超声微波协同萃取-气相色谱法测定土壤中邻苯二甲酸酯类化合物

Determination of PAEs in Soil by Gas Chromatography after Ultrasonic and Microwave Assisted Extraction

研究了超声微波协同萃取-气相色谱测定土壤中的邻苯二甲酸酯类化合物。考察了萃取溶剂、微波功率、萃取时间等因素对回收率的影响,得到了最佳萃取条件为：以正己烷/丙酮（1∶1）为萃取剂,溶剂用量为60 mL,微波辐射功率为100 W（超声功率固定为50 W）,萃取12 min。该条件下,模拟土样中酞酸酯的平均回收率可达92.5%。方法的检出限为0.05~0.16 mg/kg,相对标准偏差（RSD）〈5.8%。与直接超声、开放式微波萃取法相比,此法具有明显的优势。方法用于实际土样的测定,所得结果与索氏抽提的结果相当。

The determination of four PAEs（DBP,BBP,DEHP,DNOP） in soil by ultrasonic and microwave assisted extraction combined with GC-FID was studied.The influence of several parameters on the extraction efficiencies such as solvent,microwave power,extraction time was investigated,and the optimal operation conditions were obtained.With 60 mL n-hexane-acetone（1/1,V/V） as the extraction solvent,the average recoveries of PAEs was 92.5% after 12 min extraction at 100 W microwave and 50 W ultrasonic treatment.Contrast to the traditional MAE,satisfactory recoveries could be obtained without adding water in the solvent in this method.The recoveries of PAEs with this method were higher than those with single open MAE and USE.This method was applied in the determination of PAEs in the lake sediment,the results were in agreement with those obtained with SOX-GC.The detection limits of the developed method were between 0.05 and 0.16 mg/kg,and the relative standard deviations were below 5.8%.