【摘要】 建立了近岸及河口海水中全氟辛基磺酸(PFOS)、全氟辛酸(PFOA)、全氟十一酸(PFUn A)、全氟十二酸(PFDo A)、全氟十三酸(PFTr DA)、全氟十四酸(PFTA)6种全氟化合物(PFCs)的超高效液相色谱-串联质谱(UHPLC-MS/MS)测定方法。使用C18固相萃取小柱对500 m L水样中的目标物进行富集后,用15 m L甲醇-乙酸乙酯混合淋洗液(4∶1)进行洗脱,浓缩,定容至1.0 m L后,用Kinetex XB-C18色谱柱以均含5.0mmol/L甲酸铵的甲醇-水为流动相梯度洗脱方式进行分离,电喷雾负离子模式(ESI-)电离,多重反应监测模式(MRM)以及内标法对6种PFCs进行定性定量测定。优化了固相萃取、色谱分离及质谱测定条件,考察了海水盐度对方法回收率的影响。在优化实验条件下,方法在2.0,5.0,10.0 ng/L加标水平下,实际海水样品的回收率为80.1%~117.4%,在2.0 ng/L加标水平的相对标准偏差(RSD,n=7)为8.2%~12.1%。6种PFCs的线性范围为0.5~50.0μg/L,相关系数大于0.999 0;方法的定量下限(LOQ,S/N=10)为0.5~1.5 ng/L。该方法具有样品前处理简单、分析速度快、选择性好的特点,适用于近岸及河口海水中全氟化合物的快速测定。更多还原

【Abstract】 A rapid method was developed for the quantitative analysis of perfluorinated compounds( PFCs) including perfluorooctane sulfonic acid( PFOS),perfluorooctanoic acid( PFOA),perfluoroundecanoic acid( PFUn A),perfluorododecanoic acid( PFDo A),perfluorotridecanoic acid( PFTr DA),perfluorotetradecanoic acid( PFTA) in coastal and estuarine seawater by solid phase extraction( SPE)enrichment with ultra high performance liquid chromatography tandem electrospray ionization mass spectrometry( UHPLC- MS / MS). Seawater sample was enriched and purified through a 500 mg C18 SPE cartridge at 5. 0 m L / min,eluted with 15 m L mixed solvent of methanol and ethyl acetate( 4 ∶ 1),and finally concentrated into 1. 0 m L with an automated de-solvent device. Target analytes were separated on a Kinetex XB- C18 column using methanol( containing 5. 0 mmol / L NH4COOH- water( containing5. 0 mmol / L NH4COOH) as mobile phase. The negative electrospray ionization( ESI-) and multiple reaction monitoring mode( MRM) were utilized. An internal standard calibration method was chosen for the quantitative analysis. The calibration curves of PFCs were linear in the range of 0. 5- 50. 0μg /L with correlation coefficients more than 0. 999 0. The limits of quantitation( LOQs,S /N = 10)were between 0. 5 ng / L and 1. 5 ng / L. The recoveries of 6 PFCs at three spiked levels( 2. 0,5. 0,10. 0 ng / L) were in the range of 80. 1%- 117. 4%,and relative standard deviations( RSDs) were8. 2%- 12. 1% at spiked level of 2. 0 ng / L.更多还原