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50mmol/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0.2-20μg/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0.15μg/L,定量限均小于0.43μg/L;在0.5、1.0、2.0和5.0μg/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5.05μg/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。
A method of high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was developed for the simultaneous determination of 16 perflu-oroalkylated 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 sub s tance s, 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 perfluoroal-kylated substances is less than 10. 5 %. The method is simple, rapid and sensi tive, which suits for determination of 16 perfluoroalkylated substances in oral liquid samples.