UPLC-QTOF-MSE based metabolomics and chemometrics study of the pitaya processing.

The search for knowledge related to the Pitaya (Hylocereus polyrhizus [F.A.C. Weber] Britton & Rose, family Cactaceae) is commonly due to its beneficial health properties e aesthetic values. But process to obtain pitaya pulp is a first and important step in providing information for the subsequent use of this fruit as colorant, for example. Therefore, the effects of the pulping process on the metabolomic and chemometric profile of non-volatile compounds of pitaya were assessed for the first time. The differences in metabolic fingerprints using UPLC-QTOF-MSE and multivariate modeling (PCA and OPLS-DA) was performed in the following treatments: treatment A, which consists of pelled pitaya and no ascorbic acid addition during pulping; treatment B, use of unpelled pitaya added of ascorbic acid during pulping; and control, unpelled pitaya and no ascorbic acid addition during pulping. For the metabolomic analysis, UPLC-QTOF-MSE shows an efficient method for the simultaneous determination of 35 non-volatile pitaya metabolites, including isorhamnetin glucosyl rhamnosyl isomers, phyllocactin isomers, 2'-O-apiosyl-phylocactin and 4'-O-malonyl-betanin. In addition, the chemometric analysis efficiently distinguished the metabolic compounds of each treatment applied and shows that the use of unpelled pitaya added of ascorbic acid during pulping has an interesting chemical profile due to the preservation or formation of compounds, such as those derived from betalain, and higher yields, which is desirable for the food industry.

Metabolomic approaches to explore chemodiversity in seeds of guaraná (Paullinia cupana) using UPLC-QTOF-MSE and NMR analysis.

The growing interest in health and well-being has spurred the evolution of functional foods, which provide enhanced health benefits beyond basic nutrition. Guaraná seeds (Paullinia cupana) have been widely studied and used as a functional food due to their richness in caffeine, phenolic compounds, amino acids, and other nutrients. This has established guaraná as a significant food supplement, with Brazil being the largest producer of the world. This study aims to propose a set of analytical methods to chemically evaluate fifty-six different guaraná clones, from the Guaraná Germplasm Active Bank, to accommodate the diverse requirements of the food industry. Metabolomic approaches were employed, in which a non-target metabolomic analysis via UPLC-QTOF-MSE led to the annotation of nineteen specialized metabolites. Furthermore, targeted metabolomics was also used, leading to the identification and quantification of metabolites by NMR. The extensive data generated were subjected to multivariate analysis, elucidating the similarities and differences between the evaluated guaraná seeds, particularly concerning the varying concentration levels of the metabolites. The metabolomics approach based on the combination of UPLC-QTOF-MSE, NMR and chemometric tools provided sensitivity, precision and accuracy to establish the chemical profiles of guaraná seeds. In conclusion, evaluating and determining the metabolic specificities of different guarana clones allow for their application in the development of products with different levels of specific metabolites, such as caffeine. This caters to various purposes within the food industry. Moreover, the recognized pharmacological properties of the annotated specialized metabolites affirm the use of guarana clones as an excellent nutritional source.

Metabolomic Profile of Volatile Organic Compounds from Leaves of Cashew Clones by HS-SPME/GC-MS for the Identification of Candidates for Anthracnose Resistance Markers.

Anthracnose caused by Colletotrichum gloeosporioides affects the leaves, inflorescences, nuts, and peduncles of cashew trees (Anacardium occidentale). The use of genetically improved plants and the insertion of dwarf cashew clones that are more resistant to phytopathogens are strategies to minimize the impact of anthracnose on cashew production. However, resistance mechanisms related to the biosynthesis of secondary metabolites remain unknown. Thus, this study promoted the investigation of the profile of volatile organic compounds of resistant cashew clone leaves ('CCP 76', 'BRS 226' and 'BRS 189') and susceptible ('BRS 265') to C. gloeosporioides, in the periods of non-infection and infection of the pathogen in the field (July-December 2019 - Brazil). Seventy-eight compounds were provisionally identified. Chemometric analyses, such as Principal Component Analysis (PCA), Discriminating Partial Least Squares Analysis (PLS-DA), Discriminating Analysis of Orthogonal Partial Least Squares (OPLS-DA), and Hierarchical Cluster Analysis (HCA), separated the samples into different groups, highlighting hexanal, (E)-hex-2-enal, (Z)-hex-2-en-1-ol, (E)-hex-3-en-1-ol, in addition to α-pinene, α-terpinene, γ-terpinene, ß-pinene, and δ-3-carene, in the samples of the resistant clones in comparison to the susceptible clone. According to the literature, these metabolites have antimicrobial activity and are therefore chemical marker candidates for resistance to C. gloeosporioides in cashew trees.

Antagonism of volatile organic compounds of the Bacillus sp. against Fusarium kalimantanense.

Fusarium kalimantanense is a genetic lineage of Fusarium oxysporum f. sp. cubense (Foc) and belongs to the Fusarium oxysporum species complex (FOSC). This pathogen is a causative agent of Panama disease, an infection that has caused damage to the banana crop worldwide. Bacillus sp. (LPPC170) showed preliminary antagonist activity against F. kalimantanense (LPPC130) in vitro tests from the cultivation of axenic culture and co-culture with inhibition of mycelial growth of phytopathogen of 41.23%. According to these findings, volatile organic compounds (VOCs) emitted from Bacillus sp. were obtained by solid-phase microextraction and identified by gas chromatography coupled with a mass spectrometer (GC-MS). The multivariate data analysis tool (PLS-DA and Heatmap) identified short-chain organic acids as the main antagonistic VOCs responsible for inhibiting the mycelial growth of LPPC130. Acetic acid, propanoic acid, butanoic acid, valeric acid, and isovaleric acid exhibited a strong inhibitory effect on the mycelial growth of LPPC130, with inhibition of 20.68%, 33.30%, 26.87%, 43.71%, and 53.10%, respectively. Scanning electron microscopy revealed that VOCs caused damage to the vegetative and reproductive structures of the fungus. These results suggest Bacillus LPPC170 as an excellent biocontrol tool against the phytopathogen causative agents of Panama disease.

Synthesis and evaluation of a pentafluorobenzamide stationary phase for HPLC separations in the reversed phase and hydrophilic interaction modes.

A pentafluorobenzamide stationary phase was synthesized by an easy method with no intermediate purification steps. Physicochemical characterization (elemental analysis, fourier transform infrared spectroscopy, 29 Si and 13 C nuclear magnetic resonance spectroscopy) confirmed the presence of pentafluorobenzamide functionalization on the surface of the silica particles. The pentafluorobenzamide stationary phase proved to be quite versatile as it can be used in two different modes in liquid chromatography: reversed phase and hydrophilic interaction liquid chromatography. Chromatographic characterizations in both modes confirmed the multiple interactions established by the new stationary phase, such as hydrogen bonding and π-π and ion-exchange interactions. The pentafluorobenzamide stationary phase was successfully employed for the separation of nucleosides and antihypertensive drugs under hydrophilic interaction liquid chromatography conditions, as well as pesticides and benzodiazepine using reversed phase conditions. The stationary phase showed significant potential when compared with commercial columns.