超声辅助分散液液微萃取-气相色谱检测污泥中氯苯

Optimized ultrasonic assisted extraction dispersive liquid-liquid microextraction coupled with gas chromatography- electron capture detector for extraction and determination of chlorobenzenes in sludge

采用超声辅助分散液液微萃取结合气相色谱（UAE-DLLME-GC-ECD）检测了污泥中6种氯苯化合物.用丙酮作为萃取污泥样品中氯苯的萃取剂,通过改变萃取剂类型和用量、超声时间以及离子强度等影响因子的实验,确定了最优条件的关键性控制参数.结果表明,6种氯苯的相关系数r2=0.9993~0.9999,相对标准偏差RSD=3.2%~4.4%,检测限LOD为0.001~0.2μg/kg,对造纸、印染和市政3种污泥样品检测的回收率分别为89.2%~103.8%,94.5%~112.1%和89.1%~104.3%.该方法检测污泥中的氯苯不仅具有快速、灵敏和重复性好的特点,而且相对于传统方法,可以节省大量对人体有毒害作用的有机溶剂和分析时间.

Ultrasonic assisted extraction dispersive liquid-liquid microextraction（UAE-DLLME） coupled with gas chromatography-electron capture detection（GC-ECD） was applied to extract and determine six different types of chlorobenzenes（CBs） in sludge samples. Acetone was used as extraction solvent for CBs. The effects of various parameters such as ultrasonic time,ionic strength,volume of disperser and extraction solvents as well as extraction types were investigated to determine the optimum conditions for this method. Under the optimum conditions,the method＇s coefficients of correlation（r2） were between 0.9993 and 0.9999. The relative standard deviations（R.S.D.,n = 6） varied between 3.2% and 4.4%. The limits of detection（LODs）,based on signal-to-noise（S/N） of 3,were between 0.001 and 0.2 μg/kg. The relative recoveries of the six CBs from three sludge samples,S1,S2 and S3,were in the range of 89.2%~103.8%,89.1%~104.3% and 94.5%~112.1%,respectively. It required less analysis time and harmful solvent than the conventional methods. The results showed that UAE-DLLME coupled with GC-ECD was an efficient,sensitive,and reliable method for the determination of CBs in sludge samples.