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固相萃取-液相色谱/荧光检测法同时测定水中8种烷基酚和烷基酚聚氧乙烯醚

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郭文建, 王超, 吕怡兵, 王桂勋. 固相萃取-液相色谱/荧光检测法同时测定水中8种烷基酚和烷基酚聚氧乙烯醚[J]. 环境化学, 2018, 37(3): 497-504. doi: 10.7524/j.issn.0254-6108.2017071301
引用本文: 郭文建, 王超, 吕怡兵, 王桂勋. 固相萃取-液相色谱/荧光检测法同时测定水中8种烷基酚和烷基酚聚氧乙烯醚[J]. 环境化学, 2018, 37(3): 497-504. doi: 10.7524/j.issn.0254-6108.2017071301
shu
GUO Wenjian, WANG Chao, LYU Yibing, WANG Guixun. Simultaneous determination of eight alkylphenols and alkylphenol ethoxylates in water by solid phase extraction and high performance liquid chromatography with fluorescence detection[J]. Environmental Chemistry, 2018, 37(3): 497-504. doi: 10.7524/j.issn.0254-6108.2017071301
Citation: GUO Wenjian, WANG Chao, LYU Yibing, WANG Guixun. Simultaneous determination of eight alkylphenols and alkylphenol ethoxylates in water by solid phase extraction and high performance liquid chromatography with fluorescence detection[J]. Environmental Chemistry, 2018, 37(3): 497-504. doi: 10.7524/j.issn.0254-6108.2017071301
shu

固相萃取-液相色谱/荧光检测法同时测定水中8种烷基酚和烷基酚聚氧乙烯醚

  • 1.

    中国环境监测总站, 北京, 100012;

  • 2.

    山东省环境监测中心站, 济南, 250101

  • 基金项目:

    国家高科技技术研究发展计划（863）重大项目（2013AA06A308）资助.

Simultaneous determination of eight alkylphenols and alkylphenol ethoxylates in water by solid phase extraction and high performance liquid chromatography with fluorescence detection

  • 1.

    China National Environmental Monitoring Centre, Beijing, 100012, China;

  • 2.

    Shandong Province Environmental Monitoring Centre, Ji'nan, 250101, China

  • Fund Project: Supported by the National High Technology R&D Program of China(2013AA06A308).

  • 摘要: 本文通过优化色谱条件、前处理条件、样品保存条件等，建立了水中8种烷基酚（APs）和烷基酚聚氧乙烯醚（APEOs）的固相萃取（SPE）—高效液相色谱/荧光检测（HPLC-FLD）分析方法.水样经酸化（pH 2.0—3.0）后加入甲醇至20%体积分数，并以10 mL·min-1速度通过HLB固相萃取小柱进行浓缩和净化，收集SPE洗脱液进行HPLC-FLD检测分析.采用Waters PAH C18色谱柱（4.6×250 mm，5.0 μm），以乙腈和5 mmol·L-1醋酸铵溶液进行梯度洗脱，流速为1.0 mL·min-1，荧光检测的激发和发射波长分别为228 nm和300 nm.结果表明，8种组分的线性关系良好（R>0.998），方法检出限为0.2—0.5 μg·L-1.在低、中、高加标水平下，8种组分的回收率分别为82.5%—119.4%、92.1%—118.0%、89.7%—103.9%，平均相对标准偏差分别为5.3%、5.4%、2.9%.该方法灵敏度高、操作简单、易于推广应用，适用于水中多种APs与APEOs的同时分析.
    Abstract: This study presents a method for the simultaneous determination of eight alkylphenols (APs) and alkylphenol ethoxylates (APEOs) in water samples by solid phase extraction (SPE) and high performance liquid chromatography with fluorescence detector (HPLC-FLD). Samples were acidified (pH 2.0-3.0) and adjusted to containing 20% methanol before concentration and purification by HLB SPE cartridges. APs and APEOs were analyzed by liquid chromatography with PAH C18 chromatographic column (4.6×250 mm, 5.0 μm) and fluorescence detector. The excitation wavelength and emission wavelength were 228 nm and 300 nm, respectively. Acetonitrile-5 mmol·L-1 ammonium acetate were used as the mobile phase with gradient elution at a flow rate of 1 mL·min-1. Results indicated that the method has a good linear relationship (R>0.998). The limits of detection (LODs) for eight APs and APEOs were 0.2-0.5 μg·L-1. The recoveries of eight analytes at low, medium, and high spiked levels were 82.5%-119.4%, 92.1%-118.0% and 89.7%-103.9%, respectively. The corresponding average relative standard deviations (RSD) were 5.3%, 5.4% and 2.9%, respectively. The method is simple, senvitive and easy to implement. It is suitable for the simultaneous detection of various APs and APEOs in water.
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  • 收稿日期:  2017-07-13
  • 刊出日期:  2018-03-15
郭文建, 王超, 吕怡兵, 王桂勋. 固相萃取-液相色谱/荧光检测法同时测定水中8种烷基酚和烷基酚聚氧乙烯醚[J]. 环境化学, 2018, 37(3): 497-504. doi: 10.7524/j.issn.0254-6108.2017071301
引用本文: 郭文建, 王超, 吕怡兵, 王桂勋. 固相萃取-液相色谱/荧光检测法同时测定水中8种烷基酚和烷基酚聚氧乙烯醚[J]. 环境化学, 2018, 37(3): 497-504. doi: 10.7524/j.issn.0254-6108.2017071301
shu
GUO Wenjian, WANG Chao, LYU Yibing, WANG Guixun. Simultaneous determination of eight alkylphenols and alkylphenol ethoxylates in water by solid phase extraction and high performance liquid chromatography with fluorescence detection[J]. Environmental Chemistry, 2018, 37(3): 497-504. doi: 10.7524/j.issn.0254-6108.2017071301
Citation: GUO Wenjian, WANG Chao, LYU Yibing, WANG Guixun. Simultaneous determination of eight alkylphenols and alkylphenol ethoxylates in water by solid phase extraction and high performance liquid chromatography with fluorescence detection[J]. Environmental Chemistry, 2018, 37(3): 497-504. doi: 10.7524/j.issn.0254-6108.2017071301
shu

固相萃取-液相色谱/荧光检测法同时测定水中8种烷基酚和烷基酚聚氧乙烯醚

  • 1.  中国环境监测总站, 北京, 100012;
  • 2.  山东省环境监测中心站, 济南, 250101
  • 收稿日期:  2017-07-13
基金项目:

国家高科技技术研究发展计划（863）重大项目（2013AA06A308）资助.

摘要: 本文通过优化色谱条件、前处理条件、样品保存条件等，建立了水中8种烷基酚（APs）和烷基酚聚氧乙烯醚（APEOs）的固相萃取（SPE）—高效液相色谱/荧光检测（HPLC-FLD）分析方法.水样经酸化（pH 2.0—3.0）后加入甲醇至20%体积分数，并以10 mL·min-1速度通过HLB固相萃取小柱进行浓缩和净化，收集SPE洗脱液进行HPLC-FLD检测分析.采用Waters PAH C18色谱柱（4.6×250 mm，5.0 μm），以乙腈和5 mmol·L-1醋酸铵溶液进行梯度洗脱，流速为1.0 mL·min-1，荧光检测的激发和发射波长分别为228 nm和300 nm.结果表明，8种组分的线性关系良好（R>0.998），方法检出限为0.2—0.5 μg·L-1.在低、中、高加标水平下，8种组分的回收率分别为82.5%—119.4%、92.1%—118.0%、89.7%—103.9%，平均相对标准偏差分别为5.3%、5.4%、2.9%.该方法灵敏度高、操作简单、易于推广应用，适用于水中多种APs与APEOs的同时分析.

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