超高效超临界色谱分析聚合物制品中的7种添加剂  

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

作　　者：张云[1] 杜振霞[1] 于文莲 

机构地区：[1]北京化工大学掌分析测试中心,北京100029 [2]中国检验检检疫科学研究院,北京100025

出　　处：《色谱》2014年第1期52-56,共5页Chinese Journal of Chromatography

基　　金：国家级质检公益性行业科研专项项目(201110020)

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220nm条件下，通过考察样品的稀释溶剂、流动相添加剂、柱温、背膻、杞流速对分离的影响，最终确定7种添加剂分离的最优化条件：采用正已烷／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2mL／min，柱温50℃，背压12．41～13．79MPa条件下，7种聚合物添加剂能够在5rain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。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 tile important parameters of UPSFC, such as the diluting solvent, mobile phase addi- tive, colunm 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 （l/l, 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 rain, and full baseline separation was achieved. The real sample was pretreated by microwave-assis- ted extraction （MAE） and analyzed by UPSFC-PDA. The seven additives can be detected with the recoveries of 59.9% - 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.

关 键 词：超高效超临界色谱 二极管阵列检测器 添加剂 聚合物制品 

分 类 号：O658[理学—分析化学]