高效液相色谱法测定苹果酸中的其它有机酸  

Determination of other organic acids in malic acid by high performance liquid chromatography

作　　者：段先哲 李南[1,2] 谭凯旋[1] 谢焱石[1] 胡杨[1] 陈亮[1] 韩世礼[1] 冯志刚[1] 马强[1] 刘珊[1] 

机构地区：[1]南华大学,衡阳421001 [2]湖南省核燃料循环技术与装备协同创新中心,衡阳4210001

出　　处：《分析仪器》2016年第1期17-20,共4页Analytical Instrumentation

基　　金：国家自然科学基金(41503016);湖南省教育厅优秀青年项目(15B201);中国博士后科学基金(2015M582334);国防基础科研计划项目(B3720110004);南华大学博士启动基金(2014XQD08);南华大学"蒸湘学者计划"

摘　　要：建立了测定苹果酸中的马来酸与富马酸的高效液相色谱检测方法。色谱柱为磺酸基Carbomix H-NP（7.8×300mm;10μm）,流动相为0.002mol/L H2SO4,流速为0.5mL/min,进样量为50μL,检测波长为210nm,柱温为55℃。系统适用性实验中苹果酸的理论塔板数大于5000,马来酸与富马酸分别与相邻的峰分离度大于1.9,说明此方法检测苹果酸中的马来酸和富马酸灵敏度高,分离度良好。重复性实验中6份供试溶液中富马酸和马来酸含量的相对标准偏差小于3%,方法精密度良好。3种水平浓度下的加标实验中,马来酸和富马酸平均回收率都在90%~120%之间,相对标准偏差均小于4%,方法准确度良好。该方法可作为苹果酸中的马来酸与富马酸的定量分析方法。Chromatographic column was Carbomix H--NP （7.8 × 300mm, 10μm） ; the mobie phase was 0. 002mol/L H2SO4 ; the flow rate was 0. 5mL/min. ; the injection volume was 50μL; the detection wavelength was 210nm,and the column temperature was 55℃. In the system suitability experiment,the theoretical plate number of malic acid was more than 5000,the resolution of maleic and fumaric acids were greater than 1.9 ,indicating that this method had a high sensitivity and good resolution for detection of maleic and fumaric acids in malic acid. In the repeated experiment,the relative standard deviation of the concentrations of fumaric and maleic acids in 6 repeated samples was less than 3 %, showing a satisfactory precision of this method. In the spiked experiment of three levels,the average recovery of maleic and fumaric acids was between 90% and 120% ,all the relative standard deviations were less than 4%, demonstrating that this method was considerably accurate. This method can be used for quantitative determination of maleic and fumaric acids in the malic acid.

关 键 词：苹果酸 马来酸 富马酸 高效液相色谱 

分 类 号：O657.72[理学—分析化学] TQ225.1[理学—化学]