正相高效液相色谱法测定L-苹果酸中的对映异构体D-苹果酸  

Determination of enantiomer D-malic acid in L-malic acid by normal-phase high performance liquid chromatography

作　　者：段先哲 李南[1,2] 谭凯旋[1] 谢焱石[1] 陈亮[1] 胡杨[1] 冯志刚[1] 韩世礼[1] 马强[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421001

出　　处：《分析仪器》2016年第2期25-29,共5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);南华大学博士启动基金(2014XQD08);南华大学"蒸湘学者计划";国防基础科研计划项目(B3720110004)

摘　　要：建立了测定L-苹果酸中对映异构体D-苹果酸的的正相高效液相色谱检测方法。色谱柱为手性色谱柱CHIRALPAK-IC(4.6×250mm;5μm),流动相为正己烷∶异丙醇∶三氟乙酸=80∶20∶0.1,流速为0.5mL/min,进样量为100μL,检测波长为210nm,柱温为35℃。系统适用性实验中L-苹果酸和D-苹果酸的理论塔板数大于5000,L-苹果酸与相邻峰的分离度为2.6,D-苹果酸与相邻峰的分离度为2.9。此方法检测L-苹果酸中的D-苹果酸敏度高,分离度良好。溶液稳定性实验中,在24小时内测定D-苹果酸含量的相对标准偏差为5.78%,溶液在24小时内稳定性良好。精密度实验中6次重复进样D-苹果酸含量的相对标准偏差为3.59%,精密度良好。L-苹果酸的检出限为0.22ng。该方法可用于分离L-苹果酸及其对映异构体D-苹果酸。The chromatographic column was CHIRALPAK-IC（4.6×250mm;5um）;the mobie phase was N-hexane∶isopropyl alcohol∶trifluoroacetic acid（80：20：0.1）,the flow rate was 0.5ml/min,the injection volume was 100μL,the detection wavelength was at 210 nm,and the column temperature was35℃.In the suitability experiment,the theoretical plate number of L-malic and D-malic acids were more than 5000,the resolution between L-malic acid and its adjacent peak was 2.6,and the resolution between D-malic acid and its adjacent peak was 2.9,indicating that this method had a high sensitivity and good resolution.In the solution stability experiment,the relative standard deviation of D-malic acid concentration was 5.78% within 24 hours,demonstrating that the solution was stable within 24 hours.In the precision experiment,the relative standard deviation of the D-malic acid concentrations in six repeated sampling was3.59%,showing a satisfactory precision of this method.The detection limit of L-malic acid was 0.22 ng.This method could be used for quantitative determination of D-malic acid in the L-malic acid.

关 键 词：L-苹果酸 对映异构体 D-苹果酸 正相高效液相色谱法 

分 类 号：O657.72[理学—分析化学] TS202.3[理学—化学]