鸡肝中15种全氟烷基酸的液相色谱-串联质谱法分析

Determination of 15 perfluoroalkyl acids in chicken liver by liquid chromatography-tandem mass spectrometry

中文关键词:  全氟烷基酸  液相色谱-串联质谱法  碱消解  鸡肝

英文关键词:perfluoroalkyl acids  liquid chromatography-tandem mass spectrometry  modified NaOH digestion  chicken liver

中文摘要:

      目的 建立液相色谱-串联质谱法检测鸡肝中15 种全氟烷基酸(perfluoroalkyl acids, PFAs)的分析方法。方法 采用C18型色谱柱分离, 液相色谱串联质谱仪(liquid chromatography-tandem mass spectrometry, LC-MS/MS)在负离子模式下检测, 前处理以碱消解结合固相萃取净化, 考察不同碱液浓度、温度和时间条件下15 种PFAs的加标回收率。结果 15 种PFAs在0.5~20.0 μg/L浓度范围内线性良好, 相关系数r＞0.997, 检出限(limit of detection, LOD)为0.004~0.064 μg/kg, 定量限(limit of quantification, LOQ)为0.014~0.213 μg/kg。除两种长碳链的PFAs外, 其余13 种PFAs的加标回收率为80%~120%, 相对标准偏差(relative standard deviation, RSD)范围为0.93%~14.5%。结论 本方法灵敏度高、重现性好, 适用于鸡肝中15种PFAs的定量检测。

英文摘要:

      Objective To establish a method for the determination of 15 perfluoroalkyl acids (PFAs) in chicken liver by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods PFAs were separated on C18 column and detected by LC-ESI-MS/MS under multiple reaction monitoring (MRM) via negative-ion mode. PFAs in chicken liver were extracted with a modified NaOH digestion WAX method, investigated recoveries of 15 PFAs in LC-ESI-MS/MS determinations with different concentrations of NaOH/methanol, different temperatures and different time. Results This method showed a good linearity over the range from 0.5 μg/L to 20 μg/L for 15 PFAs with correlation coefficient r>0.997. The limit of detection was 0.0040.064 μg/kg. The limit of quantification was 0.0140.213 μg/kg. In addition to two kinds of long carbon chain PFAs, the recoveries of other 13 PFAs were found to be in the range from 80% to 120% with relative standard deviation of 0.93.5%. Conclusion This method shows highly sensitive and reproducible, and it is suitable for the detection of 15 PFAs in chicken liver.