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    谢琳娜, 胡小键, 张海婧, 张续, 杨艳伟, 王梦梦, 石国华, 朱英. SPE-UPLC-MS/MS法检测人尿液中全氟化合物的空白值研究[J]. 环境卫生学杂志, 2020, 10(6): 584-589. DOI: 10.13421/j.cnki.hjwsxzz.2020.06.013
    引用本文: 谢琳娜, 胡小键, 张海婧, 张续, 杨艳伟, 王梦梦, 石国华, 朱英. SPE-UPLC-MS/MS法检测人尿液中全氟化合物的空白值研究[J]. 环境卫生学杂志, 2020, 10(6): 584-589. DOI: 10.13421/j.cnki.hjwsxzz.2020.06.013
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    XIE Linna, HU Xiaojian, ZHANG Haijing, ZHANG Xu, YANG Yanwei, WANG Mengmeng, SHI Guohua, ZHU Ying. Blank Value in the Determination of Per- and Polyfluoroalkyl Substances in Human Urine by SPE-UPLC-MS/MS[J]. Journal of Environmental Hygiene, 2020, 10(6): 584-589. DOI: 10.13421/j.cnki.hjwsxzz.2020.06.013
    Citation: XIE Linna, HU Xiaojian, ZHANG Haijing, ZHANG Xu, YANG Yanwei, WANG Mengmeng, SHI Guohua, ZHU Ying. Blank Value in the Determination of Per- and Polyfluoroalkyl Substances in Human Urine by SPE-UPLC-MS/MS[J]. Journal of Environmental Hygiene, 2020, 10(6): 584-589. DOI: 10.13421/j.cnki.hjwsxzz.2020.06.013
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    SPE-UPLC-MS/MS法检测人尿液中全氟化合物的空白值研究

    Blank Value in the Determination of Per- and Polyfluoroalkyl Substances in Human Urine by SPE-UPLC-MS/MS

      摘要
    • 摘要:
      目的 分析人体尿液中全或多氟化合物（PFASs）固相萃取-超高效液相色谱-串联质谱（SPE-UPLC-MS/MS）方法空白值偏高的影响因素，并提出处理措施。
      方法 样品首先进行固相萃取，洗脱液经氮气吹干后，用甲醇复溶，最后用UPLC-MS/MS进行分析检测。进一步对实验仪器（UPLC-MS/MS）、实验试剂、实验耗材、前处理步骤、实验环境等因素中18种PFASs的空白值进行分析和探讨。
      结果 在18种PFASs目标分析物中，4种全氟羧酸（PFCAs，C4-C7）和全氟辛烷磺酸（PFOS）存在空白问题。其中，全氟丁酸（PFBA）、全氟戊酸（PFPeA）、全氟己酸（PFHxA）的空白值较高，均超过0.500 ng/mL，PFBA空白值最高可达到40.0 ng/mL。氨水中有少量PFBA检出，但是其对空白值的影响可以忽略不计；人工尿液中有PFPeA检出，实验中应对此加以关注；甲酸在空白问题中起到关键作用，通过更换甲酸品牌和规格可以达到解决空白问题的目的。
      结论 UPLC-MS/MS、实验耗材、实验环境均不是影响PFASs空白值的因素，实验试剂是以上5种PFASs空白值检出的主要原因。该研究对于尿液中PFASs的分析测定具有重要参考价值。

       

      Abstract:
      Objective To investigate the influencing factors for the high blank value in the determination of per- and polyfluoroalkyl substances (PFASs) in human urine by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS), and to propose treatment measures.
      Methods The samples were firstly extracted and eluted by solid phase extraction (SPE), then dried by nitrogen and redissolved in methanol, and finally analyzed by UPLC-MS/MS. The blank values of 18 PFASs were analyzed in terms of the factors of experimental instruments (UPLC-MS/MS), experimental reagent, experimental consumables, pretreatment procedures, and experimental environment.
      Results Among the 18 target analytes, four perfluorinated carboxylic acids (PFCAs, C4-C7) and perfluorooctane sulfonate acid (PFOS) were found to have blank values, among which perfluorobutanoic acid (PFBA), perfluoropentanoic acid (PFPeA), and perfluorohexanoic acid (PFHxA) had relatively high blank values (> 0.500 ng/mL), and the blank value of PFBA was up to 40.0 ng/mL. A relatively low concentration of PFBA was detected in ammonia, and its influence on the blank value could be ignored; PFPeA was detected in artificial urine, which should be taken seriously in the experiment; formic acid played a key role in the issue of blank value, which was solved by changing the brand and specification of formic acid.
      Conclusion UPLC-MS/MS, experimental consumables, and experimental environment are not the influencing factors for the blank values of PFASs, and experimental reagent is the main cause of the detection of blank values of the above five PFASs. Therefore, this study provides an important reference for the determination of PFASs in human urine.

       

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