Development of an HPLC method with relative molar sensitivity based on 1H-qNMR to determine acteoside and pedaliin in dried sesame leaf powders and processed foods

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.

Study on the Synthesis of Methylated Reference and Their Application in the Quantity of Curcuminoids Using Single Reference Liquid Chromatography Based on Relative Molar Sensitivity

“…20,21) Indeed, for catechins, the flavonoid structure strongly interacted with the C 18 polymers of the column; thus, altering specific functional groups was challenging at a similar retention time. 16) We speculated that at the same wavelength, a change in the polarity-sensitive retention is observed, leading to good separation and suitable retention time. Thus, a novel approach is attempted to make the MR for retaining the key structure of Curs.…”

“…13) Single reference (SR)-LC assay based on relative molar sensitivity (RMS) is a recently applied method for the quantitative determination of natural compounds in various food materials. [14][15][16][17] Each natural analyte could be quantitated according its intensity ratio with SR coefficient on a one-running chromatogram. 18) Compare to conventional LC evaluation, SR-LC assay demonstrates that the calibration analysis of RMS using 1 H-quantitative nuclear magnetic resonance spectroscopy (qNMR) is a simple and reliable quantification that does not require these certified references.…”

Chemometric-Guided Approaches for Profiling and Authenticating Botanical Materials

“…These targeted compounds are analyzed by a chemical methodology and compared against reference standards and literature values; common analytical techniques include charged aerosol detection (CAD), ultraviolet-visible (UV/VIS) spectrophotometry, and mass spectrometry (MS), often with chromatographic separation beforehand (liquid chromatography, "LC", or gas chromatography, "GC" being the two primary forms). Nuclear magnetic resonance (NMR) is an analytical technique that has become more quantitative recently (qNMR) to facilitate comparisons between complex botanical samples (34)(35)(36).…”

Miroestrol Quantification in <i>Pueraria mirifica</i> Crude Drugs and Products by Single-Reference UPLC/PDA/MS Using Relative Molar Sensitivities to Kwakhurin

“…Recently, Sugimoto and colleagues have developed a singlereference HPLC method with relative molar sensitivity (RMS) determined by off-line combination of 1 H-quantitaive NMR ( 1 H-qNMR) and LC/photo diode array (PDA) for quantitative analysis of analytes in natural products. [12][13][14][15][16] A single reference standard is used as an internal standard in the 1 H-qNMR and HPLC methods to calculate the RMS values of each tar-geted analyte in various samples. These values can be determined as analyte-specific factors from the response ratios obtained by HPLC and the molar ratios obtained by 1 H-qNMR.…”