超高效液相-荧光检测器法测定柴油中多环芳烃

Determination of polycyclic aromatic hydrocarbons in diesel oil using ultra HPLC-fluorescence detection method

建立了采用超高效色谱（UPLC）-荧光检测器法测定柴油中10种常见的多环芳烃含量的方法。这10种常见的多环芳烃为萘、苊、二氢苊、芴、菲、蒽、荧蒽、芘、苯并[a]蒽、艹屈、苯并[b]荧蒽、苯并[k]荧蒽、苯并[a]芘和苯并[g,h,i]芘。样品经过固相萃取后用甲醇溶解,采用Acquity UPLC BEH Phenyl C18柱（100 mm×2.1 mm,1.7μm）分离,乙腈-水为流动相进行梯度洗脱,采用荧光检测器检测,并用外标法进行定量分析。结果表明,在一定质量浓度范围内,峰面积与质量浓度的线性关系良好,用标准加入法进行回收率实验,对方法的准确度进行考察,相对标准偏差为0.56%～8.76%,加标回收率为100.04%～115.04%。与其他检测柴油中多环芳烃方法比较,该方法简单,分离效果好,快速及准确。

A method for the determination of polycyclic aromatic hydrocarbons in diesel oil using ultra performance liquid chromatography with fluorescence detector. These components were naphthalene,acenaphthylene,acenaphthene,fluorene,phenanthrene,anthracene,fluoranthene,pyrene,benzo [a] anthracene,chrysene,benzo[b] fluoranthene,benzo [k] fluoranthene,benzo [a] pyrene and benzo [g,h,i] pyrene. The sample was dissolved in methanol after solid phase extraction from the products. The separation column was an Acquity UPLC BEH Phenyl C18（ 100 mm × 2. 1 mm,1. 7 μm） and the mobile phase was acetonitrile-water. The sample was detected by fluorescence detector and quantitative analysis by external standard method. The results showed that the sample of a good linear relationship between peak area and mass concentration in a certain concentration range. The accuracy of the method were investigated by standard addition method recovery experiments. The relative standard deviation was from 0. 56% to8. 76% and the recovery was from 100. 04% to 115. 04%. Compared with other detection of PAHs in diesel fuel,the method is simple,good separation,fast and accurate.