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目的建立同时测定沉积物中15种多环芳烃(PAHs)污染物的凝胶渗透色谱-高效液相色谱分析方法。方法样品中的多环芳烃通过环己烷-乙酸乙酯(1∶1,V/V)提取,凝胶渗透色谱净化,液相色谱-荧光检测器测定,外标法定量。结果通过对梯度洗脱条件、荧光激发和发射波长等条件的优化,实现了15种多环芳烃组分的完全分离和荧光高灵敏度检测,在优化后的测定条件下,15种多环芳烃在0.20μg/L~50.0μg/L时具有良好线性关系,相关系数(r)≥0.999 4,方法的检出限为0.3μg/kg~1.0μg/kg,回收率为68.8%~104.0%,相对标准偏差≤6.7%。结论该方法准确、灵敏,适用于沉积物中15种多环芳烃的同时测定。
Objective To establish a method for simultaneous determination of 15 polycyclic aromatic hydrocarbons (PAHs) in sediments by gel permeation chromatography - high performance liquid chromatography. Methods Polycyclic aromatic hydrocarbons (PAHs) were extracted by cyclohexane - ethyl acetate (1: 1, V / V), purified by gel permeation chromatography (GPC), determined by liquid chromatography - fluorescence detector and quantified by external standard method. Results The conditions of gradient elution, fluorescence excitation and emission wavelength were optimized. Complete separation and high sensitivity detection of 15 polycyclic aromatic hydrocarbons (PAHs) were achieved. Under optimized conditions, 15 PAHs The linear range was 0.20μg / L ~ 50.0μg / L with the correlation coefficient (r) ≥0.999 4. The detection limit was 0.3μg / kg ~ 1.0μg / kg and the recovery was 68.8% ~ 104.0% Standard deviation ≤ 6.7%. Conclusion The method is accurate and sensitive and suitable for the simultaneous determination of 15 PAHs in sediments.