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快速溶剂萃取-凝胶净化-高效液相色谱法测定土壤中6种邻苯二甲酸酯
Determination of Phthalate Esters in Soil Samples by High Performance Liquid Chromatography with Accelerated Solvent Extraction and Gel Permeation Chromatograph Cleanup
投稿时间:2017-01-05  修订日期:2017-03-15
DOI:10.19316/j.issn.1002-6002.2018.03.20
中文关键词:  PAES  ASE  GPC  HPLC  土壤
英文关键词:phthalate esters  accelerated solvent extraction  gel permeation chromatography cleanup  HPLC  soil
基金项目:
作者单位
郭文建 山东省环境监测中心站, 山东 济南 250101 
张慧 山东省环境监测中心站, 山东 济南 250101 
朱晨* 山东省环境监测中心站, 山东 济南 250101 
李红莉 山东省环境监测中心站, 山东 济南 250101 
岳太星 山东省环境监测中心站, 山东 济南 250101 
李洪霞 山东大学环境科学与工程学院, 山东 济南 250013 
郭文波 青岛国家海洋科学研究中心, 山东 青岛 266071 
通讯作者:朱晨*  山东省环境监测中心站, 山东 济南 250101  
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中文摘要:
      建立一种快速溶剂萃取(ASE)-凝胶净化(GPC)-高效液相色谱(HPLC)法测定土壤中6种邻苯二甲酸酯(PAEs)的方法。土壤样品经二氯甲烷-丙酮(体积比为1:1)快速溶剂萃取后,过Bio-Beads SX-3凝胶层析柱净化,收集12~28 min的GPC洗脱液,并进行HPLC-DAD检测分析。通过分段收集,消除了土壤中共存的16种多环芳烃在225 nm紫外波长下对6种PAEs测定的干扰。采用ZORBAX Eclipse Plus C18(150×4.6 mm,5 μm)反相色谱柱,以乙腈-水为流动相进行梯度洗脱,流速为1 mL/min。结果表明,6种PAEs的线性关系良好,相关系数大于0.999 9,方法检出限为2.7~11.5 μg/kg,精密度的相对标准偏差为1.5%~9.5%,加标回收率为66.5%~102%。该方法适用于含多环芳烃的土壤中PAEs的准确测定。
英文摘要:
      High performance liquid chromatography (HPLC) with accelerated solvent extraction (ASE) and gel permeation chromatography cleanup (GPC) were used to determine six phthalate esters in soil samples. Samples were rapidly extracted with a mixture of methylene chloride-acetone (1:1) and purified using a Bio-Beads SX-3 gel with a cyclohexane-ethyl acetate (1:1) elution solvent. Collecting fractional elution (12-28 min), and the interference of co-existed 16 polycyclic aromatic hydrocarbons (PAHs) in phthalate esters detection at 225 nm was removed. ZORBAX Eclipse Plus C18 (150×4.6 mm, 5 μm) and a diode-array UV-vis detector were applied, and acetonitrile/water were used as the mobile phase with gradient elution at a flow rate of 1 mL/min. Results indicated that the method had a good linear relationship (r2>0.9999). The limits of detection (LODs) for six phthalate esters were between 2.7-11.5 μg/kg. The relative standard deviations (RSD) and average recovery rate were 1.5%-9.5%, 66.5%-102%, respectively. This method is suitable for the determination of PAEs in soil containing PAHs.
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