固相萃取GC-MS/MS法测定海水中多环芳烃研究

建立了同时测定海水中10种多环芳烃的精确定量检测方法. 利用固相萃取GC-MS/MS法, 确定10种多环芳烃的色谱分离条件和质谱定性、定量离子. 通过比对不同固相萃取柱和萃取条件对多环芳烃的萃取效果发现C18为最佳固相萃取柱, 最佳洗脱溶剂为二氯甲烷. 同时, GC-MS/MS采用多反应监测模式(MRM)及内标法定量, 该方法的线性范围为1.0~200.0μg?L-1, 检出限为0.01~0.08ng?L-1, 加标回收率为83.0%~108.7%, 相对标准差小于6.5%. 表明该方法具有较好的准确度和精密度, 最后将其应用于象山港海水中多环芳烃的测定, 10种多环芳烃的检出率为100%.

Simultaneous determination of polycyclic aromatic hydrocarbons in seawater by solid phase extraction coupled with gas chromatography tandem mass spectrometry (GC-MS/MS)

In the current study, a solid phase extraction coupled with GC-MS/MS method was established to investigate 10 kinds of polycyclic aromatic hydrocarbons in seawater. The chromatographic separation conditions and the qualitative and quantitative ions of PAHs were determined with experiments. The solid phase extraction columns and extraction solvents were also optimized. Finally, the PAHs in seawater samples were concentrated by C18 SPE cartridge and eluted by dichloromethane, qualified and quantified by multiple reaction monitoring mode (MRM) with GC-MS/MS, where the internal standard method was used. Using the proposed method, the limit of detection ranged from 0.01-0.08ng?L-1, the spiked recoveries were 83.0%-108.7%, and the relative standard deviation was less than 6.5%. The method has been successfully applied to analyze target PAHs in seawater samples collected from Xiangshan Harbor, with the detective rate being 100%.