加压毛细管电色谱测定糕点中富马酸二甲酯
Determination of dimethyl fumarate in pastry by pressurized capillary electro-chromatography
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摘要: 建立了利用加压毛细管电色谱(pCEC)测定糕点中富马酸二甲酯(DMF)的分析方法。样品采用甲醇超声提取,提取液经反相毛细管电色谱柱分离,流动相乙腈-水(3∶7,v/v),泵流速0.05mL/min,分离电压-5kV,紫外检测器检测。该方法在2.0100mg/kg质量浓度范围内线性关系良好(r2=0.9998),定量限为20mg/kg,加标回收率为85.5%93.6%,相对标准偏差小于5%。该方法操作简单、快速,准确可靠,为糕点中富马酸二甲酯的检测提供了新的技术手段。Abstract: An effective and convenient method for determination of dimethyl fumarate ( DMF) in pastry by pressurized capillary electro-chromatography (pCEC) with ultra-violet detection was developed. The samples were extracted with methanol. The separation was performed on a reversed phase C18column in an isocratic mode with 220nm as the UV detection wavelength. The effects of ratio of organic phase and separation voltage on separation efficiency were optimized. The mobile phase was composed of acetonitrile and water (3∶7, v/v) , at a pump flow rate of 0.05mL/min. Under the optimal conditions, the linear range of DMF was 2.0100mg/kg with correlation coefficient higher than 0.9998. The mean recoveries were 85.5%93.6% and the relative standard deviations (RSD) were less than 5%.