色谱

色谱 ›› 2016, Vol. 34 ›› Issue (8): 795-800.DOI: 10.3724/SP.J.1123.2016.03017

• 研究论文 • 上一篇    下一篇

超高效合相色谱快速检测塑料制品中的15种邻苯二甲酸酯

李武林1,2, 李雪敏2, 李根容1, 李沿飞1, 徐溢2, 李泽全2   

  1. 1. 重庆市计量质量检测研究院, 重庆 401123;
    2. 重庆大学化学化工学院, 重庆 400030
  • 收稿日期:2016-03-14 出版日期:2016-08-08 发布日期:2016-07-26
  • 通讯作者: 李武林
  • 基金资助:

    重庆市社会民生科技创新专项（cstc2015shmszx00015）.

Determination of 15 phthalate esters in plastic products by ultra performance convergence chromatography

LI Wulin1,2, LI Xuemin2, LI Genrong1, LI Yanfei1, XU Yi2, LI Zequan2   

  1. 1. Chongqing Academy of Metrology and Quality Inspection, Chongqing 401123, China;
    2. College of Chemistry and Chemical Engineering, Chongqing University, Chongqing 400030, China
  • Received:2016-03-14 Online:2016-08-08 Published:2016-07-26
  • Supported by:

    Science and Technology Innovation Project for Social Livelihood of Chongqing (No. cstc2015shmszx00015).

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被引次数

15

摘要：

建立了使用超高效合相色谱检测塑料中15种邻苯二甲酸酯的方法。样品经正己烷超声萃取，过0.45 μ m有机膜后上机测试。采用ACQUITY UPC2 HSS C18 SB色谱柱（150 mm×3 mm, 1.8 μ m），以超临界CO2流体为主流动相、乙腈为流动相改性剂进行梯度洗脱，流速为1.5 mL/min。在系统背压为12.41 MPa、色谱柱温度为65 ℃、二极管阵列检测器（PDA）检测波长为220 nm的条件下，15种邻苯二甲酸酯可以在8 min内实现分离检测。实验结果表明：15种邻苯二甲酸酯的线性范围为0.5~10 mg/L，相关系数大于0.9960，检出限（S/N=3）为1.0~2.2 mg/kg，加标回收率为78.1%~122.3%，相对标准偏差为2.95%~8.26%。该方法分析速度快，为邻苯二甲酸酯类物质的检测提供了新的选择。

关键词: 超高效合相色谱, 二极管阵列检测器, 邻苯二甲酸酯, 塑料

Abstract:

Ultra performance convergence chromatography (UPC2) is cost effective, sustainable, and it uses green technology that lowers the use of organic solvents. Based on these advantages, a method was developed for the determination of 15 phthalate esters in plastic products by UPC2. The samples were extracted with hexane and then quantitatively analyzed by UPC2. The separation of the 15 phthalate esters was achieved on an ACQUITY UPC2 HSS C18 SB column (150 mm×3 mm, 1.8 μ m) by a gradient elution with supercritical CO2 and acetonitrile as mobile phases. External standard method was used for the quantitative determination and the calibration curves showed good linearity in the concentration range of 0.5-10 mg/L for the phthalate esters with correlation coefficients higher than 0.9960. The limits of quantification of the phthalate esters were 1.0-2.2 mg/kg. Their spiked recoveries were 78.1%-122.3%, and the relative standard deviation range was from 2.95% to 8.26%. The method can be successfully applied for the determination of the phthalate esters in plastic products.

Key words: photodiode array detector (PDA), phthalate esters (PAEs), plastic, ultra performance convergence chromatography (UPC2)

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