加速溶剂-固相萃取-高效液相色谱法测定废气中多环芳烃

摘要

建立了加速溶剂萃取(ASE)、固相萃取柱净化(SPE)、高效液相色谱仪联合测定废气中16种多环芳烃的分析方法.选定正己烷/丙酮(V/V=1:1)为ASE萃取溶剂,萃取液经硅胶柱净化,洗脱溶剂为正己烷/二氯甲烷(V/V=1:1),洗脱体积为10 mL,洗脱液经旋转蒸发浓缩,用乙腈定容至1 mL,最后用HPLC-紫外检测器对提取液中16种PAHs进行定性与定量分析.方法检出限为0.01~0.03 μg/m3,平均加标回收率为78.7%~106%,相对标准偏差为2.8%~6.8%,能够满足废气中PAHs分析的质量控制要求,该方法稳定性好、准确度高、可操作性强,可用于废气中PAHs的准确定量分析.%The analysis method of 16 kinds of PAHs in waste gas was established by accelerated solvent extraction,solid phase extraction purification and high performance liquid chromatograph.N-hexane/acetone(1+1,V/V)was selected for ASE extraction solvent,extraction liquid was purified by silica column,n-hexane/dichloromethane(1+1,V/V)was elution solvent,elution volume was 10 mL,elution solution was concentrated by rotary evaporation,filled to 1 mL with acetonitrile,finally using HPLC-uv detector to qualitative and quantitative analysis of 16 kinds of PAHs in extraction solution.The method detection limit was 0.01~0.03 μg/m3, average recovery was 78.7%~106%,relative standard deviation was 2.8%~6.8%,could satisfy the requirement for quality control of analyzing PAHs in waste gas.This method had good stability,high accuracy and strong practicality,was able to accurate quantitative analyse of PAHs in waste gas.