Two Ways to Achieve the Same Goal—Two Validated Quantitative NMR Strategies for a Low-Abundance Natural Product in Standardized Extracts: The Case of Hepatodamianol in ITurnera diffusa/I

The quantification of low-abundance secondary metabolites in plant extracts is an analytical problem that can be addressed by different analytical platforms, the most common being those based on chromatographic methods coupled to a high-sensitivity detection system. However, in recent years nuclear...

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Published inMolecules (Basel, Switzerland) Vol. 27; no. 19
Main Authors Parra-Naranjo, Aída, Delgado-Montemayor, Cecilia, Salazar-Aranda, Ricardo, Castro-Ríos, Rocío, Saucedo, Alma L, Waksman-Minsky, Noemí
Format Journal Article
LanguageEnglish
Published MDPI AG 01.10.2022
Subjects
Analysis
Biological products
Chromatography
Health aspects
Metabolites
Nuclear magnetic resonance
Mexico
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Summary:The quantification of low-abundance secondary metabolites in plant extracts is an analytical problem that can be addressed by different analytical platforms, the most common being those based on chromatographic methods coupled to a high-sensitivity detection system. However, in recent years nuclear magnetic resonance (NMR) has become an analytical tool of primary choice for this type of problem because of its reliability, inherent simplicity in sample preparation, reduced analysis time, and low solvent consumption. The versatility of strategies based on quantitative NMR (qNMR), such as internal and external standards and electronic references, among others, and the need to develop validated analytical methods make it essential to compare procedures that must rigorously satisfy the analytical well-established acceptance criteria for method validation. In this work, two qNMR methods were developed for the quantification of hepatodamianol, a bioactive component of T. diffusa. The first method was based on a conventional external standard calibration, and the second one was based on the pulse length-based concentration determination (PULCON) method using the ERETIC2 module as a quantitation tool available in TopSpin software. The results show that both procedures allow the content of the analyte of interest in a complex matrix to be determined in a satisfactory way, under strict analytical criteria. In addition, ERETIC2 offers additional advantages such as a reduction in experimental time, reagent consumption, and waste generated.
ISSN:1420-3049
1420-3049
DOI:10.3390/molecules27196593