液相色谱法测定中药材中的富马酸单甲酯与富马酸二甲酯

Simultaneous Determination of Monomethyl Fumarate and Dimethyl Fumarate in Chinese Herbal Medicine by High Performance Liquid Chromatography

建立了同时测定中药材中富马酸单甲酯（MMF）和富马酸二甲酯（DMF）的高效液相色谱方法.样品经乙酸乙酯提取、氨基复合石墨碳固相萃取柱净化后,C18柱分离,二极管阵列检测器检测.在0.025～5.0μg/mL浓度范围内,色谱峰面积与分析物浓度呈良好线性关系,MMF和DMF的检出限（S/N=3）分别为0.015、0.020 mg/kg,定量下限（S/N=10）分别为0.05、0.06 mg/kg.当加标浓度水平为0.1、0.2、0.5mg/kg时,MMF和DMF的回收率为78.9％～97.3％,相对标准偏差（RSD,n=6）为1.7％～6.0％.方法灵敏、可靠,能够满足中药材中MMF和DMF残留检测的要求.

A high performance liquid chromatographic （HPLC） method was developed for the simultaneous determination of monomethyl fumarate （MMF）and dimethyl fumarate （DMF）in Chinese herbal medicine.Samples were extracted with ethyl acetate,purified with NH2-carb solid phase extraction column,separated with C18 column,and determined with diode army detector （DAD）.The results showed that there were good linear relationships between peak areas and concentrations of MMF and DMF in the range of 0.025-5.0 μg/mL,with limits of detection（LODs） of 0.015 and 0.020 mg/kg,and limits of quantitation （LOQs） of 0.05 mg/kg and 0.06 mg/kg,respectively.The mean recoveries of MMF and DMF at spiked levels of 0.1,0.2,0.5 mg/kg were in the range of 78.9%-97.3%,with relative standard deviations（RSDs,n =6）of 1.7%-6.0%.This method is sensitive and reliable,and could meet the requirements for simultaneous detections of MMF and DMF in Chinese herbal medicine.