Abstract
A high-performance liquid chromatography (HPLC) method with relative molar sensitivity (RMS) based on 1H quantitative NMR spectroscopy (1H-qNMR) has been developed for food ingredients such as acteoside (verbascoside) and pedaliin (pedalitin-6-O-glucoside) without requiring authentic and identical standards as the reliable analytical methods. This method is used methyl 4-hydroxybenzoate (MHB) as an alternative reference standard. Each RMS is also calculated from the ratio of each analyte's molar absorption coefficient to that of MHB after correcting the purities of the analytes and reference standard by 1H-qNMR. Therefore, this method can quantify several analytes with metrological traceability to the International System of Units (SI) using the RMS and one alternative reference standard. In this study, the content of acteoside and pedaliin in several samples, such as dried sesame leaf powders and commercially processed foods, can be determined by the proposed RMS method and demonstrated in good agreement that obtained by a conventional method. Moreover, the proposed method yields analytical data with SI-traceability without the need for an authentic and identical analyte standard. Thus, the proposed RMS method is a useful and practical tool for determining acteoside and pedaliin in terms of the accuracy of quantitative values, the routine analysis, and the cost of reagents.
Highlights
It is crucial to ensure the quality and safety of food sold domestically and internationally using analytical evaluations, and there is a need to develop highly reliable analytical methods for various food-related compounds
This study reports an high-performance liquid chromatography (HPLC) method for acteoside and pedaliin with relative molar sensitivity (RMS) based on 1HqNMR that ensured the quantitative values’ reliability
Pedaliin was isolated from young sesame leaf powder and was identified by spectral analyses and comparison with reported data. 2,2-dimethyl-2-silapentane-5-sulfonate-d6 sodium salt (DSS-d6), the certified reference material, was obtained from Fujifilm Wako Pure Chemical Industries (Osaka, Japan) and was obtained from Fujifilm Wako Pure Chemical Industries (Osaka, Japan) and used as the internal standard for 1H quantitative NMR spectroscopy (1H-qNMR)
Summary
It is crucial to ensure the quality and safety of food sold domestically and internationally using analytical evaluations, and there is a need to develop highly reliable analytical methods for various food-related compounds. Quantification is commonly accomplished by purifying a sample and analyzing it with chromatographic methods such as high-performance liquid chromatography (HPLC). The sensitivity of HPLC methods depends on the molar absorption coefficient of the specific analyte. An authentic and identical analyte standard, such as certified reference material (CRM) with proven identity and purity determined by valid. Development of an LC method with relative molar sensitivity based on qNMR to determine acteoside and pedaliin supported by the Nihon University Fund for Supporting Education and Research (TO). The funder provided support in the form of salaries for TO but did not have any additional role in the study design, data collection, and analysis, decision to publish, or preparation of the manuscript
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