基于高效液相色谱-电雾式检测器的全氟磺酸盐响应规律与校准方法研究  

Response and Calibration of Perfluoalkane Sulfonates by High Performance Liquid Chromatography-Charged Aerosol Detector

作　　者：陈日安 高燕 初红涛[1] 张庆合[2] CHEN Ri-an;GAO Yan;CHU Hong-tao;ZHANG Qing-he(College of Chemistry and Chemical Engineering,Qiqihar University,Qiqihar 161006,China;Division of Chemical Metrology and Analytical Science,National Institute of Metrology,Beijing 100029,China)

机构地区：[1]齐齐哈尔大学化学与化学工程学院,黑龙江齐齐哈尔161006 [2]中国计量科学研究院化学计量与分析科学研究所,北京100029

出　　处：《化学试剂》2023年第9期134-139,共6页Chemical Reagents

基　　金：多组分有机物混合溶液标准物质研制项目(ANL2006)。

摘　　要：基于高效液相色谱-电雾式检测器(HPLC-CAD),建立了全氟丁基磺酸盐(PFBS)、全氟己基磺酸盐(PFHxS)和全氟辛基磺酸盐(PFOS)3种全氟磺酸盐(PFSAs)的分析方法。PFBS、PFHxS和PFOS的方法检出限为1.0μg/g。3种化合物在5.0~2000.0μg/g范围内双对数线性拟合及在5.0~200.0μg/g范围内线性拟合,相关系数R 2>0.99。低于200.0μg/g浓度时采用线性拟合曲线、高浓度采用双对数拟合曲线进行分段校准时,计算值和配制值相对标准偏差(RSD)低于24.6%。采用化合物独立校准曲线对3种化合物的浓度进行校准,计算值与配制值RSD在0.3%~29.9%范围内,与3种PFSAs分别校准结果较为一致。采用建立的方法进行直链/支链混合PFOS标准品的分析,直链PFOS主成分的含量为77.8%。为CAD检测器在PFSAs含量分析及化合物独立校准研究中的应用提供支撑。A method for the analysis of three perfluorosulfonates(PFSAs)was developed by high performance liquid chromatography coupled with charged aerosol detector(HPLC-CAD).The limits of detection(LODs)of PFBS,PFHxS and PFOS were 1.0μg/g,respectively.The linearity of the double logarithmic fit was good with R 2>0.99 for 3 PFSAs in the range of 5.0~2000.0μg/g;The linearity was good with R 2>0.99 for 3 PFSAs in the range of 5.0~200.0μg/g.Linear fitting regression was adopted at concentrations lower than 200.0μg/g while double logarithmic fitting regression was adopted at higher concentrations,with relative standard deviations between calculated and prepared values lower than 24.6%.The concentrations of 3 PFSAs were calculated using compound-independent calibration,and the deviations between the calculated and prepared values were in the range of 0.3%~29.9%.The analysis of linear and branched PFOS(n-/br-PFOS)standard was performed using the developed method,and the results showed that the content of the n-PFOS was 77.8%.The investigation supports the application of CAD detectors in the analysis of PFSAs and compound independent calibration.

关 键 词：高效液相色谱-电雾式检测器 全氟磺酸盐 响应规律 拟合方程 化合物独立校准 异构体分析 

分 类 号：O65[理学—分析化学]