摘要
比较了索氏提取法和微波萃取法对土壤中15种多环芳烃的提取效果,优化了层析柱的淋洗体积和DAD检测波长。结果表明,用二氯甲烷在50℃下索氏提取24h,将提取液旋转蒸干,加入环己烷溶解后过硅胶柱净化,正己烷和二氯甲烷(1∶1)洗脱,收集50 mL洗脱液,25℃氮吹浓缩后用高效液相色谱法测定。测定中采用梯度洗脱,DAD检测器的波长为230 nm,15种多环芳烃在30 min内就能达到良好的分离,方法回收率在65.18%~93.4%之间,检测限为5.2×10-3~1.8×10-2mg/kg,且重现性好,并对实际土壤样品进行了测定及分析。
The effects of Soxhlet extraction and microwave extraction for 15 PAHs in soil were studied and column elution volume and DAD detection wavelength were optimized.The results demonstrated the mixture was Soxhlet extracted for 24 h at 50 ℃,the extraction was evaporated to dryness in a rotary evaporator,cyclohexane was added to dissolve it and then added the solution to a silica gel column for purification,and eluted with n-hexane and dichloromethane(1∶1),collecting 50 mL eluent,concentrated by nitrogen purge at 25 ℃,then determined by high performance liquid chromatography under the condition of gradient elution and DAD detection wavelength at 230 nm,under this condition,only in 30 min a good separation for 15 PAHs could be gotten,its recovery was 65.18% to 93.4 %,and the detection limit was 5.2 × 10- 3to 1.8 × 10- 2mg /kg,showing good reproducibility,and PAHs in the actual soil samples were detected and analyzed.
出处
《环境工程》
CAS
CSCD
北大核心
2014年第S1期988-991,1004,共5页
Environmental Engineering
基金
上海市科委重点项目(09230500200)