Damila Rodrigues de Morais

Subcritical extraction of flaxseed oil with n-propane: Composition and purity

Flaxseed (Linum usitatissimum L.) oil was obtained via subcritical n-propane fluid extraction (SubFE) under different temperatures and pressures with an average yield of 28% and its composition, purity and oxidative stability were compared to oils obtained via conventional solvent extraction methods (SEMs). When the oxidative stability was measured by differential scanning calorimetry, the oil was found to be up to 5 times more resistant to lipid oxidation as compared to the SEM oils. Direct infusion electrospray ionization mass spectrometry (ESI-MS) analysis showed characteristic and similar TAG profiles for SubFE and SEMs oils but higher purity for the SubFE oil. The flaxseed oil content of β-tocopherol, campesterol, stigmasterol and sitosterol were quantified via GC-MS. SubFE showed to be a promising alternative to conventional SEM since SubFE provides an oil with higher purity and higher oxidation stability and with comparable levels of biologically active components.

Subcritical Extraction of Salvia hispanica L. Oil with N-Propane: Composition, Purity and Oxidation Stability as Compared to the Oils Obtained by Conventional Solvent Extraction Methods

This study evaluated the Chia (Salvia hispanica L.) oil composition in terms of fatty acids (FA), sterols, acylglycerols and oxidative stability obtained via subcritical n-propane fluid extraction (SubFE-propane), in different temperatures and pressure conditions, as compared to Bligh & Dyer (BD), Soxhlet (SE) and Folch (FLS) extractions. Total lipid varied from 23.25 to 30.21% and the best yield was obtained by both SubFE-propane extraction at 45 oC and 12 MPa (A). α-Linolenic acid (18:3n-3) was the most abundant FA and SubFE-propane extraction provided the best results for the sum of n-3 and PUFA. All oil samples were similar in regard to triacylglycerols (TAG) profiles as measured via direct electrospray ionization mass spectrometry (ESI-MS) analysis. The total amounts of stigmasterol, β-tocopherol and tocopherol total were highest in the Chia oil obtained by BD, campesterol and sitosterol by SE and γ-tocopherol by SubFE-propane extraction. The SubFE-propane oil also presented the best (2 to 5 times) oxidation stability. SubFE-propane was the most efficient extraction method for Chia oil, providing the highest extraction yields, purity, oxidation stability and diverse profile of sterols.

Purple carrot extract protects against cadmium intoxication in multiple organs of rats: Genotoxicity, oxidative stress and tissue morphology analyses

The aim of this study was to investigate if purple carrot extract is able to protect against the noxious activities induced by cadmium exposure in multiple organs of rats. For this purpose, histopathological analysis, genotoxicity and oxidative status were investigated in this setting. A total of twenty Wistar rats weighing 250g on the average, and 8 weeks age were distributed into four groups (n=5), as follows: Control group (non-treated group, CTRL); Cadmium group (Cd) and Purple carrot extract groups at 400mg/L or 800mg/L. Histopathological analysis revealed that liver from animals treated with purple carrot extract improved tissue degeneration induced by cadmium intoxication. Genetic damage was reduced in blood and hepatocytes as depicted by comet and micronucleus assays in animals treated with purple carrot extract. SOD-CuZn and cytocrome C gene expression increased in groups treated with purple carrot extract. Purple carrot extract also reduced the 8OHdG levels in liver cells when compared to cadmium group. Taken together, our results demonstrate that purple carrot extract is able to protect against cadmium intoxication by means of reducing tissue regeneration, genotoxicity and oxidative stress in multiple organs of Wistar rats.

Characterization of ANFO explosive by high accuracy ESI(±)-FTMS with forensic identification on real samples by EASI(-)-MS.

Ammonium nitrate fuel oil (ANFO) is an explosive used in many civil applications. In Brazil, ANFO has unfortunately also been used in criminal attacks, mainly in automated teller machine (ATM) explosions. In this paper, we describe a detailed characterization of the ANFO composition and its two main constituents (diesel and a nitrate explosive) using high resolution and accuracy mass spectrometry performed on an FT-ICR-mass spectrometer with electrospray ionization (ESI(±)-FTMS) in both the positive and negative ion modes. Via ESI(-)-MS, an ion marker for ANFO was characterized. Using a direct and simple ambient desorption/ionization technique, i.e., easy ambient sonic-spray ionization mass spectrometry (EASI-MS), in a simpler, lower accuracy but robust single quadrupole mass spectrometer, the ANFO ion marker was directly detected from the surface of banknotes collected from ATM explosion theft.

Determination of free, esterified, glycosylated and insoluble-bound phenolics composition in the edible part of araticum fruit (Annona crassiflora Mart.) and its by-products by HPLC-ESI-MS/MS

Phenolics present in the free, esterified, glycosylated and insoluble-bound forms of araticum pulp, peel and seed were for the first time characterized and quantified using HPLC-ESI-MS/MS. Levels of total phenolics, flavonoids, condensed tannins and antioxidant activities from araticum fruit followed the order peelu202f>u202fpulpu202f>u202fseed. Overall, insoluble-bound and esterified phenolics were the dominant forms of phenolics from araticum fruit parts and the highest contributors to their antioxidant activities. Extracts were found to contain contrasting levels of phenolics that were specific to each fruit part. From 10 phenolics quantified in araticum fruit, catechin and epicatechin were the major ones from pulp and peel, whereas seed displayed caffeic acid, catechin and epicatechin as its main phenolics. Araticum fruit was found to provide a good source of phenolics, and the full exploitation of this fruit may find applications in the food, cosmetic and pharmaceutical industries.

A dopant for improved sensitivity in easy ambient sonic‐spray ionization mass spectrometry

Recently, 3-nitrobenzonitrile (3-NBN) has been used to improve sensitivity of sonic-spray ionization mass spectrometry. Easy ambient sonic-spray ionization (EASI) is one of the simplest, gentlest and most used spray-based desorption/ionization ambient techniques, but limited sensitivity has been commonly taken as its major drawback. Herein we investigate the use of 3-NBN as a dopant in EASI-MS for improved sensitivity. Using a few typical EASI samples as test cases, the presence of 10u2009ppm (µgu2009ml(-1) ) of 3-NBN in the spray solvent showed two to fourfold gains in EASI-MS sensitivity as measured both by total ion current and S/N ratios, accompanied with significant reductions in chemical noise. Sensitivity for DESI using 3-NBN as a dopant also improved and dopant DESI versus dopant EASI sensitivities were compared. The use of solvent dopants seems therefore to be a promising strategy to improve sensitivity for spray-based ambient MS techniques. Copyright

Forensic Application of X-ray Fluorescence Spectroscopy for the Discrimination of Authentic and Counterfeit Revenue Stamps

Energy-dispersive X-ray fluorescence (ED-XRF) spectroscopy with data treatment via chemometric tools was explored as an analytical protocol to discriminate between authentic and counterfeit revenue stamps. Untreated samples were directly analyzed, and the discrimination was based on the characterization of constituent elements present in the inks and paper. Authentic samples and samples that were suspected of being counterfeit were analyzed at three different areas on their surfaces: the ink-printed area, the non-printed area, and the holographic area. Principal component analysis (PCA) was applied to the data to discriminate between authentic and counterfeit revenue stamps. Major differences in the elemental composition were noted (according to chemometrics and t-test, pu2009<u20090.05), and ED-XRF spectroscopy plus PCA protocol is proposed for use by non-specialist operators to screen for counterfeit stamps.

Ayahuasca and Kambo intoxication after alternative natural therapy for depression, confirmed by mass spectrometry

PurposeWe present a case report about an acute intoxication episode after an oral administration of Ayahuasca and dermal exposure of Kambo for treatment of depression. The clinical features observed were hallucination, agitation, tremors of extremities, oral paresthesia, skin lesions and seizures. Diazepam was administered by the emergency service and was effective in controlling hallucination, but failed to control agitation and seizures.MethodsPatient biological fluids (urine and serum) and the samples of Ayahuasca and Kambo were submitted to toxicological analysis using liquid-liquid extraction followed by liquid chromatography–tandem mass spectrometry and high-resolution electrospray ionization-mass spectrometry.ResultsThe main active compounds present in Ayahuasca, N,N-dimethyltryptamine, harmine, harmaline and tetrahydroharmine were found and quantified in the different samples, confirming the use by the patient. In Kambo secretion used in the ritual, we were able to find sixteen potently active peptides: adenoregulin, bombesin, bombesinnona peptide, bradykinin -phe(8)-psi-CH2NH-arg(9)-, caerulein, deltorphin, neurokinin B, phyllomedusin, phyllocaerulein, phyllokinin, phyllolitorin, preprotachykinin B (50–79), ranatachykinin A, sauvagine, T-kinin and urechistachykinin II.ConclusionsThe patient was discharged the day after exposure without any sequel. Clinical and toxicological analysis indicated that the symptoms presented by the patient occurred due to a joint action produced by the substances identified in both materials. To the best of our knowledge, this is the first case involving probable intoxication by simultaneous administration of Ayahuasca and Kambo.

EASI-IMS an expedite and secure technique to screen for 25I-NBOH in blotter papers

The increasing number of new psychoactive substances (NPS) and their quick worldwide spreading, often only slightly modified in the form of new derivatives and analogues, have brought the need for fast, wide-ranging, and unequivocal identification methods in clinical and forensic investigations. Because it usually provides secure results, gas chromatography coupled to mass spectrometry (GC-MS) has been routinely employed as the standard technique for the detection of NPS in blotter papers. For 25I-NBOH (N-(2-hydroxybenzyl)-2-(4-iodo-2,5-dimethoxyphenyl)ethan-1-aminium), however, GC-MS analysis of an blotter paper extract leads to incorrect results. In this work, we investigated whether easy ambient sonic-spray mass spectrometry imaging (EASI-IMS), and ambient ionization MS method can be applied directly to the surface of the sample requiring therefore no extraction or sample preparations, would serve as an efficient, sensitive, and secure alternative for 25I-NBOH screening.

Novel natural food colourant G8000 benefits LDL- and HDL-cholesterol in humans.

Abstract The aim of this study was to investigate the phenolic composition of a natural food colourant (G8000™) as well as its effects on plasma markers after 28-day consumption by healthy individuals at a dietary dose (70u2009g). Parameters of total cholesterol and its fractions, triglycerides and plasma enzymes biomarkers of muscle injury were measured. Major compounds identified in G8000™ by ESI-MS showed the presence of anthocyanins, organic acids, phenolic acids as well as monosaccharides. HDL levels significantly increased from 43u2009±u200910.2u2009mg/dL to 95u2009±u200916.9u2009mg/dL. LDL levels significantly decreased from 110u2009±u200940.9u2009mg/dL to 69u2009±u200939u2009mg/dL (pu2009<u20090.001). No significant statistical differences (pu2009>u20090.05) were observed for total cholesterol, triglycerides and VLDL. After the intake, plasma enzyme CK-MB decreased from 20u2009±u200912.1 U/L to 10u2009±u20091.9 U/L while LDH levels increased from 275u2009±u2009124.4 U/L to 317u2009±u2009114.7 U/L (pu2009<u20090.005). No significant differences were observed for CK levels. Taken together, dietary intake of natural colourant G8000™ was able to exert beneficial effects on atherosclerosis biomarkers.