高效液相色谱法测定黄浦江表层沉积物中的痕量多环芳烃

Determination of Trace Polycyclic Aromatic Hydrocarbons in Surface Sediments of Huangpu River by High Performance Liquid Chromatography

建立了高效液相色谱-二极管阵列检测器（PDA）测定上海市黄浦江表层沉积物中16种多环芳烃（PAHs）的方法。在保留时间定性分析的基础上，利用PDA获取的紫外扫描光谱图对目标组分进行了准确的定性，并通过异构体紫外光谱图中特征峰的差异有效地识别了样品中的4种异构体，即苯并[b]荧蒽、苯并[k]荧蒽、苯并[a]芘和苯并[e]芘。通过检测波长的优化，减少了干扰物的影响，提高了检测灵敏度；针对分离度较差的两种目标组分（苯并[b]荧蒽和苯并[k]荧葸）的定量进行了分析讨论。该方法对16种PAHs的检出限（以于基计）介于1．1～18．3ng／g之间，具有较高的方法灵敏度。黄浦江表层沉积物测定结果表明，除二氢苊外的15种PAHs都被检出。含量为10．1～253．0ng／g。

The 15 polycyclic aromatic hydrocarbons, included in US EPA Priority Pollutant List, in surface sediments from Huangpu River were qualified and quantified using high performance liquid chromatograph （HPLC） coupled with photodiode array detector （PDA）. On the basis of qualification by retention times, the ultraviolet spectra of 16 PAHs obtained from PDA were used to improve the qualification. Furthermore, benzo [ b ] fluoranthene, benzo [ k ] fluoranthene, benzo [ a ]pyrene and benzo [ e ] pyrene in sediment samples were identified with the differences of ultraviolet spectra of isomers. The quantitative method for 16 trace PAHs in the sediments was developed. In order to intensify ultraviolet response of target components and reduce those of the interferents, detection wavelengths of 16 PAHs were optimized. The limits of detection were improved further and were from 1.1 to 18.3 ng/g on dry basis, and spiked recoveries from environmental samples were 87% - 113%. Therefore, the quantitative method in this study was sensitive and accurate and was satisfied for the determination of trace PAHs in environmental samples. Finally, the quantitative method was successfully used for the analysis of the surface sediments of Huangpu River. All the PAHs, except acenaphthylene, were detected. The concentrations of the PAHs were 10. 1 - 253.0 ng/g and their relative standard deviations （RSD） were less than 10%.