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

作　　者：黎文茵 岳振峰[1] 郑宗坤[2] 沈金灿[1] 张毅[1] 

机构地区：[1]深圳出入境检验检疫局食品检验检疫技术中心,深圳市食品安全检测技术研发重点实验室,深圳518045 [2]深圳大学化学与化工学院,深圳518060

出　　处：《食品安全质量检测学报》2014年第1期210-218,共9页Journal of Food Safety and Quality

基　　金：国家科技基础性工作专项重点项目(2013FY113100);科技部十二五科技支撑计划项目(2012BAD33B02)~~

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0.5~20.0μg/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 (LC-MS/MS). Methods PFAs were sepa-rated on C18 column and detected by LC-ESI-MS/MS under multiple reaction monitoring (MRM) via nega-tive-ion mode. PFAs in chicken liver were extracted with a modified NaOH digestion WAX method, investi-gated 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 0.5μg/L to 20μg/L for 15 PFAs with correlation coefficient r>0.997. The limit of detection was 0.004～0.064μg/kg. The limit of quantification was 0.014～0.213μg/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%～14.5%. Conclusion This method shows highly sensitive and reproducible, and it is suitable for the detection of 15 PFAs in chicken liver.

关 键 词：全氟烷基酸 液相色谱-串联质谱法 碱消解 鸡肝 

分 类 号：O657.63[理学—分析化学] TS251.7[理学—化学]