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| 分散式固相萃取净化-气相色谱-质谱联用测定土壤中的邻苯二甲酸酯 | |
| 引用本文： | 张渝,张新申,杨坪,张丹.分散式固相萃取净化-气相色谱-质谱联用测定土壤中的邻苯二甲酸酯[J].分析化学,2009,37(10). |
| 作者姓名： | 张渝 张新申 杨坪 张丹 |
| 作者单位： | 1. 四川大学制革清洁技术国家工程实验室,成都,610065;四川省环境监测中心站,成都,610041 2. 四川大学制革清洁技术国家工程实验室,成都,610065 3. 四川省环境监测中心站,成都,610041 |
| 摘 要： | 建立了土壤中18种邻苯二甲酸酯类内分泌干扰物的微波提取-分散式固相萃取净化-GC/MS分析方法.10 g土壤样品经20 mL二氯甲烷和丙酮混合溶剂微波提取后,以丙酮为置换溶剂并浓缩至1.5 mL.浓缩液中加入0.2 g C18吸附剂,振摇3 min后离心10 min(8000 r/min),取1.0 mL上层清液经正己烷置换后用气相色谱-质谱联用分析,并通过基质标准加入校准曲线补偿邻苯二甲酸酯的基体效应.净化所需时间少于20 min.净化后土壤萃取液的基质去除率达到72.7%.方法线性范围7.5～750 μg/kg,相关系数大于0.998; 6次土壤样品测定值的RSD在5.5%～12.1%之间; 加标土壤样品测定值RSD在7.3%～19.4%之间; 平均回收率在94.4%～114.6%之间; 检出限为1.2～4.3 μg/kg. |
| 关 键 词： | 邻苯二甲酸酯 分散式固相萃取 基体效应 土壤 |
Dispersive Solid Phase Extraction Clean-up and Gas Chromatography-Mass Spectrometry for Determination of Phthalate Esters in Soil Samples |
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| ZHANG Yu,ZHANG Xin-Shen,YANG Ping,ZHANG Dan.Dispersive Solid Phase Extraction Clean-up and Gas Chromatography-Mass Spectrometry for Determination of Phthalate Esters in Soil Samples[J].Chinese Journal of Analytical Chemistry,2009,37(10). | |
| Authors: | ZHANG Yu ZHANG Xin-Shen YANG Ping ZHANG Dan |
| Affiliation: | ZHANG Yu1,2,ZHANG Xin-Shen1,YANG Ping2,ZHANG Dan21(National Engineering Laboratory for Clean Technology of Leather Manufacture,Sichuan University,Chengdu 610065)2(The Environmental Monitoring,Center of Sichuan Province,Chengdu 610041) |
| Abstract: | A method was developed to determine phthalate esters in soil samples.The entire pre-treatment process involved microwave-assisted extraction,solvent conversion and clean-up of dispersive solid-phase extraction(DSPE).A total of 10 g soil sample was extracted by microwave mixed with 20 mL mixed-phase solvent of dichloromethane and acetone.And then the extract of mixed-phase was converted into the acetone-phase and then concentrated to 1.5 mL extract.The concentrated extract was shaken for 3 min that mixed wit... |
| Keywords: | Phthalate esters dispersive solid phase extraction matrix effect soil |
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