超声萃取-高效液相色谱法测定土壤中8种烷基酚和烷基酚聚氧乙烯醚  

Determination of Eight Kinds of Alkylphenols and Alkylphenol Ethoxylates in Soil by Ultrasonic-assisted Extraction and High Performance Liquid Chromatography

作　　者：赵陈晨 王超[1] 郭文建[3] 吕怡兵[1] 陈红雨 ZHAO Chen-Chen;WANG Chao;GUO Wen-Jian;LYU Yi-Bing;CHEN Hong-Yu(China National Environmental Monitoring Centre,Beijing 100012,China;Chengdu Environmental Monitoring Center,Chengdu 610000,China;Shandong Environmental Monitoring Center,Jinan 250101,China)

机构地区：[1]中国环境监测总站,北京100012 [2]成都市环境监测中心站,成都610000 [3]山东省环境监测中心站,济南250101

出　　处：《分析化学》2018年第8期1306-1313,共8页Chinese Journal of Analytical Chemistry

基　　金：国家高技术研究发展计划项目(No.2013AA06A308)资助~~

摘　　要：建立了一种测定土壤中8种烷基酚(APs)和烷基酚聚氧乙烯醚(APEOs)的分析方法。样品用二氯甲烷-乙酸乙酯(4∶1,V/V)混合溶剂进行3次超声提取,经硅胶固相萃取柱净化,采用高效液相色谱(HPLC)和Waters PAH C_(18)色谱柱(250 mm×4.6 mm,5.0μm),以乙腈-水(85∶15,V/V)溶液等度洗脱,在16 min内完成分离,通过荧光检测器(λ_(ex)/λ_(em)=228/300 nm)检测。结果表明,8种组分在10.0~500μg/L范围内有良好的线性关系(R>0.999),检出限为1.2~3.0μg/kg,测定下限为4.8~12.0μg/kg。在高、低浓度基体加标测试中,8种组分的回收率分别为69.9%~81.8%和70.3%~84.8%,相对标准偏差(RSD)分别为2.2%~6.8%和5.1%~12.1%。本方法灵敏度高、重现性好,操作简单且便于推广,可用于土壤中烷基酚及烷基酚聚氧乙烯醚的同时测定。.A method for determination of 8 kinds of alkylphenols（ APs） and alkylphenol ethoxylates（ APEOs） in soil was developed in this work. The samples were extracted by ultrasonic-assisted procedure for three times with dichloromethane-ethyl acetate（ 4 ∶ 1,V/V）,and purified by silica gel cartridge. Then the eight compounds were separated in 16 min by high performance liquid chromatography（ HPLC） with a chromatographic column of Waters PAH C18 column（ 250 mm × 4. 6 mm,5. 0 μm）. The mobile phase was acetonitrile-water（ 85 ∶ 15,V/V） with a flow rate of 0. 8 mL/min. Fluorescence detection was used to sensitively measure the targets. The excitation and emission wavelength was 228 nm and 300 nm,respectively.The qualitative and the quantitative detection were carried out based on retention time and external calibration peak area,respectively. The results indicated that linear relationships（ R） were higher than 0. 999 in the range of 10.0-500 μg/L for 8 kinds of APs and APEOs. The detection limits（ MDL） were 1.2-3.0 μg/kg,and the quantification limits were 4. 8-12. 0 μg/kg. The recoveries of the 8 kinds of targets at high and low spiked levels were in the range of 69.9%-81.8% and 70.3%-84.8%,respectively. The corresponding relative standard deviations（ RSD） were 2.2%-6. 8% and 5. 1%-12. 1%,respectively. The method was simple and sensitive with high reproducibility,and could be applied in the detection of 8 kinds of alkylphenols and alkylphenol ethoxylates in soil.

关 键 词：烷基酚 烷基酚聚氧乙烯醚 超声萃取 高效液相色谱法 荧光检测 土壤 

分 类 号：O657.72[理学—分析化学]