Determination of L-norvaline and L-tryptophan in dietary supplements by nano-LC using an O-[2-(methacryloyloxy)-ethylcarbamoyl]-10,11- dihydroquinidine-silica hybrid monolithic column  

作　　者：Dongsheng Xu Elena Sanchez-Lopez Qiqin Wang Zhengjin Jiang María Luisa Marina 

机构地区：[1]Departamento de Química Analítica,Química Física e Ingeniería Química,Universidad de Alcala,Ctra.Madrid-Barcelona Km.33.600,28871,Alcala de Henares(Madrid),Spain [2]Institute of Pharmaceutical Analysis,College of Pharmacy,Jinan University,Guangzhou,510632,China [3]Department of Pharmacy and Guangdong Province Key Laboratory of Pharmacodynamic Constituents of Traditional Chinese Medicine&New Drug Research,Jinan University,Guangzhou,510632,China [4]Instituto de Investigacion Química“Andres M.del Río”(IQAR),Universidad de Alcala,Ctra.Madrid-Barcelona Km.33.600,28871,Alcala de Henares(Madrid),Spain

出　　处：《Journal of Pharmaceutical Analysis》2020年第1期70-77,共8页药物分析学报（英文版）

摘　　要：An analytical methodology based on an O-[2-(methacryloyloxy)-ethylcarbamoyl]-10,11-dihydroquinidine(MQD)-silica hybrid monolithic column was developed for the enantioseparation of 9-fluorenylmethoxycarbonyl(FMOC)derivatized amino acids by nano-liquid chromatography.The mobile phase was optimized including the apparent pH,content of ACN,and concentration of the buffer to obtain a satisfactory enantioresolution performance.27 FMOC derivatized amino acids including 19 protein and 8 non-protein amino acids were tested,and 19 out of them were enantiomerically discriminated obtaining baseline separation for 11 of them.Analytical characteristics of the method were evaluated for norvaline and tryptophan in terms of linearity,precision,accuracy,limits of detection(LOD)and quantitation(LOQ)showing good performance to be applied to the enantiomeric determination of these amino acids in dietary supplements.LOD and LOQ values were 9.3 and 31 mM for norvaline enantiomers and 7.5 and 25 mM for tryptophan enantiomers,respectively.The contents of D-norvaline and D-tryptophan were below their respective LODs in all the analyzed samples.Quantitation of L-tryptophan and L-norvaline showed good agreement with the labeled contents except for one sample which did not show presence of L-norvaline,contrary to the label indication.

关 键 词：9-Fluorenylmethoxycarbonyl Amino acids Chiral separation NANO-LC Quinidine-silica hybrid monolithic column 

分 类 号：R927[医药卫生—药学]