凝固漂浮有机液滴-分散液液微萃取结合高效液相色谱法同时测定自来水中氯代多环芳烃与多环芳烃

Determination of Chlorinated Polycyclic Aromatic Hydrocarbons and Polycyclic Aromatic Hydrocarbons in Tap Water Samples by High Performance Liquid Chromatography with Dispersive Liquid-liquid Microextraction Based on Solidification of Floating Organic Drop

建立了自来水中6种氯代多环芳烃和15种多环芳烃的凝固漂浮有机液滴-分散液液微萃取高效液相色谱分析方法,并探讨了萃取剂种类和用量、分散剂种类和用量、氯化钠含量及涡旋振荡时间等因素对萃取效率的影响。优化后的萃取实验条件为:10μL十二醇为萃取溶剂,500μL甲醇为分散溶剂,6%NaCl,涡旋振荡时间2 min。目标化合物经多环芳烃专用柱(SUPELCOSILTMLC-PAH,150 mm×4.6 mm,5μm)分离后,外标法定量。结果表明,21种目标化合物在一定质量浓度范围内线性良好,相关系数均不低于0.999;在低、中、高3个加标水平下的回收率为70.6%~98.7%,相对标准偏差(RSD)为2.0%~10%;方法的检出限(LOD,S/N=3)为0.0007~0.009μg/L,定量下限(LOQ,S/N=10)为0.0022~0.028μg/L。可用于自来水中氯代多环芳烃和多环芳烃的分析检测。

A novel dispersive liquid-liquid microextraction method based on solidification of floating organic droplets(DLLME-SFO)was developed for the determination of six kinds of chlorinated polycyclic aromatic hydrocarbons and fifteen kinds of polycyclic aromatic hydrocarbons in water samples by high performance liquid chromatography with fluorescence detection.The factors relevant to the microextraction efficiency,such as type and volume of disperant and extraction solvents,amount of NaCl and extraction time were investigated and optimized.The optimal liquid-liquid microextraction experiment conditions were as follows:10μL of 1-dodecanol as extractant solvent,500μL of methanol as dispersive solvent,6%(mass percentage)NaCl,2 min of extraction time for vortex oscillation.The separation of the target compounds was performed on a SUPELCOSILTMLC-PAH column(150 mm×4.6 mm,5μm)with acetonitrile-water as mobile phase by gradient elution.Quantitative determination was achieved by external standard method.Results showed that there existed good linear relationships for 21 target compounds in certain concentration ranges with their correlation coefficients(r)not less than 0.999.The average recoveries for the target compounds ranged from 70.6%to 98.7%with corresponding relative standard deviations(RSD,n=3)of 2.0%-10%.The limits of detection(LOD,S/N=3)and limits of quantification(LOQ,S/N=10)were in the ranges of 0.0007-0.009μg/L and 0.0022-0.028μg/L,respectively.The proposed method is applicable for the rapid determination of chlorinated polycyclic aromatic hydrocarbons and polycyclic aromatic hydrocarbons in surface water samples.