建立了固相萃取-气质联用法测定水中佳乐麝香(HHCB)和吐纳麝香(AHTN)这两种主要的多环麝香的方法。利用Oasis HLB固相萃取小柱预处理水样,通过对固相萃取条件的优化,得出了最佳实验条件:洗脱溶剂为正己烷,洗脱体积为10mL,水样中添加体积分数0.5%甲醇作为有机改性剂,控制上样流速为5~10mL/min,洗脱速率为0.5~2mL/min。该方法线性相关性好,相对标准偏差在1.67%~5.48%之间,对两种多环麝香的方法检测限均为0.025μg/L。利用该方法对污水处理厂进出水中多环麝香进行测定,佳乐麝香和吐纳麝香的去除率分别为61.3%和51.6%。
A method for the determination of two representative polycyclic musks HHCB(1,3,4,6,7,8-hexahydro-4,6,6,7,8,8-hexamethylcyclopenta-(g)-2-benzopyran) and AHTN(7-acetyl-1,1,3,4,4,6-hexamethyl-1,2,3,4-tetrahydronaphthalene) in water by GC-MS with selective ion monitoring(SIM) mode and the Oasis HLB solid-phase extraction(SPE)pre-treatment was proposed.The test of the main factors influencing SPE was carried out,and the optimal extraction conditions were obtained,in which hexane was the eluting solvent,eluting solvent volume was 10 mL,0.5% methanol as an organic modifier,eluting rate was 0.5~2 mL/min,and flow rate of water sample was 5~10 mL/min.This method had good linear correlation coefficent,and the relative standard deviation ranged from 1.67% to 5.48%.The detection limits were 0.025μg/L for two polycyclic musks.Then the contents of polycyclic musks in influent and effluent from a municipal sewage treatment plant in Shanghai were determined by this method.The results showed that the removal efficiencies of HHCB and AHTN were 61.3% and 51.6%,respectively.