛, 金宁. 在线固相萃取-超高效液相色谱-串联质谱法测定水源水和饮用水中51种全氟和多氟烷基物质. 色谱, 2025 , 43 (11) : 1222 -1234 . DOI: 10.3724/SP.J.1123.2024.12020
Yongyan CHEN, Jia LYU, Bixiong YE, Lan ZHANG, Yuanyuan WANG, Ning JIN. Determination of 51 per- and polyfluoroalkyl substances in raw water and drinking water by online solid-phase extraction coupled with ultra performance liquid chromatography- tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2025 , 43 (11) : 1222 -1234 . DOI: 10.3724/SP.J.1123.2024.12020
Year 2025 volume 43 Issue 11
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7
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doi: 10.3724/SP.J.1123.2024.12020
  • Receive Date:2024-12-20
  • Online Date:2026-10-30
  • Published:2025-11-08
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  • Received:2024-12-20
Affiliations
    China CDC Key Laboratory of Environment and Population Health,National Institute of Environmental Health,Chinese Center for Disease Control and Prevention,Beijing 100050,China
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表12种不同金属材料的力学参数
科
Family
属数
Number of
genus
种数
Number of
species
占总种数比例
Percentage of
total species (%)
属
Genus
种数
Number of
species
占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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