色谱

色谱 ›› 2014, Vol. 32 ›› Issue (1): 52-56.DOI: 10.3724/SP.J.1123.2013.08036

• 研究论文 • 上一篇    下一篇

超高效超临界色谱分析聚合物制品中的7种添加剂

张云1, 杜振霞1, 于文莲2   

  1. 1. 北京化工大学分析测试中心, 北京 100029;
    2. 中国检验检疫科学研究院, 北京 100025
  • 收稿日期:2013-08-23 修回日期:2013-11-04 出版日期:2014-01-08 发布日期:2013-12-26
  • 通讯作者: 杜振霞
  • 基金资助:

    国家级质检公益性行业科研专项项目(201110020).

Determination of seven additives in polymer products by ultra performance supercritical fluid chromatography

ZHANG Yun1, DU Zhenxia1, YU Wenlian2   

  1. 1. Analysis and Testing Center of Beijing University of Chemical Technology, Beijing 100029, China;
    2. Chinese Academy of Inspection and Quarantine, Beijing 100025, China
  • Received:2013-08-23 Revised:2013-11-04 Online:2014-01-08 Published:2013-12-26

PDF

140

被引次数

18

摘要：

采用超高效超临界色谱(UPSFC)-二极管阵列检测器(PDA)建立了快速分析高分子材料中7种常用聚合物添加剂的方法。在检测波长为220 nm条件下，通过考察样品的稀释溶剂、流动相添加剂、柱温、背压、柱流速对分离的影响，最终确定7种添加剂分离的最优化条件：采用正己烷/异丙醇(1/1，v/v)为稀释溶剂，流动相添加剂为甲醇/乙腈(1/1，v/v)，流速2 mL/min，柱温50 ℃，背压12.41~13.79 MPa条件下，7种聚合物添加剂能够在5 min之内达到完全基线分离。利用微波辅助萃取方法对实际样品中的添加剂进行提取，经UPSFC-PDA分析，7种添加剂的回收率为69.9%~118.9%，相对标准偏差(RSD，n=9)低于10%。该方法简便、快速，选择性强，能够准确快速地分析聚合物制品中的添加剂。

关键词: 超高效超临界色谱, 二极管阵列检测器, 聚合物制品, 添加剂

Abstract:

A method for rapid determination of seven commonly used additives in polymer products by ultra performance supercritical fluid chromatography (UPSFC)-photodiode array detector (PDA) was developed. In this experiment, the detection wavelength was set at 220 nm. After the important parameters of UPSFC, such as the diluting solvent, mobile phase additive, column temperature, automatic back pressure regulator (ABPR) and flow rate were investigated, the optimized conditions were acquired as follows: n-hexane/isopropanol (1/1, v/v) was chosen as the diluting solvent, the mixture of methanol/acetonitrile (1/1, v/v) as the mobile phase additive, 2 mL/min as the flow rate, 50 ℃ as the column temperature, 12.41-13.79 MPa as the ABPR. Under these conditions, seven additives were separated in 5 min, and full baseline separation was achieved. The real sample was pretreated by microwave-assisted extraction (MAE) and analyzed by UPSFC-PDA. The seven additives can be detected with the recoveries of 69.9%-118.9%, and the relative standard deviations (RSDs, n=9) were less than 10%. This method is simple, fast with good selectivity and suitable for the analysis of the additives in polymer products.

Key words: additives, photodiode array detector (PDA), polymer products, ultra performance supercritical fluid chromatography (UPSFC)

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