在线固相萃取-液相色谱法同时测定米粉中4种维生素E的含量

Simultaneous determination of 4 vitamins E in rice flour by online solid phase extraction combined with liquid chromatography

本文采用在线固相萃取-液相色谱技术同时检测米粉中4种维生素E(α、β、γ、δ-维生素E)的含量。主要过程是样品皂化处理后,经过在线固相萃取小柱自动完成维生素E的富集和净化,利用液相色谱自动完成4种维生素E的定量分析测定。考察了不同填料固相萃取柱以及液相色谱柱对于4种维生素E的净化分离效果,最终选取PLRP-S柱作为在线固相萃取柱,Poroshell 120 PFP柱作为液相分析柱。结果表明,4种维生素E在1.0-50μg/mL范围内均线性良好,相关系数R 2均大于0.995,平均回收率在91.2%-102.0%之间,相对标准偏差为1.69%-4.58%(n=6)。该方法利用固相萃取净化分离维生素E,并将其与液相色谱仪在线耦合,实现了前处理过程自动化,减少了人工操作,提高了结果准确性,适用于米粉中4种维生素E的测定。

In this paper,a method for rapid determination of vitamin E(α,β,γ,δ-vitamin E)in rice flour is established by on-line solid phase extraction combined with liquid chromatography.After saponification of the sample,the enrichment and purification of vitamin E are automatically completed by online solid phase extraction column,and the quantitative analysis and determination of four kinds of vitamin E are automatically completed by liquid chromatography.In this paper,the purification and separation effects of four vitamin E are investigated on solid-phase extraction columns and liquid chromatography columns with different fillers.Finally,PLRP-S column is selected as online solid-phase extraction column and Poroshell 120 PFP column is selected as liquid analysis column.The results show that the four kinds of vitamin E have good linearity in the range of 1.0~50μg/mL,the correlation coefficient R^(2) are all greater than 0.995,the average recovery rate is between 91.2%and 102.0%,and the relative standard deviation is between 1.69%and 4.58%(n=6).Vitamin E is separated by solid phase extraction clean-up and coupled with a liquid chromatograph online in this method,which realizes the automation of pretreatment process,reduces manual operation,improves the accuracy of results and detection efficiency,and is suitable for the determination of four vitamins in rice flour.