摘要
建立鱼肉中8种全氟化合物的同位素稀释-超高效液相色谱-串联质谱快速分析方法.鱼肉加入同位素内标后使用乙腈超声萃取,经WAX固相萃取小柱净化后,采用C1s反相色谱柱进行分离,用配有电喷雾离子源的三重四极杆质谱进行多反应离子监测,同位素稀释内标法定量.8种全氟化合物在0.1~50.0 μg/L范围内线性关系良好,相关系数不低于0.998,方法检出限在0.03~0.15 μg/kg之间,平均加标回收率为87.7%~104.4%,相对标准偏差为4.1%~10.7%.该法灵敏度高、快速准确,适用鱼肉中全氟化合物的定性和定量检测.
A method for the rapid determination of eight perfluorinated compounds (PFCs) in fish muscles was developed by isotope dilution ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS).Samples were extracted with acetonitrile after addition of eight isotopically labeled internal standards.The extracts were cleaned up on a WAX solid phase extraction column.The target compounds were separated on a ZORBAX Eclipse plus C18 (100 mm ×3.0 mm,3.5 μm) and analyzed by a triple quadruple tandem mass spectrometer with electrospray ionization source (EIS) in multiple reaction monitoring (MRM) mode.The analytes were quantified by the internal standards labeled with stable isotopes.The standard curves were linear in the ranges of 0.1-50.0 μg/L for 8 PFCs with correlation coefficients greater than 0.998.The limits of detection were 0.03-0.15 μg/kg.The average recoveries of PFCs in fish muscles were in the range of 87.7%-104.4%.The relative standard deviations (RSD) for PFCs were in the range of 4.1%-10.7%.These results show that the method is sensitive and accurate,and suitable for the qualitative and quantitative determination of PFCs residues in fish muscle samples.
出处
《食品科学》
EI
CAS
CSCD
北大核心
2014年第8期193-197,共5页
Food Science
基金
中挪合作持久性有机污染物地方履约能力建设项目二期(C/V/S/12/067)
关键词
同位素稀释
超高效液相色谱-串联质谱法
鱼肉
全氟化合物
isotope dilution
ultra-performance liquid chromatography-tandem mass spectrometry
fish muscles
perfluorinated compounds