口服液中全氟烷基类化合物的快速测定

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。

Rapid Determination of Perfluoroalkylated Substances in Oral Liquid

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.