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1.深圳市疾病预防控制中心,广东 深圳 518055
2.SCIEX(中国)有限公司,广东 广州 510623
张建清,博士,主任医师,研究方向:新污染物与人群健康效应研究,E-mail:969676617@qq.com
收稿日期:2025-03-31,
修回日期:2025-05-09,
录用日期:2025-05-22,
纸质出版日期:2025-08-15
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刘源,卓兰,伍倩仪,宋嘉宜,蒋友胜,彭金铃,林晓仕,孙雯雯,张建清.超高效液相色谱-串联质谱法测定人体血清中52种全氟及多氟烷基化合物[J].分析测试学报,2025,44(08):1631-1640.
LIU Yuan,ZHUO Lan,WU Qian-yi,SONG Jia-yi,JIANG You-sheng,PENG Jin-ling,LIN Xiao-shi,SUN Wen-wen,ZHANG Jian-qing.Determination of 52 Perfluorinated and Polyfluorinated Substances in Human Serum by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2025,44(08):1631-1640.
刘源,卓兰,伍倩仪,宋嘉宜,蒋友胜,彭金铃,林晓仕,孙雯雯,张建清.超高效液相色谱-串联质谱法测定人体血清中52种全氟及多氟烷基化合物[J].分析测试学报,2025,44(08):1631-1640. DOI: 10.12452/j.fxcsxb.250331250.
LIU Yuan,ZHUO Lan,WU Qian-yi,SONG Jia-yi,JIANG You-sheng,PENG Jin-ling,LIN Xiao-shi,SUN Wen-wen,ZHANG Jian-qing.Determination of 52 Perfluorinated and Polyfluorinated Substances in Human Serum by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2025,44(08):1631-1640. DOI: 10.12452/j.fxcsxb.250331250.
建立了超高效液相色谱‒串联质谱(UHPLC‒MS/MS)测定人体血清中52种全氟及多氟烷基化合物(PFASs)的方法。200 μL血清样本经3 mL 0.6%甲酸‒乙酸乙酯和正己烷混合溶液(体积比3∶2)进行3次液液萃取后,采用UHPLC‒MS/MS检测分析。52种PFASs在线性范围内线性良好,相关系数(
r
2
)为0.995 5~0.999 8,方法检出限(LOD)为0.000 9~0.015 0 μg/L,定量下限(LOQ)为0.002 9~0.050 0 μg/L,加标回收率为75.1%~115%,平均加标回收率为78.9%~107%,相对标准偏差(RSD)为1.6%~15%,基质效应为85.0%~115%。使用该方法对180份人体血清进行检测,共检出48种化合物,其中PFHpA、PFOA、PFNA、PFDA、PFUdA、PFDoA、PFTrDA、PFTeDA、PFHxS、PFHpS、PFOS和6∶2 Cl-PFAES等12个单体化合物的检出率为100%。该方法操作简便,检出限低、精密度好、准确度高且重复性好,符合血清中PFASs检测分析的要求。
A method for the determination of 52 perfluorinated and polyfluorinated substances(PFASs) in human serum based on ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS) was developed. 200 μL human serum sample was subjected to liquid-liquid extraction three times using 3 mL of the mixed solution of 0.6% formic acid-ethyl acetate and
n
-hexane(3∶2,volume ratio),then analyzed by UHPLC-MS/MS. 52 PFASs exhibited good linearity in the range,with correlation coefficients(
r
²) ranging from 0.995 5 to 0.999 8. The limits of detection(LOD) were in the range of 0.000 9-0.015 0 μg/L,and the limit of quantitation (LOQ) were 0.002 9-0.050 0 μg/L. The spiked recoveries ranged from 75.1% to 115% with average recoveries of 78.9%-107%,the relative standard deviations(RSDs) were in the range of 1.6%-15%,and the matrix effects ranged from 85.0% to 115%. The method was used for the analysis of 180 human serum samples,and 48 PFASs were detected. Among them,the detection frequency of 12 compounds,including PFHpA,PFOA,PFNA,PFDA,PFUdA,PFDoA,PFTrDA,PFTeDA,PFHxS,PFHpS,PFOS,and 6∶2 Cl-PFAES,showed 100%. This method is simple,sensitive,accurate,and reproducible,could meet
the requirements for PFAS analysis in serum.
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