固相萃取-高效液相色谱法测定城市污水中痕量多环芳烃的研究

Study on the Determination of Trace Amount of Polycyclic Aromatic Hydrocarbons in Urban Sewage by Solid-phase Extraction Coupled with High Performance Liquid Chromatograph

[目的]采用固相萃取-高效液相色谱法测定城市污水中痕量多环芳烃.[方法]从固相萃取柱、洗脱溶剂、洗脱体积、洗脱速度等方面,对固相萃取-反相高效液相色谱法的试验条件进行优化,并检测城市污水中痕量多环芳烃。[结果]优化得到的固相萃取条件为:选择SUPELCLEAN LC-18固相萃取柱;以二氯甲烷为洗脱溶剂,洗脱体积为15 ml,分3次洗脱,洗脱速度为2 ml/min;上样速度为5ml/min,上样体积为1 000 ml,并向水样添加200 ml甲醇作有机改性溶剂。在该萃取条件下,该方法的加标回收率高,为76.3%～105.2%;相对标准偏差为3.8%～6.0%,精密度好;检出限低,为0.000 8～0.048μg/L。[结论]固相萃取-反相高效液相色谱法操作简便,灵敏度高,精密度好,适用于大体积水样连续测定。

[Method] The study aimed at determining trace amount of polycyclic aromatic hydrocarbons（PAHs） in urban sewage by using solid-phase extraction（SPE） coupled with high performance liquid chromatograph（HPLC）.[Method] From the aspects of solid-phase extraction column,elution solvent,elution volume,elution speed and so forth,the test conditions of SPE-HPLC method were optimized,and trace amounts of PAHs in urban sewage was determined by this method.[Result] The optimized solid-phase extraction conditions were SUPELCLEAN LC-18 solid-phase extraction column,methylene dichloride as elution solvent,15 ml elution volume,2 ml/min elution speed,5 ml/min loading speed,1 000 ml water with 200 ml methanol loading volume.Under the optimized extraction conditions,the average recovery was high,namely 76.3%-105.2%;relative standard deviation was 3.8%-6.0%,showing good precision;detection limit was low,only 0.000 8-0.048 μg/L.[Conclusion] The method is user-friendly,with high sensitivity and good precision,and suitable for continuous determination of a large volume of water.