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

Autor(es)

Pilon, Alan Cesar ^[1] ; Neto, Fausto Carnevale ^[1] ; Freire, Rafael Teixeira ^[1] ; Cardoso, Patricia ^[1] ; Carneiro, Renato Lajarim ^[2] ; Bolzani, Vanderlan Da Silva ^[1] ; Castro-Gamboa, Ian ^[1]

Afiliação do(s) autor(es)

^[1] UNESP, Inst Chem, Dept Organ Chem, Biosynth & Ecophysiol Nat Prod NuBBE, Nucleus Bioa, Rua Prof Francisco Degni 55 CP 355, BR-14800900 Araraquara, SP - Brazil

^[2] Sao Carlos Fed Univ UFSCar, CCET, Dept Chem, Rodovia Washington Luiz, Sao Carlos, SP - Brazil

• Tipo de documento: Artigo Científico
• Fonte: JOURNAL OF SEPARATION SCIENCE; v. 39, n. 6, p. 1023-1030, MAR 2016.
• Citações Web of Science: 5

Resumo

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 L sample volume, 3.0 mL min(-1) flow rate and 25 degrees 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 L sample volume, 2.0 mL min(-1) flow rate, and 30 degrees 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. (AU)

• Processo FAPESP: 10/17935-4 - Desenvolvimento de métodos analíticos de desreplicação por RMN e análise multivariada do perfil metabolômico de espécies de Solanaceae com potencial biológico.
• Beneficiário: Alan Cesar Pilon
• Modalidade de apoio: Bolsas no Brasil - Doutorado
• Processo FAPESP: 13/07600-3 - CIBFar - Centro de Inovação em Biodiversidade e Fármacos
• Beneficiário: Glaucius Oliva
• Modalidade de apoio: Auxílio à Pesquisa - Centros de Pesquisa, Inovação e Difusão - CEPIDs
• Processo FAPESP: 11/50816-1 - A rizosfera de Senna spectabilis: estudo das interações planta/microrganismos utilizando ferramentas metabolômicas
• Beneficiário: Ian Castro-Gamboa
• Modalidade de apoio: Auxílio à Pesquisa - Programa BIOTA - Regular