色谱

色谱 ›› 2018, Vol. 36 ›› Issue (7): 678-684.DOI: 10.3724/SP.J.1123.2018.01014

• 研究论文 • 上一篇    下一篇

超临界流体色谱同时测定运动饮料中的8种邻苯二甲酸酯类增塑剂

韦俊芳1, 姜磊2, 楼超艳3, 朱岩3   

  1. 1. 浙江大学公共体育与艺术部, 浙江 杭州 310000;
    2. 浙江省纺织测试研究院, 浙江 杭州 310013;
    3. 浙江大学化学系, 浙江 杭州 310000
  • 收稿日期:2018-01-09 出版日期:2018-07-08 发布日期:2014-06-03
  • 通讯作者: 楼超艳,E-mail:11437039@zju.edu.cn;朱岩,E-mail:zhuyan@zju.edu.cn

Simultaneous determination of eight phthalate ester plasticizers in sports beverages using supercritical fluid chromatography

WEI Junfang1, JIANG Lei2, LOU Chaoyan3, ZHU Yan3   

  1. 1. Department of Public Physical Art Education, Zhejiang University, Hangzhou 310000, China;
    2. Zhejiang Textile Testing Research Institute, Hangzhou 310013, China;
    3. Department of Chemistry, Zhejiang University, Hangzhou 310000, China
  • Received:2018-01-09 Online:2018-07-08 Published:2014-06-03

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摘要：

建立了同时快速测定运动饮料中邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二丙酯、邻苯二甲酸二丁酯、邻苯二甲酸二戊酯、邻苯二甲酸丁基苄基酯、邻苯二甲酸二（2-乙基己基）酯、邻苯二甲酸二辛酯8种邻苯二甲酸酯（PAEs）类增塑剂的超临界流体色谱-紫外检测分析方法。实际样品经液相萃取后，用超临界流体色谱分析，以超临界态二氧化碳-3%（体积分数）甲醇作为色谱流动相进行等度洗脱，检测波长为225 nm，6 min即可实现分离。8种PAE类增塑剂在0.05~25 mg/L范围内均具有良好的线性关系，相关系数为0.9991~0.9997，方法检出限为7.5~15 μg/L。8种PAE类增塑剂在运动饮料样品中的加标回收率为91.7%~100.2%，相对标准偏差均不大于6.5%（n=3）。应用该方法对多种市售运动饮料中的8种PAE类增塑剂进行检测，结果表明，该方法环保、快速、灵敏、选择性高、结果准确，能满足运动饮料中增塑剂含量检测的要求。

关键词: 超临界流体色谱, 邻苯二甲酸酯, 液相萃取, 运动饮料, 增塑剂

Abstract:

Phthalate esters (PAEs) are a group of serious environmental pollutants that are carcinogenic or tumorigenic to humans. In this work, a green, rapid, and effective analytical method based on supercritical fluid chromatography (SFC) has been proposed for the simultaneous determination of the eight PAE plasticizers in sports beverage samples. They are dimethyl phthalate (DMP), diethyl phthalate (DEP), dipropyl phthalate (DPRP), dibutyl phthalate (DBP), dipentyl phthalate (DPP), benzyl butyl phthalate (BBP), di-2-ethylhexyl phthalate (DEHP), and di-n-octyl phthalate (DNOP). Liquid phase extraction (LPE) was employed to extract the PAE plasticizers before testing using SFC with ultraviolet (UV) detection. SFC parameters, including stationary phase screening, modifier composition and volume percentage, column temperature, flow rate, and backpressure, were optimized. Under the optimum conditions, all the eight PAE plasticizers could be determined simultaneously by SFC within 6 min at 225 nm. The optimized eluent was supercritical CO2 with 3% (v/v) methanol. The performance of the developed method was also evaluated. The eight PAE plasticizers exhibited satisfactory linearities with correlation coefficients (r) of 0.9991-0.9997 in the range of 0.05-25 mg/L. The limits of detection ranged from 7.5 to 15 μg/L (S/N=3, n=3). Recoveries of all the PAE plasticizers for the spiked samples ranged from 91.7%-100.2% with relative standard deviations of no more than 6.5% (n=3). This method is green, time-saving, simple, selective, robust, and convenient for the analysis of the eight PAE plasticizers in real sports beverage samples.

Key words: liquid phase extraction(LPE), phthalate esters(PAEs), plasticizer, sports beverages, supercritical fluid chromatography(SFC)

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