18 research outputs found
Solid-phase microextraction for determination of 3-chloro-4-(dichloromethyl)-5-hydroxy-2[5H]-furanone in water
Solid-phase microextraction, using on-line bis(trimethylsilyl)trifluoroacetamide derivatisation, gas chromatography, and mass spectrometry, was evaluated in the quantification of 3-chloro-4-(dichloromethyl)-5-hydroxy-2(5H)-furanone (MX) in water samples. Fibres encompassing a wide range of polarities were used with headspace and direct immersion sampling. For the immersion procedure, various parameters affecting MX extraction, including pH, salinity, temperature, and extraction time were evaluated. The optimised method (polyacrylate fibre; 20% Na2SO4; pH 2.0; 60 min; 20 °C) was applied for reservoir chlorinated water samples-either natural or spiked with MX (50 ng L-1 and 100 ng L-1). The recovery of MX ranged from 44 to 72%. Quantification of MX in water samples was done using external standard and the selected ion monitoring mode. Correlation coefficient (0.98%), relative standard deviation (5%), limit of detection (30 ng L-1) and limit of quantification (50 ng L-1) were obtained from calibration curve.Microextração em fase sólida, usando a derivatização on-line com bis(trimetilsilil)trifluoroacetamida, cromatografia a gás e espectrometria de massas, foi avaliada para a quantificação de 3-cloro-4-(diclorometil)-5-hidróxi-2(5H)-furanona (MX) em amostras de água. Foram usadas fibras de diferentes polaridades empregando a amostragem por imersão e por headspace. Para o sistema de imersão, foram avaliados vários parâmetros que afetam a extração de MX, como pH, salinidade, temperatura e tempo de extração. O método otimizado (fibra de poliacrilato; 20% Na2SO4; pH 2,0; 60 min; 20 °C) foi aplicado para águas cloradas proveniente de reservatórios de abastecimento de água-amostras naturais e amostras com adição de MX (50 ng L-1 e 100 ng L-1). A recuperação de MX variou de 44 a 72%. A quantificação do MX em amostras de água foi feita por padrão externo empregando o modo de monitoramento de íon selecionado. O coeficiente de correlação (0,98%), o desvio padrão relativo (5%), o limite de detecção (30 ng L-1) e o limite de quantificação (50 ng L-1) foram obtidos a partir da curva analítica.FAPES
Isomeric separation of cannabinoids by UPLC combined with ionic mobility mass spectrometry (TWIM-MS)-Part I
The Cannabis sativa L. plant is rich in a wide variety of cannabinoids. δ9-tetrahydrocannabinol (δ9-THC) is the main chemical compound responsible for its psychoactive effect, and it can be identified as [M+H]+ and [M-H]- ions at m/z 315 and 313, respectively, where M=C21H30O2. However, six other isomeric or isobaric forms of δ9-THC can exist, which makes its unequivocal characterization a challenge. In this work, ultra-high liquid chromatography coupled to traveling wave ion mobility mass spectrometry (UPLC-TWIM-MS) were applied to both electrospray ionization modes (ESI(±)) and used to analyze hashish, marijuana, and parts of the Cannabis Sativa L. plant (flower and leaf). The presence of a complex isomeric mixture of cannabinoids has been identified, and the mixture mainly contains δ9-THC, cannabidiol (CBN-C5 and Mw =310Da), δ9-tetrahydrocannabinolic acid A and B (δ9-THCA-C5 A/B and Mw =358Da) and their isomers. Three isomers of the ions were identified at m/z 315/313, 311, and 357 by using direct infusion ESI-TWIM-MS technique, while higher selectivity was observed in UPLC-ESI-TWIM-MS data, with the maximum isomeric separation between four and five compounds achieved when using single-ion mode (SIM) acquisition. The ions at m/z 311/309, 315/313, 345, and 357 correspond to CBN-C5, δ9-THC, cannabielsioc acid, δ9-THCA-C5 and their isomers, respectively, and they were the main species found. The calculations of collision cross sections were reported for all isomers of cannabinoids and associated with TWIM-MS results
2-(4-IODO-2,5-DIMETOXIFENIL)-N-[(2-METOXIFENIL)METIL]ETAMINA OU 25I-NBOME: CARACTERIZAÇÃO QUÍMICA DE UMA DESIGNER DRUG
Drug trafficking and the introduction of new drugs onto the illicit market are one of the main challenges of the forensic community. In this study, the chemical profile of a new designer drug, 2-(4-iodine-2,5-dimethoxyphenyl)-n-[(2-methoxyphenyl)methyl]etamine or 25I-NBOMe was explored using thin layer chromatography (TLC), ultraviolet-visible spectrophotometry (UV-Vis), attenuated total reflection with Fourier transform infrared spectroscopy(ATR-FTIR), gas chromatography mass spectrometry (GC-MS) and electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry (ESI-FT-ICR MS). First, the TLC technique was effective for identifying spots related to 25C-, 25B- and 25I-NBOMe compounds, all with the same retention factor, Rf ≈ 0.50. No spot was detected for 2,5-dimethoxy-4-bromoamphetamine, 2,5-Dimethoxy-4-chloroamphetamine or lysergic acid diethylamide compounds. ATR-FTIR preserved the physical-chemical properties of the material, whereas GC-MS and ESI-MS showed better analytical selectivity. ESI(+)FT-ICR MS was used to identify the exact mass (m/z428.1706 for the [M + H]+ ion), molecular formula (M = C18H22INO3), degree of unsaturation (DBE = 8) and the chemical structure (from collision induced dissociation, CID, experiments) of the 25I-NBOMe compound. Furthermore, the ATR-FTIR and CID results suggested the presence of isomers, where a second structure is proposed as an isomer of the 25I-NBOMe molecule
Fractionation of Asphaltene by Adsorption onto Silica and Chemical Characterization by Atmospheric Pressure Photoionization Fourier Transform Ion Cyclotron Resonance Mass Spectrometry, Fourier Transform Infrared Spectroscopy Coupled to Attenuated Total Reflectance, and Proton Nuclear Magnetic Resonance
Asphaltenes
are defined as the petroleum fraction insoluble in <i>n</i>-alkanes and soluble in aromatic solvents, such as toluene. Such
definition implies that asphaltenes are not a homogeneous material
but a mixture of fractions. Asphaltenes represent one of the major
contributors to several problematic issues for the petroleum industry.
Destabilized asphaltenes can cause arterial clogging within pipelines
and wellbores, corrosion and fouling of production equipment, reduction
of catalyst activity in refining processes, and other problems. This
work describes an investigation of the separation of asphaltenes into
three different fractions by adsorption onto silica particles. These
fractions (two adsorbed and one non-adsorbed onto silica) were characterized
by elemental analysis (C, H, and N), Fourier transform infrared spectroscopy
coupled to attenuated total reflectance (ATR–FTIR), proton
nuclear magnetic resonance (<sup>1</sup>H NMR) spectroscopy, and atmospheric
pressure photoionization Fourier transform ion cyclotron resonance
mass spectrometry (APPI–FT-ICR MS). APPI–FT-ICR MS and
ATR–FTIR accessed chemical information on a molecular level
[molecular formula, carbon number (CN) and double bond equivalent
(DBE) distributions, and organic groups], whereas <sup>1</sup>H NMR
and elemental analysis provided the aromaticity degree and C/H atomic
ratio of the samples, respectively. The C/H atomic ratio decreases
in the following the order: non-adsorbed > whole asphaltene >
adsorbed > irreversibly adsorbed. The irreversible fraction adsorbed
had the lowest percentage of aromatic hydrogen compared to other fractions
by <sup>1</sup>H NMR. There was a good correlation between the results
of NMR and elemental analysis. The efficiency of fractionation on
silica particles was proven to be successful by the low concentration
of polyaromatic hydrocabons observed for two samples adsorbed onto
silica and the increasing of the aromaticity degree and C/H ratio
for the non-adsorbed fraction. N<sub>2</sub>, N<sub>2</sub>O, and
NO compound classes were selectively separated from whole asphaltene
and concentrated in polar fractions (adsorbed fractions onto silica),
with their CN and DBE distributions reported. Therefore, this work
demonstrated the selectivity of the fractionation method onto silica
to retain highly polar compounds and, moreover, extends to the study
of the adsorbent surface and how the molecules of the asphaltenes
will behave against this change
Frequent Infection of Cats With SARS-CoV-2 Irrespective of Pre-Existing Enzootic Coronavirus Immunity, Brazil 2020.
Carnivores such as cats and minks are highly susceptible to SARS-CoV-2. Brazil is a global COVID-19 hot spot and several cases of human-to-cat transmission have been documented. We investigated the spread of SARS-CoV-2 by testing 547 domestic cats sampled between July-November 2020 from seven states in southern, southeastern, and northeastern Brazil. Moreover, we investigated whether immune responses elicited by enzootic coronaviruses affect SARS-CoV-2 infection in cats. We found infection with significantly higher neutralizing antibody titers against the Gamma variant of concern, endemic in Brazil during 2020, than against an early SARS-CoV-2 B.1 isolate (p<0.0001), validating the use of Gamma for further testing. The overall SARS-CoV-2 seroprevalence in Brazilian cats during late 2020 validated by plaque reduction neutralization test (PRNT90) was 7.3% (95% CI, 5.3-9.8). There was no significant difference in SARS-CoV-2 seroprevalence in cats between Brazilian states, suggesting homogeneous infection levels ranging from 4.6% (95% CI, 2.2-8.4) to 11.4% (95% CI, 6.7-17.4; p=0.4438). Seroprevalence of the prototypic cat coronavirus Feline coronavirus (FCoV) in a PRNT90 was high at 33.3% (95% CI, 24.9-42.5) and seroprevalence of Bovine coronavirus (BCoV) was low at 1.7% (95% CI, 0.2-5.9) in a PRNT90. Neutralizing antibody titers were significantly lower for FCoV than for SARS-CoV-2 (p=0.0001), consistent with relatively more recent infection of cats with SARS-CoV-2. Neither the magnitude of SARS-CoV-2 antibody titers (p=0.6390), nor SARS-CoV-2 infection status were affected by FCoV serostatus (p=0.8863). Our data suggest that pre-existing immunity against enzootic coronaviruses neither prevents, nor enhances SARS-CoV-2 infection in cats. High SARS-CoV-2 seroprevalence already during the first year of the pandemic substantiates frequent infection of domestic cats and raises concerns on potential SARS-CoV-2 mutations escaping human immunity upon spillback
Performance characteristics of finger-stick dried blood spots (DBS) on the determination of human immunodeficiency virus (HIV) treatment failure in a pediatric population in Mozambique
l -carnitine supplementation during vitrification or warming of in vivo -produced ovine embryos does not affect embryonic survival rates, but alters CrAT and PRDX1 expression
Chemical characterization of synthetic cannabinoids by electrospray ionization FT-ICR mass spectrometry
The First Modified Delphi Consensus Statement for Resuming Bariatric and Metabolic Surgery in the COVID-19 Times.
The purpose of this study was to achieve consensus amongst a global panel of expert bariatric surgeons on various aspects of resuming Bariatric and Metabolic Surgery (BMS) during the Coronavirus Disease-2019 (COVID-19) pandemic. A modified Delphi consensus-building protocol was used to build consensus amongst 44 globally recognised bariatric surgeons. The experts were asked to either agree or disagree with 111 statements they collectively proposed over two separate rounds. An agreement amongst ≥ 70.0% of experts was construed as consensus as per the predetermined methodology. We present here 38 of our key recommendations. This first global consensus statement on the resumption of BMS can provide a framework for multidisciplinary BMS teams planning to resume local services as well as guide future research in this area