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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0.5~20.0μg/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0.004~0.064μg/kg,定量限(limit of quantification,LOQ)为0.014~0.213μg/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。
Objective To establish a method for the determination of 15 perfluoroalkyl acids (PFAs) in chicken liver by liquid chromatography-tandem mass spectrometry. Methods The compounds were separated on a C18 column and analyzed by liquid chromatography-tandem mass spectrometry (LC-MS / MS) in negative ion mode. The pretreatment was cleaned up by alkaline digestion and solid-phase extraction. , Spiked recoveries of 15 PFAs at temperature and time. Results The linearity of 15 PFAs in the range of 0.5-20.0 μg / L was good with a correlation coefficient of 0.997. The limit of detection (LOD) ranged from 0.004 to 0.064 μg / kg. The limit of quantification (LOQ) 0.014 ~ 0.213μg / kg. Except PFAs containing two kinds of long carbon chains, the spiked recoveries of the remaining 13 PFAs ranged from 80% to 120% with a relative standard deviation (RSD) ranging from 0.93% to 14.5%. Conclusion The method has high sensitivity and reproducibility and is suitable for quantitative determination of 15 kinds of PFAs in chicken liver.