Premium
Design of synthetic single reference standards for the simultaneous determination of sesamin, sesamolin, episesamin, and sesamol by HPLC using relative molar sensitivity
Author(s) -
Takahashi Miki,
Nishizaki Yuzo,
Morimoto Koji,
Sugimoto Naoki,
Sato Kyoko,
Inoue Koichi
Publication year - 2018
Publication title -
separation science plus
Language(s) - English
Resource type - Journals
ISSN - 2573-1815
DOI - 10.1002/sscp.201800081
Subject(s) - sesamin , sesamol , analyte , chemistry , high performance liquid chromatography , chromatography , calibration curve , analytical chemistry (journal) , detection limit , organic chemistry , food science , antioxidant
A single reference standard can be used as an internal standard for both quantitative proton NMR spectroscopy and high‐performance liquid chromatography to estimate the relative molar sensitivity for a simultaneous determination of multiple analytes. However, we find it difficult to choose a candidate single reference standard from currently existing compounds. The present work aims to design and synthesize idealized single reference standards for the simultaneous determination of sesamin, sesamolin, episesamin and sesamol by high‐performance liquid chromatography using relative molar sensitivity. These analytes all contain a 1,3‐benzodioxole derivative that has an absorption wavelength near 290 nm. Using this core structure, piperoanol and synthetic methyl, butyl and hexyl sesamol derivatives were evaluated by quantitative proton NMR spectroscopy. The purities of these candidate single reference standards were higher than 97.0%. The relative molar sensitivity of the analyte was calculated from slope ratios of the calibration curves (three ranges from 0 to 100 mM, r 2 = 0.999). The averaged relative molar sensitivity values of the analytes and other single reference standards ranged from 0.73 ± 0.01 to 2.26 ± 0.01. Using these relative molar sensitivity values, the concentrations of sesamin, sesamolin, episesamin and sesamol in sesame oil, health foods, and food additives could be evaluated by high‐performance liquid chromatography within the expanded uncertainty. This approach for the design of single reference standards based on structural information can be applied for the simultaneous determination of similar chemical compositions where native standards do not yet exist.