首页> 中文期刊> 《色谱》 >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

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

         

摘要

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 simulta-neous 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 CO2with 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 0.999 1-0.999 7 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.%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 0.999 1~0.999 7,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.

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