Determination of perfluorooctane sulfonic acid in water by high performance liquid chromatography-tandem mass spectrometry
-
摘要: 建立了水中全氟辛烷磺酸（perfluoro-rooctane sulfonate，PFOS）的高效液相色谱-串联质谱法分析方法。用0.22 μm PP滤膜过滤水样，Poly-Sery HLB固相萃取柱对200 mL水样进行富集处理，以质量分数为10%的甲醇水溶液淋洗HLB柱以去除表面杂质，随后抽真空，再用4 mL纯甲醇溶液洗脱HLB柱。取洗脱液上机检测，以质量分数为0.1%的甲酸为流动相A，甲醇为流动相B，采用ACQΜITY ΜPLC BEH C18色谱柱对洗脱液进行分离，负离子多反应监测模式检测，碎片离子m/z=80，内标法定量分析。在优化条件下，PFOS在0.01～50 μg/L范围内线性较好，相关系数r>0.99，方法检出限为0.25 μg/L。方法加标回收实验添加浓度0.2、2.0和20 μg/L，PFOS加标回收率为82.1%~104.5%，相对标准偏差（RSD）为2.34%~5.64%。采集湖泊及养殖虾塘进出口水样进行测定，其PFOS含量均低于检出限，其中，湖水加标回收率为84.75%~112.2%，RSD<5.62%，养殖塘水样加标回收率为81.7%~118.6%，RSD<7.51%，实验所建方法可方便准确地检测水中PFOS含量。
-
关键词:
- 全氟辛烷磺酸 /
- 液相色谱-串联四极杆质谱 /
- 前处理方法优化 /
- 仪器检测条件优化
Abstract: A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS)method or perfluorooctane sulfonic acid (PFOS) analysis in water was established. The water sample was pretreated with a 0.22 μm PP filter membrane, and then 200 mL pretreated water was enriched with a Poly-Sery HLB solid phase extraction column. The enriched extraction column was eluted by passing it through 10% aqueous methanol, after which the elution chamber was evacuated and the column was washed again with 4 mL methanol. And then ACQ MITY MPLC BEH C18 chromatographic column was used to separate the eluent in the negative ion multi-reaction monitoring mode detection, fragment ion m/z=80, by internal standard method quantitative analysis, using a 0.1% formic acid aqueous solution-methanol solution as mobile phase. Under preferred conditions, PFOS was linear in the concentration range 0.01-50 μg/L with a correlation coefficient r>0.99, and the method limit of detection was 0.25 μg/L. The spiked recoveries ranged from 82.1% to 104.5% and the relative standard deviations (RSD) ranged from 2.34% to 5.64% for PFOS at the spiked concentrations of 0.2, 2.0, and 20 μg/L, respectively. The PFOS content in the actual water samples was below the detection limit, the lake water spiked recovery rate was between 84.75%-112.2%, RSD<5.62%, and the aquaculture water sample spiked recovery rate was between 81.7%-118.6%, RSD<7.51%. The established method can accurately detect PFOS in environmental water. -
-
SONG Y M,ZHOU L N,HAO W L,et al. Pollution status of perfluorinated compounds and research progress at home and abroad[J]. Environmental Engineering,2017,35(10):82-86.
HUANG J,SUN L,MENNIGEN J A,et al. Developmental toxicity of the novel PFOS alternative OBS in developing zebrafish:An emphasis on cilia disruption[J]. J Hazard Mater,2021. DOI:10.1016/j.jhazmat.2020.124491
WANG H,DU H,YANG J,et al. PFOS,PFOA,estrogen homeostasis,and birth size in Chinese infants[J]. Chemosphere,2019,221:349-355.
CAO W,LIU X,LIU X,et al. Perfluoroalkyl substances in umbilical cord serum and gestational and postnatal growth in a Chinese birth cohort[J]. Environment International,2018,116:197-205.
ALVES R N,MAULVAULT A L,BARBOSA V L,et al. Preliminary assessment on the bioaccessibility of contaminants of emerging concern in raw and cooked seafood[J]. Food and Chemical Toxicology,2017,104:69-78.
JEONG Y J,BANG S,KIM J,et al. Comparing levels of perfluorinated compounds in processed marine products[J]. Food and Chemical Toxicology,2019,126:199-210.
QI X,ZHOU J,WANG M,et al. Perfluorinated compounds in poultry products from the Yangtze River Delta and Pearl River Delta regions in China[J]. Science of The Total Environment,2019,689:1079-1086.
ZHANG M,LI J,ZHANG C,et al. In-situ synthesis of fluorinated magnetic covalent organic frameworks for fluorinated magnetic solid-phase extraction of ultratrace perfluorinated compounds from milk[J]. Journal of Chromatography A,2020.DOI:10.1016/j.chroma.2019.460773.
KARRMAN A,DOMINGO J L,LLEBARIA X,et al. Biomonitoring perfluorinated compounds in Catalonia,Spain:concentrations and trends in human liver and milk samples[J]. Environmental Science and Pollution Research,2010,17(3):750-758.
LI P,OYANG X,ZHAO Y,et al. Occurrence of perfluorinated compounds in agricultural environment,vegetables,and fruits in regions influenced by a fluorine-chemical industrial park in China[J]. Chemosphere,2019,225:659-667.
LIANG M,XIAN Y,WANG B,et al. High throughput analysis of 21 perfluorinated compounds in drinking water,tap water,river water and plant effluent from southern China by supramolecular solvents-based microextraction coupled with HPLC-Orbitrap HRMS[J]. Environmental Pollution,2020.DOI:10.1016/j.envpol.2020.114389.
XIE H,WEI Y,LI J,et al. In-situ exfoliation of graphitic carbon nitride with metal-organic framework via a sonication-assisted approach for dispersive solid-phase extraction of perfluorinated compounds in drinking water samples[J]. Journal of Chromatography A,2020.DOI:10.1016/j.chroma.2020.461337.
TSUDA T,INOUE A,IGAWA T,et al. Seasonal changes of PFOS and PFOA concentrations in Lake Biwa water[J]. Bulletin of Environmental Contamination and Toxicology,2010,85(6):593-597.
WU J,JUNAID M,WANG Z,et al. Spatiotemporal distribution,sources and ecological risks of perfluorinated compounds (PFCs) in the Guanlan River from the rapidly urbanizing areas of Shenzhen,China[J]. Chemosphere,2020. DOI:10.1016/j.chemosphere.2019.125637.
ZHENG Y L,GUO H,SHAO P W,et al. Distribution characteristics of perfluorinated compounds in the water environment of the eastern transition zone of the Qinghai-Tibet Plateau[J].Environmental Chemistry,2020,39(5):1192-1201.
SUN J S,WANG S L,Pollution characteristics of perfluorooctane carboxylic acid (PFOA) and perfluorooctane sulfonic acid (PFOS) in water bodies and sediments of typical wetlands in Shandong Province[J]. Environmental Chemistry,2019,38(07):1528-1538.
HE X,LI A,WANG S,et al. Perfluorinated substance assessment in sediments of a large-scale reservoir in Danjiangkou,China[J]. Environmental Monitoring and Assessment,2018,190(2):66.
CAI M,ZHAO Z,YANG H,et al. Spatial distribution of per- and polyfluoroalkyl compounds in coastal waters from the East to South China Sea[J]. Environmental Pollution,2012,161:162-169.
SHAFIQUE U,SCHULZE S,SLAWIK C,et al. Gas chromatographic determination of perfluorocarboxylic acids in aqueous samples-A tutorial review[J]. Analytica Chimica Acta,2017,949:8-22.
WU M,SUN R,WANG M,et al. Analysis of perfluorinated compounds in human serum from the general population in Shanghai by liquid chromatography-tandem mass spectrometry (LC-MS/MS)[J]. Chemosphere,2017,168:100-105.
ZHU P,LING X,LIU W,et al. Simple and fast determination of perfluorinated compounds in Taihu Lake by SPE-UHPLC-MS/MS[J]. Journal of Chromatography B,2016,1031:61-67.
HE S S,SHI Y L,CAI Y Q,et al. Research progress of analysis methods for perfluorinated/polyfluorinated compounds[J].Chromatography,2020,38(3):287-296.
HE J C,ZHANG S Y,SU Y Y,et al. Research progress in sample pretreatment and analysis methods of typical perfluorinated organic acids[J].Chromatography,2020,38(1):86-94.
WU J G,LONG Q,XIAO W,et al. Research progress in analytical methods of perfluorosulfonic acid and perfluorocarboxylic acid compounds in environmental water samples[J]. Environmental Chemistry,2018,37(8):1851-1859.
SPELTINI A,MAIOCCHI M,CUCCA L,et al. Solid-phase extraction of PFOA and PFOS from surface waters on functionalized multiwalled carbon nanotubes followed by UPLC-ESI-MS[J]. Analytical and Bioanalytical Chemistry,2014,406(15):3657-3665.
YANG W L,GUO J,DU W,et al. Determination of Perfluorooctanoic Acid and Perfluorooctane Sulfonic Acid in Environmental Water and Soil by Ultra Performance Liquid Chromatography-New Tandem Quadrupole Mass Spectrometry[J]. Environmental Chemistry,2018,37(12):2820-2823.
HUANG D R,WEN Y Y,CHEN Z H,et al. Solid-phase extraction enrichment/ultra high performance liquid chromatography-tandem mass spectrometry determination of perfluorinated compounds in coastal and estuary seawater[J]. Journal of Analysis and Testing,2016,35(3):305-310.
LACINA O,HRADKOVA P,PULKRABOVA J,et al. Simple,high throughput ultra-high performance liquid chromatography/tandem mass spectrometry trace analysis of perfluorinated alkylated substances in food of animal origin:milk and fish[J]. Journal of Chromatography A,2011,1218(28):4312-4321.
CHEN C,LIANG X,WANG J, et al. Development of a polymeric ionic liquid coating for direct-immersion solid-phase microextraction using polyhedral oligomeric silsesquioxane as cross-linker[J]. J Chromatogr A,2014,1348:80-86.
APARICIO I,MARTIN J,SANTOS J L,et al. Stir bar sorptive extraction and liquid chromatography-tandem mass spectrometry determination of polar and non-polar emerging and priority pollutants in environmental waters[J]. J Chromatogr A,2017,1500:43-52.
DONG W H,YANG H,LINGHU W S. Analysis of Influencing Factors in the Determination of Perfluorooctanoic Acid and Perfluorooctane Sulfonic Acid in Water by Tandem Liquid Mass Spectrometry[J]. Chemical World,2017,58(1):1-6.
(6):88-92.
WANG X F,WANG Q,LI Z G,et al. Determination of 23 perfluorinated alkylated substances in water and suspended particles by ultra-performance liquid chromatography/tandem mass spectrometry[J]. Journal of Environmental Science and Health Part A,2018,53(14):1277-1283.
PAPADOPOULOU A,ROMAN I P,CANALS A,et al. Fast screening of perfluorooctane sulfonate in water using vortex-assisted liquid-liquid microextraction coupled to liquid chromatography-mass spectrometry[J]. Anal Chim Acta,2011,691(1/2):56-61.
WILLE K,VANDEN B J,NOPPE H,et al. A validated analytical method for the determination of perfluorinated compounds in surface-sea- and sewagewater using liquid chromatography coupled to time-of-flight mass spectrometry[J]. Journal of Chromatography A,2010,1217(43):6616-6622.
计量
- 文章访问数: 712
- PDF下载数: 69
- 施引文献: 0
下载:
