沉积物中12种羟基多环芳烃的分析

摘要

A sample pretreatment method was developed for 12 hydroxylated polycylic aromatic hydrocar-bons (OH-PAHs)in sediment samples.The OH-PAHs was extracted by accelerated solvent extraction (ASE)from sediment matrix and clean up by solid phase extraction (SPE),the target compounds were finally analyzed by GC-MS after derivatization by BSTFA.Several parameters,including the extraction solvent for ASE,alumina oxide sorbent for SPE and derivatization time that affected the proposed method, were optimized.The results showed that the LODs of the target analytes were ng·kg-1 level and the RS-Ds were acceptable (<10%)when using methanol as ASE extraction reagent at 60 ℃for 60 min and a-lumina oxide as SPE sorbent.Moreover,the recoveries of the analytes were higher than 60% except for 9-hydroxy-phenanthrene (39.5%).The proposed method was applied to determine 12 hydroxylated PAHs in sediments of Humen estuary,south China and 10hydroxylated PAHs were detected with the con-centrations ranging from 0.58 (4-hydroxy-phenanthrene)to 2.4 ng·g-1 (6-hydroxy-chyrene).%建立了一种同时检测沉积物中12种羟基化多环芳烃代谢物（OH-PAHs）的方法。样品经冷冻干燥后，分别采用加速溶剂萃取（ASE）、固相萃取（SPE）及衍生化进行样品前处理，气相色谱－质谱联用仪（GC-MS）进行分析测定。通过单因子优化后，12种代谢物的方法检出限（LODs）均达到ng·kg－1级别，并且重现性较好。通过加标回收的方法，在样品中加入12种代谢物至质量分数均为10 ng·g－1以评价方法的回收率，结果发现除了9－羟基菲较低外（39.5％），其余待测组分的回收率均在60％以上。所建立的分析方法最终被应用于检测珠江虎门河口沉积物中的12种羟基化多环芳烃，其中10种待测组分被检出，并且质量分数介于0.58（4－羟基菲）～2.4 ng·g－1（6－羟基屈）之间。