不同食品中富马酸二甲酯的高效液相色谱分析方法研究

Study on the Determination of Dimethyl Fumarate in Different Food by Liquid Chromatography

用反相高效液相色谱法测定食品中防霉剂富马酸二甲酯,建立了不同基质样品的前处理方法。水果、饮料等样品经沉淀、离心、甲醇超声提取后直接测定;对不易分散的肉制品及油脂含量高的糕点采用中性氧化铝作分散剂和脱水剂,乙腈超声提取后用正己烷脱脂净化。采用Inertsil ODS-sp C18柱分离,二极管阵列检测器于波长220 nm处检测。结果表明,该方法处理的样品干净,无杂峰干扰。富马酸二甲酯在0～20μg/mL范围内线性关系良好,相关系数r大于0.999 5,检出限(LOD)0.02 mg/kg(信噪比S/N=3)。在不同样品中平均加标回收率在82.3%～104.8%范围内,相对标准偏差为0.87%～2.34%(n=6)。该方法简便、准确、有效,可用于不同食品中富马酸二甲酯的测定。

Abstract A reverse phase high-performance liquid chromatography method has been developed to determin dimethyl fumarate in food and different methods for sample preparation were established. For the samples with simple ground substance such as fruit and drink, the dimethyl fumarate was extracted with methyl alcohol after precipitate and centrifugation. The samples which difficult to disperse such as meat product and cookie with high content fat were dispersed and dehydrated by neutral alumina and extracted with acetonitrile, and then defatted by n-hexane hexyl hydride. The extracts were separated on reversed-phase Inertsil ODS-sp C18 column （4.6 mmx250 mm, 5 lam） and detected at the wavelength of 220 nm by diode array detector. Dimethyl fumarate has good linearity in the range of 0~20.0 lag/mL, the correlation coefficients is above 0.999 5 and the detection limits of 6 limited materials is 0.02 mg/kg （S/N=3）. The average recovery rates in different food were between 82.3% and 104.8%. The relative standard deviations （RSDs） of spiked samples varied from 0.87% to 2.34% （n=6）. This method is simple, accurate and efficient and suitable for analysis of dimethyl fumarate in different food.