•Methods for simultaneous analysis of polyols present in crude bioconverted glycerin.•It is possible to distinguish pairs, trios or quartets of isomers from polyols.•Column temperature was a key ...parameter for separating some stereoisomers.•Important analytical tool for bioprospecting microorganisms.
The recent increase in the production of crude glycerin through the manufacture of biodiesel has imputed a commercial issue, the excess of this raw material in the market and its constant devaluation, which resulted in the need for new technologies for its use. Crude glycerin can be used in biotechnological processes for the production of high value-added compounds. This study presents novel, simple and fast methods based on ultra-high performance liquid chromatography (UHPLC) using evaporative light scattering detection (ELSD) for simultaneous analysis of ten sugar alcohols with a hydrophilic interaction chromatography (HILIC) column. The selected compounds and their possible stereoisomers have major commercial importance and they can be obtained by biotechnological routes. Under optimized conditions, threitol, erythritol, adonitol, xylitol, arabitol, iditol, sorbitol, mannitol, dulcitol and volemitol can be analyzed simultaneously within 15.0 min. The use of different column temperatures was a key parameter to reach the selectivity during the separation of some stereoisomers. Regression equations revealed a good linear relationship (R > 0.995) over the range from 50.0 to 800.0 ng. Limits of detection (LOD) and quantification (LOQ) ranged from 30.0 to 45.0 ng and 50.0–75.0 ng, respectively. The HILIC-UHPLC-ELSD methods showed good precision with low coefficient of variation (CV%) for the intra- and inter-assays experiments (≤ 5.1%) and high repeatability in terms of retention times for each analyte (≤ 0.5%). The accuracy was confirmed with an average recovery ranging from 92.3 to 107.3%. The developed methods employ an analytical technique more accessible and suitable for routine analyzes and have shown to be suitable for simultaneous analysis of sugar alcohols present in crude bioconverted glycerin samples using different classes of microorganisms.
The methanolic extract of the leaves of the medicinal plant
Byrsonima crassa (Malpighiaceae) contain flavonoids with antioxidant activity. They were separated in a preparative scale using high-speed ...counter-current chromatography. The optimum solvent system used was composed of a mixture of ethyl acetate–
n-propanol–water (140:8:80 (v/v/v)) and led to a successful separation between monoglucosilated flavonoids (quercetin-3-
O-α-
l-arabinoside, quercetin-3-
O-β-
d-galactoside) and the biflavonoid amentoflavone in only 3.5
h. The purities of quercetin-3-
O-α-
l-arabinoside (95
mg), quercetin-3-
O-β-
d-galactoside (16
mg) and the biflavonoid amentoflavone (114
mg) were all isolated at purity over 95%. Identification was performed by
1H NMR,
13C NMR and UV analyses.
Byrsonima intermedia is a native species of the cerrado formation (tropical American savannah). In Brazil, this plant has been used for the treatment of fever, in ulcers, as a diuretic, as ...antiasthmatics and in skin infections. Members of the genus
Byrsonima (Malpighiaceae) are employed not only in the folk medicine but also as food to make juice, jellies and liquor. The aim of this work was to evaluate the mutagenic effects of
Byrsonima intermedia, common name ‘murici’. Phytochemical analysis of methanol extract furnished (+)-catechin, (−)-epicatechin, quercetin-3-
O-β-
d-galactopyranoside, methyl gallate, gallic acid, quercetin-3-
O-α-
l-arabinopyranoside, amentoflavone, quercetin, quercetin-3-
O-(2″-
O-galloyl)-β-galactopyranoside and quercetin-3-
O-(2″-
O-galloyl)-α-arabinopyranoside. Methanol, hydromethanol and chloroform extracts were evaluated in mutagenic assay with
Salmonella typhimurium (Ames test) and mice (Micronucleus test). The methanolic extract presented signs of mutagenic activity for the strains TA98 and TA100 in the Ames assay. Mutagenicity was not observed in vivo.
The methanolic extract from the barks of the medicinal plant Qualea parviflora (Vochysiaceae) was fractionated by column chromatography over silica gel followed by gel permeation over Sephadex LH-20 ...to give 3,3'-di-O-methylellagic acid-4-O-beta-D-glucopyranoside (1), 3-O-methylellagic acid-4'-O-alpha-L-rhamnopyranoside (2), 3,3',4-tri-O-methylellagic acid-4'-O-beta-D-glucopyranoside (3), and 3,3'-di-O-methylellagic acid (4), together with triterpenes and saponins. We also performed comparative analyses among this species and Q. grandiflora and Q. multiflora using high-pressure liquid chromatography. The biological assays showed that, when compared to the standard ellagic acid, compounds 1-4 are less cytotoxic but have a lower capacity of stimulating murine peritoneal macrophages to release nitric oxide and tumoural-alpha necrose factor.
Jatropha curcas L. is an oil crop that has been studied as a potential source of biodiesel. A high protein pie is produced as a byproduct of the biodiesel production, which could be used as animal ...feed. However, the pie has toxic compounds, as phorbol esters and other toxins, which prevents the use as animal feed. For this reason, Embrapa (Brazilian Agricultural Research Corporation) has been working in genetic breeding to develop non-toxic J. curcas genotypes. To evaluate this process, a simple and fast analytical technique was employed to obtain responses in a short time. Leaf spray (LS) is a recent ambient ionization mass spectrometry technique in which the sample itself serves as support and ion source. Here, toxic and non-toxic J. curcas leaves were differentiated by LS using a linear ion trap mass spectrometer and partial least squares discriminant analysis (PLS-DA) model chemometrics. It was possible to differentiate toxic and non-toxic leaves and to identify the m/z values that contribute to discrimination between the groups.
Isolated flavonoids against mammary tumour cells LM2 Carli, Camila B de A; de Matos, Djamile C; Lopes, Flávia C M ...
Zeitschrift für Naturforschung C. A journal of biosciences,
01/2009, Volume:
64, Issue:
1-2
Journal Article
Peer reviewed
Open access
The purpose of the present study was to investigate antitumour and anti-inflammatory activities of flavonoids isolated from Byrsonima crassa, Davilla elliptica and Mouriri pusa. The antitumour ...activity was measured by the MTT assay in murine mammary tumour cells (LM2) and the IC50 values of the flavonoids tested ranged from (31.5 +/- 2.97) to (203.1 +/- 5.9) microg/ml. The flavonoids 1 (myricetin-3-O-alpha-L-rhamnopyranoside) and 3 (quercetin-3-O-galactopyranoside) from D. elliptica were the most active ones against the tumour cells. The same samples were tested to determine the inhibition of the release of nitric oxide (NO) and of the tumour necrosis factor-alpha (TNF-alpha) in murine macrophages by the Griess and ELISA sandwich assay, respectively. Almost all the samples showed inhibitory activity to the release of NO but not of TNF-alpha. Of all substances tested, flavonoids 2 (quercetin) and 6 (myricetin) may show promising activity in the treatment of murine breast cancer by immunomodulatory and antiproliferative activities.
The use of bioprocess to convert low valued biomass or agroindustrial byproducts into high-value chemicals is an emerging area. However, laboratories usually use outdated analytical techniques to ...identify bioproducts, losing valuable information, such as the identification of unexpected compounds. In this work, we presented a successful systematic and modern analytical approach based on direct infusion mass spectrometry (DIMS) for an automated high-throughput screening of untargeted compounds from glycerin bioconversion process. We describe advantages of DIMS and its combined application with chemometrics towards an untargeted metabolomics approach to analyze several samples in a short time (11 samples per h). Three batches with 34 samples from the bioconversion of glycerin using several filamentous fungi strains were analyzed. Batch 347 was selected as promising, since high value chemicals, such as amide, phenolic and acid compounds, were identified. The platform presented was fast, robust, and versatile, then it could be applied to different bioprocesses.
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