Partial least squares model and design of experiments toward the analysis of the metabolome of Jatropha gossypifolia leaves: Extraction and chromatographic fingerprint optimization

Abstract

A major challenge in metabolomic studies is how to extract and analyze an entire metabolome. So far, no single method was able to clearly complete this task in an efficient and reproducible way. In this work we proposed a sequential strategy for the extraction and chromatographic separation of metabolites from leaves Jatropha gossypifolia using a design of experiments and partial least square model. The effect of 14 different solvents on extraction process was evaluated and an optimized separation condition on liquid chromatography was estimated considering mobile phase composition and analysis time. The initial conditions of extraction using methanol and separation in 30 min between 5 and 100% water/methanol (1:1 v/v) with 0.1% of acetic acid, 20 μL sample volume, 3.0 mL min(-1) flow rate and 25°C column temperature led to 107 chromatographic peaks. After the optimization strategy using i-propanol/chloroform (1:1 v/v) for extraction, linear gradient elution of 60 min between 5 and 100% water/(acetonitrile/methanol 68:32 v/v with 0.1% of acetic acid), 30 μL sample volume, 2.0 mL min(-1) flow rate, and 30°C column temperature, we detected 140 chromatographic peaks, 30.84% more peaks compared to initial method. This is a reliable strategy using a limited number of experiments for metabolomics protocols.

Metabolomics in the Context of Plant Natural Products Research: From Sample Preparation to Metabolite Analysis

“…Coffee genotypes of three different regions in Brazil were distinguished using GC-MS coupled with statistical analysis where 44 metabolites were characterized as the chemomarkers for differentiation of the origin and genotype [241]. Design of experiments (DoE) and partial least squares (PLS) were used to prove that the physicochemical properties of the solvent have a significant effect on its extraction capacity [242]. Moreover, dereplication was used to detect bromotyrosine-derived metabolites in 14 species of sponge belonging to genus Aplysina through measuring their UV absorption using LC-photodiode array detector (PDA)-MS analysis [243].…”

Method to evaluate the quality of herbal medicines based on the dynamic changes of chemical compounds and pharmacological activity

“…PLS has gained prominence in analytical, physical, and clinical chemistry. Industrial process control can benefit from the use of this method [11][12][13].…”

Aqueous Extracts of Pericopsis angolensis and Swartzia madagascariensis with High Antimicrobial Activities against Escherichia coli O157, Shigella spp. and Salmonella enterica subsp. enterica (Serovar typhi)

“…However, the utilisation of organic solvents is often limited by a low extraction yield (Wachtel-Galor, 2004). To enhance the extraction processes, scientists have adopted protocols that use a combination of organic solvents (Pilon et al, 2016). The traditional extraction methods, relying primarily on hot or cold water, utilise fresh or dried plant materials, with the obtained extracts being administered within hours from the time of plant material collection (De Wet and Ngubane, 2014;Odunmbaku et al, 2018).…”