鸡肝中15种全氟烷基酸的液相色谱-串联质谱法分析
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。
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.
标题：鸡肝中15种全氟烷基酸的液相色谱-串联质谱法分析
英文标题：Determination of 15 perfluoroalkyl acids in chicken liver by liquid chromatography-tandem mass spectrometry
作者：
黎文茵 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;深圳大学化学与化工学院,
岳振峰 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
郑宗坤 深圳大学化学与化工学院
沈金灿 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
张毅 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
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,
发表日期：2013-11-05
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