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固相萃取-高效液相色谱-串联质谱法测定水体中三苯乙烯基苯酚聚氧乙烯醚

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张雅莉, 高俊敏, 李春梅, 周杰, 贺青华, 王静, 金芬. 固相萃取-高效液相色谱-串联质谱法测定水体中三苯乙烯基苯酚聚氧乙烯醚[J]. 环境化学, 2020, (7): 1941-1948. doi: 10.7524/j.issn.0254-6108.2019090206
引用本文: 张雅莉, 高俊敏, 李春梅, 周杰, 贺青华, 王静, 金芬. 固相萃取-高效液相色谱-串联质谱法测定水体中三苯乙烯基苯酚聚氧乙烯醚[J]. 环境化学, 2020, (7): 1941-1948. doi: 10.7524/j.issn.0254-6108.2019090206
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ZHANG Yali, GAO Junmin, LI Chunmei, ZHOU Jie, HE Qinghua, WANG Jing, JIN Fen. Determination of tristyrylphenol ethoxylates in water by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry[J]. Environmental Chemistry, 2020, (7): 1941-1948. doi: 10.7524/j.issn.0254-6108.2019090206
Citation: ZHANG Yali, GAO Junmin, LI Chunmei, ZHOU Jie, HE Qinghua, WANG Jing, JIN Fen. Determination of tristyrylphenol ethoxylates in water by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry[J]. Environmental Chemistry, 2020, (7): 1941-1948. doi: 10.7524/j.issn.0254-6108.2019090206
shu

固相萃取-高效液相色谱-串联质谱法测定水体中三苯乙烯基苯酚聚氧乙烯醚

  • 1. 重庆大学三峡库区生态环境教育部重点实验室, 重庆, 400045;

  • 2. 农业部农产品质量安全重点实验室, 中国农业科学院农业质量标准与检测技术研究所, 北京, 100081

    • 通讯作者: 高俊敏, E-mail: gao-junmin@cqu.edu.cn ;  金芬, E-mail: jinfenbj@163.com
  • 基金项目:

    中央级公益性科研院所基本科研业务费专项（Y2017PT37），中国农业科学院"科研英才培育工程"项目，中国农业科学院创新工程项目和国家自然科学基金（21976021）资助.

Determination of tristyrylphenol ethoxylates in water by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry

  • 1. Key Laboratory of the Three Gorges Reservoir Region's Eco-Environment, Ministry of Education, Chongqing University, Chongqing, 400045, China;

  • 2. Key Laboratory of Agro-Product Quality and Safety, Institute of Quality Standard and Testing Technology for Agro-Products, Chinese Academy of Agricultural Sciences, Beijing, 100081, China

    • Corresponding authors: GAO Junmin, gao-junmin@cqu.edu.cn ;  JIN Fen, jinfenbj@163.com
  • Fund Project: Supported by the Central Public Interest Scientific Institution Basal Research (Y2017PT37),Young Talents Program and Agricultural Science,Technology Innovation Program under Chinese Academy of Agricultural Sciences and the National Natural Science Foundation of China (21976021).

  • 摘要: 本研究建立了固相萃取结合高效液相色谱-串联质谱测定水体中痕量三苯乙烯基苯酚聚氧乙烯醚（TSPEOn，n=6-29）的方法.水样经HLB柱富集，用10 mL二氯甲烷-甲醇混合溶液（1：1）洗脱，将洗脱液氮吹至近干后，用乙腈定容至0.5 mL.采用C18（2.1 mm×50 mm，5 μm）+Silica（2.1 mm×150 mm，4 μm）串联色谱柱，以乙腈和2 mmol·L-1乙酸铵水为流动相，在电喷雾正离子、多反应监测模式下对TSPEOs进行定性分析，外标法进行定量分析.结果表明，TSPEOn（n=6-29）在0.06-512.5 μg·L-1浓度范围内线性关系良好，线性相关系数在0.989-0.999之间，方法检出限为0.001-0.22 ng·L-1，定量限为0.004-0.72 ng·L-1，平均回收率在67.4%-103.3%之间，相对标准偏差为0.7%-14.8%，该方法可用于实际地表水样中痕量TSPEOn（n=6-29）的测定.
    Abstract: In this work, we developed a new method based on solid phase extraction-high performance liquid chromatography coupled with tandem mass spectrometry for analysis of trace tristyrylphenol ethoxylates (TSPEOn, n=6-29) in water. The water sample was concentrated by passing it through a HLB solid phase extraction cartridge. The HLB cartridge was eluted using 10 mL of a mixed solution of dichloromethane and methanol (1:1). The eluent was then concentrated under high-purity nitrogen, and reconstituted with acetonitrile to 0.5 mL for analysis. The separation was performed on a C18 column (2.1 mm×50 mm, 5 μm) and a Silica column (2.1 mm×150 mm, 4 μm) with a mobile phase of acetonitrile and 2 mmol·L-1 ammonium acetate aqueous solution. The TSPEOs were determined using electrospray ionization source in positive ion mode with multiple reaction monitoring. The external standard method was used for quantification. The results showed that TSPEOn (n=6-29) showed good linearity in the concentration range of 0.06-512.5 μg·L-1 with correlation coefficients of 0.989-0.999. The limits of detection were 0.001-0.22 ng·L-1, and the limits of quantification were 0.004-0.72 ng·L-1. The average recoveries of TSPEOn (n=6-29) were ranged from 67.4% to 103.3% with the relative standard deviations of 0.7%-14.8%. This method could be applied to determine trace TSPEOn (n=6-29) in surface water.
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  • 收稿日期:  2019-09-02
张雅莉, 高俊敏, 李春梅, 周杰, 贺青华, 王静, 金芬. 固相萃取-高效液相色谱-串联质谱法测定水体中三苯乙烯基苯酚聚氧乙烯醚[J]. 环境化学, 2020, (7): 1941-1948. doi: 10.7524/j.issn.0254-6108.2019090206
引用本文: 张雅莉, 高俊敏, 李春梅, 周杰, 贺青华, 王静, 金芬. 固相萃取-高效液相色谱-串联质谱法测定水体中三苯乙烯基苯酚聚氧乙烯醚[J]. 环境化学, 2020, (7): 1941-1948. doi: 10.7524/j.issn.0254-6108.2019090206
shu
ZHANG Yali, GAO Junmin, LI Chunmei, ZHOU Jie, HE Qinghua, WANG Jing, JIN Fen. Determination of tristyrylphenol ethoxylates in water by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry[J]. Environmental Chemistry, 2020, (7): 1941-1948. doi: 10.7524/j.issn.0254-6108.2019090206
Citation: ZHANG Yali, GAO Junmin, LI Chunmei, ZHOU Jie, HE Qinghua, WANG Jing, JIN Fen. Determination of tristyrylphenol ethoxylates in water by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry[J]. Environmental Chemistry, 2020, (7): 1941-1948. doi: 10.7524/j.issn.0254-6108.2019090206
shu

固相萃取-高效液相色谱-串联质谱法测定水体中三苯乙烯基苯酚聚氧乙烯醚

    通讯作者: 高俊敏, E-mail: gao-junmin@cqu.edu.cn ;  金芬, E-mail: jinfenbj@163.com
  • 1. 重庆大学三峡库区生态环境教育部重点实验室, 重庆, 400045;
  • 2. 农业部农产品质量安全重点实验室, 中国农业科学院农业质量标准与检测技术研究所, 北京, 100081
  • 收稿日期:  2019-09-02
基金项目:

中央级公益性科研院所基本科研业务费专项（Y2017PT37），中国农业科学院"科研英才培育工程"项目，中国农业科学院创新工程项目和国家自然科学基金（21976021）资助.

摘要: 本研究建立了固相萃取结合高效液相色谱-串联质谱测定水体中痕量三苯乙烯基苯酚聚氧乙烯醚（TSPEOn，n=6-29）的方法.水样经HLB柱富集，用10 mL二氯甲烷-甲醇混合溶液（1：1）洗脱，将洗脱液氮吹至近干后，用乙腈定容至0.5 mL.采用C18（2.1 mm×50 mm，5 μm）+Silica（2.1 mm×150 mm，4 μm）串联色谱柱，以乙腈和2 mmol·L-1乙酸铵水为流动相，在电喷雾正离子、多反应监测模式下对TSPEOs进行定性分析，外标法进行定量分析.结果表明，TSPEOn（n=6-29）在0.06-512.5 μg·L-1浓度范围内线性关系良好，线性相关系数在0.989-0.999之间，方法检出限为0.001-0.22 ng·L-1，定量限为0.004-0.72 ng·L-1，平均回收率在67.4%-103.3%之间，相对标准偏差为0.7%-14.8%，该方法可用于实际地表水样中痕量TSPEOn（n=6-29）的测定.

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