固相动态微萃取气相色谱法分析土壤中邻苯二甲酸酯类  

Fully automated determination of phthalate esters in soil using headspace solid phase dynamic extraction and gas chromatography

作　　者：盛梅[1] 曹国民[1] 杜晓丹[1] 姜虹[1] 陈杰颖[1] 张福顺[1] 

机构地区：[1]华东理工大学环境工程研究所,上海200237

出　　处：《分析试验室》2013年第5期48-52,共5页Chinese Journal of Analysis Laboratory

基　　金：上海市大学生创新性实验计划项目(S0834)资助

摘　　要：利用自动顶空固相动态微萃取毛细管气相色谱联用(HS-SPDE-GC)技术,建立了一种测定土壤中邻苯二甲酸酯类(PAEs)的方法。对固相动态微萃取的操作条件进行了优化。适宜的操作条件为:在0.5g土壤中加入0.3 mL水,置于110℃的振荡器中加热振荡20 min,推杆反复抽吸40次,可使样品中待测组分最大程度被富集在萃取头内壁。该方法线性范围宽,线性关系好(R2>0.99),4种组分的平均回收率在80.5%～124.6%,相对标准偏差为3.6%～14%,检出限分别为0.1115,0.0387,0.0588和0.1962μg/g。A simple, fast and fully automated method based on headspace solid phase dynamic extraction coupled online with gas chromatography （HS-SPDE-GC） is proposed for phthalate esters in soil. The effects of equilibrium time, added water, extraction temperature and times were studied to develop HS-SPDE condition for obtaining the highest extraction efficiency. The results indicate that the optimum conditions were： 0. 3 mL of water added into 0.5 g of soil, agitated for 20 rain at 110℃, headspace solid phase dynamic dextraction 40 times. Under the optimized conditions, the linearity was very good in the considered concentration ranges （R2≥ 0.99）. Average recoveries for spiked standards （n = 7） ranged from 80.5% to 124.6% and showed good accuracy for the proposed analytical method. Average relative standard deviations （RSDs） of four phthalic acid esters were 3.6% -14%. The limits of detection for DMP, DEP, DBP and DNAP were 0. 1115, 0.0387, 0. 0588 and 0. 1962μg/g, respectively. The method was applied to the analysis of phthalate esters in soil.

关 键 词：邻苯二甲酸酯类 土壤 固相动态微萃取 气相色谱 

分 类 号：O657.7[理学—分析化学]