口服液中全氟烷基类化合物的快速测定

肖锋, 卞学海, 沈金灿, 岳振峰, 陈沛金, 肖陈贵

肖锋, 卞学海, 沈金灿, 岳振峰, 陈沛金, 肖陈贵. 口服液中全氟烷基类化合物的快速测定[J]. 质谱学报, 2016, 37(6): 562-570. DOI: 10.7538/zpxb.youxian.2016.0039
引用本文: 肖锋, 卞学海, 沈金灿, 岳振峰, 陈沛金, 肖陈贵. 口服液中全氟烷基类化合物的快速测定[J]. 质谱学报, 2016, 37(6): 562-570. DOI: 10.7538/zpxb.youxian.2016.0039
XIAO Feng, BIAN Xue-hai, SHEN Jin-can, YUE Zhen-feng, CHEN Pei-jin, XIAO Chen-gui. Rapid Determination of Perfluoroalkylated Substances in Oral Liquid[J]. Journal of Chinese Mass Spectrometry Society, 2016, 37(6): 562-570. DOI: 10.7538/zpxb.youxian.2016.0039
Citation: XIAO Feng, BIAN Xue-hai, SHEN Jin-can, YUE Zhen-feng, CHEN Pei-jin, XIAO Chen-gui. Rapid Determination of Perfluoroalkylated Substances in Oral Liquid[J]. Journal of Chinese Mass Spectrometry Society, 2016, 37(6): 562-570. DOI: 10.7538/zpxb.youxian.2016.0039
肖锋, 卞学海, 沈金灿, 岳振峰, 陈沛金, 肖陈贵. 口服液中全氟烷基类化合物的快速测定[J]. 质谱学报, 2016, 37(6): 562-570. CSTR: 32365.14.zpxb.youxian.2016.0039
引用本文: 肖锋, 卞学海, 沈金灿, 岳振峰, 陈沛金, 肖陈贵. 口服液中全氟烷基类化合物的快速测定[J]. 质谱学报, 2016, 37(6): 562-570. CSTR: 32365.14.zpxb.youxian.2016.0039
XIAO Feng, BIAN Xue-hai, SHEN Jin-can, YUE Zhen-feng, CHEN Pei-jin, XIAO Chen-gui. Rapid Determination of Perfluoroalkylated Substances in Oral Liquid[J]. Journal of Chinese Mass Spectrometry Society, 2016, 37(6): 562-570. CSTR: 32365.14.zpxb.youxian.2016.0039
Citation: XIAO Feng, BIAN Xue-hai, SHEN Jin-can, YUE Zhen-feng, CHEN Pei-jin, XIAO Chen-gui. Rapid Determination of Perfluoroalkylated Substances in Oral Liquid[J]. Journal of Chinese Mass Spectrometry Society, 2016, 37(6): 562-570. CSTR: 32365.14.zpxb.youxian.2016.0039

口服液中全氟烷基类化合物的快速测定

Rapid Determination of Perfluoroalkylated Substances in Oral Liquid

  • 摘要: 建立了高效液相色谱-串联质谱法(HPLC-MS/MS)检测口服液中16种全氟烷基类化合物(PFASs)。样品采用2%盐酸酸化甲醇溶液提取,用NaOH溶液将提取液的pH值调至中性后,加入PSA和GCB粉末吸附剂分散固相萃取富集净化,用50 mmol/L三乙胺-甲醇溶液洗脱,HPLC-MS/MS负离子多反应监测模式测定,同位素内标法定量。结果表明:在0.2~20 μg/L浓度范围内,16种全氟烷基类化合物具有良好的线性关系,线性相关系数(r)大于0.996,方法的检出限均小于0.15 μg/L,定量限均小于0.43 μg/L;在0.5、1.0、2.0和5.0 μg/L添加水平下,化合物的平均回收率在80.8%~119%之间,相对标准偏差均小于10.5%。应用该方法对市场上随机采购的24种口服液样品进行检测,检出了14种PFASs化合物,其中以PFBA、PFOA、PFHxA、PFHpA、PFNA、PFDA最为普遍,最高浓度达5.05 μg/kg。该方法快速、简便、灵敏度高、重现性好,适用于口服液中PFASs的检测。
    Abstract: A method of high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was developed for the simultaneous determination of 16 perfluoroalkylated substances (PFASs) in oral liquid products. The residual of perfluoroalkylated substances in samples were extracted using methanol acidified with 2% hydrochloric acid solution as the extraction solvent, then enriched by N-propylethylenediamine (PSA) and PestiCarb (GCB) absorbent after adjusting extract's pH to neutral. Next, the compounds were eluted with 50 mmol/L triethylamine-methanol solution. At last, the exact was analyzed by HPLC-MS/MS in negative mode with multiple reaction monitoring (MRM). All the analyte were calibrated by the internal method. Good linearities were established for the 16 perfluoroalkylated substances in the range from 0.2 g/L to 20 g/L. For all of 16 perfluoroalkylated substances, the limit of detection is less than 0.15 g/L, while the limit of quantitation is less than 0.43 g/L. The average recoveries of 16 perfluoroalkylated substances are between 80.8% and 119% in the spiking levels of 0.5, 1.0, 2.0 and 5.0 g/L. The relative standard deviation (RSD) of 16 perfluoroalkylated substances is less than 10.5%. The method is simple, rapid and sensitive, which suits for determination of 16 perfluoroalkylated substances in oral liquid samples.
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  • 刊出日期:  2016-11-19

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