微萃取瓶富集-高效液相色谱法测定海水中多环芳烃

Determination of Polycyclic Aromatic Hydrocarbons in Seawater by Enrichment of Microextraction Flask-High Performance Liquid Chromatography

采用自制微萃取瓶富集-反相高效液相色谱法同时测定海水中的萘、菲、荧蒽。实验选择DiamonsilC18(250×4.6mmi.d.,5μm)色谱柱,体积比为88∶12的甲醇-水作流动相,流速1.0mL/min,检测波长280nm,柱温30℃。最佳萃取条件:400mL水样,300μL正辛烷作萃取剂,NaCl浓度100g/L,萃取时间15min。在10～5×104μg/L范围内,萘、菲、荧蒽呈现良好线性关系(相关系数均大于0.9997)。萘、菲、荧蒽检出限分别为13.3、13.3、7.0ng/L;加标回收率分别为94.50%、94.05%、92.59%;相对标准偏差分别为1.60%、1.82%、0.90%。

A method based on enrichment of microextraction flask-high performance liquid chromatography was developed for the simultaneous determination of three polycyclic aromatic hydrocarbons（PAHs）in seawater.The chromatographic conditions were as follows：a Diamonsil C18 column（250×4.6mm i.d.,5μm）was used for separation at 30℃ with detection wavelength at 280 nm;mobile phase was a mixture of methanol and water（the ratio of volume was 88∶12）,and flow rate was 1.0mL/min.The optimal extraction conditions were as follows：the sample was 400mL seawater; extraction solvent was 300μL n-octane;salinity of sample was 100g/L,and extraction time was 15 min.At the range of 10～5×10^4μg/L,the methodology exhibited good linearity with correlation coefficiency above 0.9997.The detection limits were 13.3ng/L for naphthalene,13.3ng/L for phenanthrene and 7.0ng/L for fluoranthene,respectively.The average recoveries and relative standard deviations were 94.50%and 1.60%for naphthalene,94.05%and 1.82%for phenanthrene,92.59% and 0.90%for fluoranthene,respectively.