高效液相色谱-荧光/紫外串联测定 海洋沉积物中16种多环芳烃

Determination of sixteen polycyclic aromatic hydrocarbons in marine sediments by high performance liquid chromatography with fluorescence and ultraviolet detection

中文关键词: 高效液相色谱  荧光-紫外检测器联用  海洋沉积物  PAHs

英文关键词: HPLC  Fluorescence-UV  Marine sediments  PAHs

中文摘要:

      采用高效液相色谱-荧光和紫外检测联用技术，建立了海洋沉积物中16种多环芳烃（PAHs）的同时测定方法。样品用异丙醇提取，HLB固相萃取柱净化，Waters PAHs C18（4.6 mm×250 mm, 5 μm）色谱柱分离，乙腈-水溶液梯度洗脱，荧光-紫外检测器串联检测。本方法中，16种PAHs在各自相应浓度范围内线性良好，相关系数均大于0.999。添加水平为5 μg/kg和10 μg/kg时，回收率在72.6%~117%之间（n=6），RSD%均小于10%，检出限（S/N=3）为0.2~4.9 μg/kg。利用该方法对采自大连和烟台沿岸的沉积物样品进行了分析，发现均含有一定的PAHs组分。该方法方便、快捷、灵敏度高，为海洋沉积物中PAHs的污染分析及风险评估提供了良好的方法基础。

英文摘要:

      An analytical method based on liquid phase of fluorescence detector combined with UV detector has been developed for the simultaneous determination of sixteen polycyclic aromatic hydrocarbons (PAHs) in marine sediments. After being extracted with isopropanol, the extract was distilled with HLB column, then performed on HPLC with a Waters PAH C18 column (4.6 mm×250 mm, 5 μm), separated by gradient elution using a mixture of acetonitrile and water as mobile phase. The calibration curves were linear with correlation coefficient over 0.999. The average recoveries from spiked marine sediments at the 5 μg/kg and 10 μg/kg concentrations ranged from 72.6%~117%(n=6) with relative standard deviations less than 10％, and limits of detection(LOD) were 0.2~4.9 μg/kg. Some PAHs were found in six marine sediment samples collected from Dalian and Yantai areas. This method was validated to be accurate and sensitive for the analysis and risk assessment of PAHs in marine sediments.