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

doi:10.7538/zpxb.youxian.2016.0039

口服液中全氟烷基类化合物的快速测定

肖锋^1,2,
卞学海^1,2,
沈金灿^1,2,
岳振峰^1,2,
陈沛金^1,2,
肖陈贵^1,2

1.
深圳出入境检验检疫局食品检验检疫技术中心,广东深圳518045
2.
深圳市检验检疫科学研究院,广东深圳518010

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- 刊出日期: 2016-11-19

Rapid Determination of Perfluoroalkylated Substances in Oral Liquid

1.
Food Inspection & Quarantine Center, Shenzhen Entry-Exit Inspection and Quarantine Bureau, Shenzhen 518045, China
2.
Shenzhen Academy of Inspection and Quarantine, Shenzhen 518010, China

摘要

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。
- 高效液相色谱-串联质谱（HPLC-MS/MS） /
- 全氟烷基类化合物（PFASs） /
- 口服液 /
- 基质分散固相萃取
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.
- perfluoroalkylated substances （PFASs） /
- oral liquid /
- matrix dispersive solid phase extraction /
- HPLC-MS/MS

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参考文献(19)

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口服液中全氟烷基类化合物的快速测定

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Rapid Determination of Perfluoroalkylated Substances in Oral Liquid

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