Your browser doesn't support javascript.
loading
Mostrar: 20 | 50 | 100
Resultados 1 - 20 de 462
Filtrar
Más filtros

Intervalo de año de publicación
1.
Anal Chem ; 96(31): 12862-12874, 2024 08 06.
Artículo en Inglés | MEDLINE | ID: mdl-39045809

RESUMEN

Surface-enhanced Raman spectroscopy (SERS) detection platforms with high signal-to-noise ratio in the "biological-silent" region (1800-2800 cm-1) are presently being developed for sensing and imaging applications, overcoming the limitations of traditional SERS studies in the "fingerprint" region. Herein, a series of cyano-programmable Raman reporters (RRs) operating in the "biological-silent" region were designed based on 4-mercaptobenzonitrile derivatives and then embedded in core-shell Au@Ag nanostars using a "bottom-up" strategy to provide SERS enhancement and encapsulation protection. The approach enabled the "one-pot" readout interference-free detection of multiple bioamines (histamine, tyramine, and ß-phenethylamine) based on aptamer-driven magnetic-induced technology. Three cyano-encoded SERS tags resulted in separate SERS signals for histamine, tyramine, and ß-phenethylamine at 2220, 2251, and 2150 cm-1, respectively. A target-specific aptamer-complementary DNA competitive binding strategy allowed the formation of microscale core-satellite assemblies between Fe3O4-based magnetic beads and the SERS tags, enabling multiple SERS signals to be observed simultaneously under a 785 nm laser excitation laser. The LODs for detection of the three bioamines were 0.61 × 10-5, 2.67 × 10-5, and 1.78 × 10-5 mg L-1, respectively. The SERS-encoded platform utilizing programmable reporters provides a fast and sensitive approach for the simultaneous detection of multiple biomarkers, paving the way for routine SERS analyses of multiple analytes in complex matrices.


Asunto(s)
Oro , Plata , Espectrometría Raman , Tiramina , Espectrometría Raman/métodos , Plata/química , Oro/química , Tiramina/química , Tiramina/análisis , Nanopartículas del Metal/química , Fenetilaminas/análisis , Aptámeros de Nucleótidos/química , Histamina/análisis , Límite de Detección , Nitrilos/química
2.
Sud Med Ekspert ; 67(5): 29-35, 2024.
Artículo en Ruso | MEDLINE | ID: mdl-39440562

RESUMEN

OBJECTIVE: To develop the method for identification of mebeverine and its metabolites in biological materials (urine and hair) for solution of the problem of possible cross-reaction with psychoactive substances during preliminary studies by immunochromatographic method. MATERIAL AND METHODS: The study was carried out using «Mebeverine¼ tablets (NAO «Severnaya Zvezda¼, Russia), enzymes, namely trypsin, chymotrypsin and hyaluronidase, papain. The obtained extracts were analyzed using HELC-MS/MS on a modular liquid Nexera XR chromatograph with a tandem LCMS-8050 (Shimadzu) mass spectrometer. Guinea pigs weighing about 500 gr were used in modelling the long-term use of mebeverine. The drug was administered per os, once to 5 guinea pigs at a dosage of 200 mg calculated as an animal weighing 500 gr and daily urine was collected. The wool was collected 30 days after regular administration. RESULTS AND CONCLUSION: The main mebeverine's metabolites have been determined and native mebeverine and its marker metabolites (mebeverine and veratric acids) have been found in urine while taking this medicine in therapeutic doses for medical purposes. The application of enzymatic hydrolysis of hair method allowed to establish that hair tissue accumulates only a native molecule of mebeverine, therefore, only by results of hair analysis it is possible to conclude, if there was pharmacological use of this medicine or psychoactive substances from the group of phenylalkilamines. The effectiveness of enzymatic hydrolysis by hyaluronidase to isolate mebeverine from hair has been shown.


Asunto(s)
Cabello , Fenetilaminas , Animales , Fenetilaminas/análisis , Cobayas , Cabello/química , Toxicología Forense/métodos , Espectrometría de Masas en Tándem/métodos , Antitusígenos/análisis
3.
Nature ; 548(7668): 476-479, 2017 08 24.
Artículo en Inglés | MEDLINE | ID: mdl-28813419

RESUMEN

Fenethylline, also known by the trade name Captagon, is a synthetic psychoactive stimulant that has recently been linked to a substance-use disorder and 'pharmacoterrorism' in the Middle East. Although fenethylline shares a common phenethylamine core with other amphetamine-type stimulants, it also incorporates a covalently linked xanthine moiety into its parent structure. These independently active pharmacophores are liberated during metabolism, resulting in the release of a structurally diverse chemical mixture into the central nervous system. Although the psychoactive properties of fenethylline have been reported to differ from those of other synthetic stimulants, the in vivo chemical complexity it manifests upon ingestion has impeded efforts to unambiguously identify the specific species responsible for these effects. Here we develop a 'dissection through vaccination' approach, called DISSECTIV, to mitigate the psychoactive effects of fenethylline and show that its rapid-onset and distinct psychoactive properties are facilitated by functional synergy between theophylline and amphetamine. Our results demonstrate that incremental vaccination against a single chemical species within a multi-component mixture can be used to uncover emergent properties arising from polypharmacological activity. We anticipate that DISSECTIV will be used to expose unidentified active chemical species and resolve pharmacodynamic interactions within other chemically complex systems, such as those found in counterfeit or illegal drug preparations, post-metabolic tissue samples and natural product extracts.


Asunto(s)
Anfetamina/farmacología , Anfetaminas/inmunología , Anfetaminas/farmacología , Estimulantes del Sistema Nervioso Central/antagonistas & inhibidores , Estimulantes del Sistema Nervioso Central/farmacología , Fraccionamiento Químico/métodos , Teofilina/análogos & derivados , Teofilina/farmacología , Vacunas/inmunología , Anfetamina/química , Anfetamina/inmunología , Anfetamina/metabolismo , Anfetaminas/antagonistas & inhibidores , Anfetaminas/metabolismo , Animales , Productos Biológicos/química , Productos Biológicos/inmunología , Productos Biológicos/metabolismo , Productos Biológicos/farmacología , Estimulantes del Sistema Nervioso Central/inmunología , Estimulantes del Sistema Nervioso Central/metabolismo , Sistema Enzimático del Citocromo P-450/metabolismo , Sinergismo Farmacológico , Haptenos/química , Haptenos/inmunología , Haptenos/farmacología , Hemocianinas/química , Hemocianinas/inmunología , Drogas Ilícitas/química , Drogas Ilícitas/inmunología , Drogas Ilícitas/metabolismo , Drogas Ilícitas/farmacología , Masculino , Ratones , Fenetilaminas/análisis , Fenetilaminas/química , Teofilina/antagonistas & inhibidores , Teofilina/química , Teofilina/inmunología , Teofilina/metabolismo , Vacunas/farmacología
4.
J Mol Recognit ; 34(10): e2903, 2021 10.
Artículo en Inglés | MEDLINE | ID: mdl-33970548

RESUMEN

A novel spectrofluorimetric sensing platform was designed for Ractopamine measurement in aqueous and plasma samples. d-penicillamine functionalized graphene quantum dots (DPA-GQDs) was utilized as a fluorescence probe, which was synthesized through the pyrolysis of citric acid in the presence of DPA. This one-pot down-top strategy causes to high-yield controllable synthesis method. The reaction time and probe concentration were optimized. Then, the fluorescence intensity of aqueous samples containing different Ractopamine concentrations and 500 ppm DPA-GQDs were measured at 25°C with an excitation wavelength of 274 nm. The sensing platform was also applied to detect Ractopamine in untreated plasma samples. The fluorescence spectroscopy technique responses indicated a linear relationship between the peak fluorescence intensity and ractopamine concentration in the range of 0.25-15 ppm with low limit of quantification of 0.25 ppm was for aqueous and plasma samples, respectively.


Asunto(s)
Colorantes Fluorescentes/química , Fenetilaminas/análisis , Puntos Cuánticos/química , Espectrometría de Fluorescencia/métodos , Agonistas Adrenérgicos beta/análisis , Agonistas Adrenérgicos beta/sangre , Análisis Químico de la Sangre/métodos , Grafito/química , Humanos , Penicilamina/química , Fenetilaminas/sangre , Espectrometría de Fluorescencia/instrumentación , Espectroscopía Infrarroja por Transformada de Fourier
5.
Molecules ; 26(20)2021 Oct 12.
Artículo en Inglés | MEDLINE | ID: mdl-34684725

RESUMEN

The analysis of psychoactive substances in hair is of great importance for both clinical and forensic toxicologists since it allows one to evaluate past and continuative exposure to xenobiotics. In particular, a new challenge is represented by new psychoactive substances: Among this new class of drugs of abuse, synthetic cathinone and phenethylamine derivatives are often detected in biological samples. Hence, there is a growing need to develop new analytical procedures or improve old ones in order to conduct evaluations of these emerging substances. This study is a systematic review of all the instrumental and experimental data available in the literature. A total of 32 articles were included in the review. Acidic solvents proved to be the most reliable solutions for extraction. Gas chromatography and liquid chromatography coupled to tandem mass spectrometric and high-resolution mass spectrometric systems represent the majority of the involved instrumental techniques. Sensitivity must be maintained at the pg/mg level to detect any occurrences up to occasional consumption. In total, 23 out of 32 articles reported real positive samples. The most frequently detected substance in hair was mephedrone, followed by butylone, methylone, MDPV, and α-pyrrolidinophenone-type substances.


Asunto(s)
Alcaloides/análisis , Cabello/química , Fenetilaminas/análisis , Cromatografía Liquida/métodos , Toxicología Forense/métodos , Cromatografía de Gases y Espectrometría de Masas/métodos , Humanos , Drogas Ilícitas/análisis , Límite de Detección , Detección de Abuso de Sustancias/métodos , Espectrometría de Masas en Tándem/métodos
6.
Mikrochim Acta ; 187(5): 285, 2020 04 23.
Artículo en Inglés | MEDLINE | ID: mdl-32322994

RESUMEN

A competitive immunochromatographic assay (ICA) is presented and used for on-site determination of ractopamine (RAC). Ultramarine blue nanoparticles were directly separated from ultramarine blue industrial products by centrifugation (< 10,000 rpm and > 4000 rpm) and used as visible labels in ICAs. The ultramarine blue nanoparticles were coated by polyacrylic acid (PAA), which provides carboxyl groups on the surface of ultramarine blue nanoparticles. An anti-RAC monoclonal antibody (mAb) was covalently immobilized on the carboxyl-modified ultramarine blue nanoparticle surface via diimide-activated conjugation between the carboxyl groups on the ultramarine blue nanoparticle surface and the amino groups of the antibodies. RAC and BSA-modified RAC competitively bind to the anti-RAC mAb on the ultramarine blue nanoparticles. The blue band in the test line is generated by the accumulation of ultramarine blue nanoparticles and is negatively associated with the RAC content. Under optimal conditions, the visual limit of detection (vLOD) of this ICA for RAC is 2.0 ng mL-1, 2.0 ng mL-1, and 1.0 ng mL-1 in phosphate-buffered saline (PBS), feed samples, and pork samples, respectively. The ultramarine blue nanoparticle-based ICA also shows no cross activity with salbutamol, clorprenaline, clenbuterol, or terbutaline. Graphical abstract Schematic representation of the ultramarine blue nanoparticles immunochromatographic assay for detection of ractopamine (RAC) based on competitive method. The ultramarine blue nanoparticles were screened from commercial ultramarine pigments for the first time and used to detect ractopamine.


Asunto(s)
Colorantes Fluorescentes/química , Nanopartículas/química , Fenetilaminas/análisis , Animales , Anticuerpos Monoclonales/química , Anticuerpos Monoclonales/inmunología , Cromatografía de Afinidad , Estructura Molecular , Tamaño de la Partícula , Fenetilaminas/inmunología , Propiedades de Superficie , Porcinos
7.
Anal Chem ; 91(9): 5483-5488, 2019 05 07.
Artículo en Inglés | MEDLINE | ID: mdl-30990678

RESUMEN

The NBOMe family is a group of new psychoactive substances (NPSs). In this study, the fragmentation patterns of NBOMe derivatives were analyzed using liquid chromatography quadrupole time-of-flight mass spectrometry (LC-QTOF/MS). The MS/MS spectral data was used to establish a molecular networking map for NBOMe derivatives. The fragmentation patterns of nine NBOMe derivatives were interpreted on the basis of their product ion spectral data. NBOMe derivatives generally showed similar product ion spectral patterns; among them, the halogen-substituted methoxybenzyl ethanamine type derivatives showed a characteristic product ion of a radical cation. Molecular network analysis of the MS/MS data revealed that all NBOMe derivatives formed one integrated networking cluster that discriminated them from other types of NPSs. NBOMe derivatives were spiked into human urine and identified by connection to the NBOMe database network. Furthermore, the NBOMe compounds that were not registered in the database were also recognized as an NBOMe-related substance by molecular networking. These results demonstrate the potential of using molecular networking-based screening methods for designer drugs, and the proposed method would be useful in forensic or doping analysis.


Asunto(s)
Drogas de Diseño/análisis , Drogas de Diseño/química , Doping en los Deportes/prevención & control , Ciencias Forenses , Fenetilaminas/análisis , Fenetilaminas/química , Halógenos/química , Espectrometría de Masas en Tándem
8.
Mikrochim Acta ; 186(12): 836, 2019 11 23.
Artículo en Inglés | MEDLINE | ID: mdl-31758341

RESUMEN

A series of phosphorene (BP) nanocomposites was prepared to realize simultaneous electrochemical determination of clenbuterol (CLB) and ractopamine (RAC). CLB and RAC are the most commonly used ß-agonists in animal-derived food. The BP nanohybrid was obtained by co-decoration with both mono(6-mercapto-6-deoxy)-ß-cyclodextrin and poly(3,4-ethylenedioxythiophene) nanoparticles. It displays high stability, antifouling capability, a large electrochemical active surface and good electrochemical response. The electrochemical assisted antifouling strategy was selected by further eliminating the fouling of the electrode surface using continuous cyclic voltammetry. The electrode was employed for electrochemical sensing of CLB and RAC at typical peak voltages of 0.8 and 1.0 V (vs. SCE). Responses are linear in the 0.3-90 µM concentration range for CLB, and from 0.3 to 9.4 µM for RAC under optimal conditions. The limit of detection are 0.14 and 0.12 µM, respectively. The sensor was employed for simultaneous determination of CLB and RAC in (spiked) beef, feed and bovine serum samples with acceptable recoveries. Graphical abstractAn electrochemically assisted anti-fouling method for simultaneous voltammetric nanosensing of clenbuterol (CLB) and ractopamine (RAC) in edible cattle product samples using high-stable and anti-foul phosphorene (BP) co-decorated with mono(6-mercapto-6-deoxy)-ß-cyclodextrin (S-ß-CD) and poly(3,4-ethylenedioxythiophene) (PEDOTNPs).


Asunto(s)
Incrustaciones Biológicas/prevención & control , Clenbuterol/análisis , Nanocompuestos/química , Fenetilaminas/análisis , Fósforo/química , Animales , Bovinos , Técnicas Electroquímicas , Electrodos , Tamaño de la Partícula , Propiedades de Superficie
9.
Mikrochim Acta ; 186(7): 421, 2019 06 11.
Artículo en Inglés | MEDLINE | ID: mdl-31187272

RESUMEN

An immunochromatographic assay (ICA) is presented that can be applied to simultaneous detection of clenbuterol (CLE) and ractopamine (RAC). It is making use of two red and blue silica nanoparticles (SiNPs) that act as labels for encoding the antibodies. This design permits multiplexed analysis in a single test line and does not require an external source for photoexcitation. Anti-CLE was labeled with red SiNPs, and anti-RAC with blue SiNPs. The capture antigens CLE-BSA and RAC-BSA were placed onto the conjugate pad and the test line of the test strip, respectively. Under bare eye examination, no cross-colored lines or nonspecific bioconjugate adsorption were observed, and the visible limit of detections for CLE (red) and RAC (blue) are 3 and 2 ng‧mL-1, respectively. This design allows for multiplexed detection with reduced device dimensions and costs, and with easy integration and manufacturing. Conceivably, the method may be extended to simultaneous determination of numerous other analytes. Graphic abstract The principle of qualitative detection strategy of multiplex immunochromatographic assay for clenbuterol (CLE) and ractopamine (RAC) is schematically illustrated. Depending on the type and ratio of organic dyes, the color of colored silica nanoparticle can be tuned from red to purple and even to black (lower right corner).


Asunto(s)
Agonistas Adrenérgicos beta/análisis , Clenbuterol/análisis , Inmunoensayo/métodos , Nanopartículas/química , Fenetilaminas/análisis , Dióxido de Silicio/química , Agonistas Adrenérgicos beta/inmunología , Anticuerpos Monoclonales/inmunología , Clenbuterol/inmunología , Color , Inmunoensayo/instrumentación , Límite de Detección , Fenetilaminas/inmunología , Pruebas en el Punto de Atención
10.
Mikrochim Acta ; 186(8): 552, 2019 07 20.
Artículo en Inglés | MEDLINE | ID: mdl-31325046

RESUMEN

Copper(II) polyphthalocyanine (CuPPc) was combined with graphitic carbon nitride (g-C3N4) to form a heterojunction with enhanced photoelectrochemical (PEC) signal. A sensitive PEC method was developed for determination of ractopamine based on a PEC inner filter effect between gold nanoparticles (AuNPs) and the g-C3N4/CuPPc. A gold electrode was modified with g-C3N4/CuPPc and the DNA was linked to the AuNPs. Initially, the PEC signal is weak due to the inner filter effect between the AuNPs and g-C3N4/CuPPc. In the presence of ractopamine, it interacts with the aptamer and the complementary chain (C chain) is released. This triggers the entropy-driven cyclic amplification and results in the release of the substrate B chain (SB chain) from three-dimensional DNA stabilizer. The probe is released from the electrode due to the interaction of probe DNA and the SB chain. As a result, the PEC signal increases linearly in the 0.1 pmol·L-1 to 1000 pmol·L-1 ractopamine concentration range. The detection limit is 0.03 pM, and the relative standard deviation is 3.4% (at a 10 pmol·L-1 level; for n = 11). The method has been successfully applied to the determination of ractopamine in pork samples. Graphical abstract Schematic presentation of detection method based on PEC inner filter effect between AuNPs and the g-C3N4/CuPPc being fabricated for ractopamine. 3D DNA was used as stabilizer to decrease the PEC blank signal.


Asunto(s)
Agonistas Adrenérgicos beta/análisis , Grafito/química , Indoles/química , Nanopartículas del Metal/química , Compuestos de Nitrógeno/química , Compuestos Organometálicos/química , Fenetilaminas/análisis , Agonistas Adrenérgicos beta/química , Aptámeros de Nucleótidos/química , ADN/química , Técnicas Electroquímicas , Contaminación de Alimentos/análisis , Oro , Luz , Fenetilaminas/química , Procesos Fotoquímicos , Carne de Cerdo/análisis
11.
Sud Med Ekspert ; 62(2): 34-39, 2019.
Artículo en Ruso | MEDLINE | ID: mdl-31213590

RESUMEN

This article is focused on the conditions for the detection and identification of 2-[4-bromo-2.5-dimethoxyl]-N-[(2-methoxyphenyl)methyl] ethamine (25B-NBOMe) and its major metabolites by the combination of the HPLC/MS/MS techniques. The high-resolution mass spectra obtained with the use of a linear ion trap are described. The results of the study give evidence of the possibility for the detection of the analytes within 24 hours after drug consumption and within 3 months after the storage of the biological material of interest in a refrigerator at a temperature of 3-5 °C. The data obtained confirmed high stability of 2-(4-bromo-2.5-dimethoxyl]-N-[(2-methoxyphenyl)methyl] ethamine and its metabolites in the biological tissues.


Asunto(s)
Anisoles/análisis , Cromatografía Líquida de Alta Presión , Ciencias Forenses/métodos , Fenetilaminas/análisis , Espectrometría de Masas en Tándem
12.
Metabolomics ; 14(5): 60, 2018 04 17.
Artículo en Inglés | MEDLINE | ID: mdl-30830413

RESUMEN

INTRODUCTION: Although it is still at a very early stage compared to its mass spectrometry (MS) counterpart, proton nuclear magnetic resonance (NMR) lipidomics is worth being investigated as an original and complementary solution for lipidomics. Dedicated sample preparation protocols and adapted data acquisition methods have to be developed to set up an NMR lipidomics workflow; in particular, the considerable overlap observed for lipid signals on 1D spectra may hamper its applicability. OBJECTIVES: The study describes the development of a complete proton NMR lipidomics workflow for application to serum fingerprinting. It includes the assessment of fast 2D NMR strategies, which, besides reducing signal overlap by spreading the signals along a second dimension, offer compatibility with the high-throughput requirements of food quality characterization. METHOD: The robustness of the developed sample preparation protocol is assessed in terms of repeatability and ability to provide informative fingerprints; further, different NMR acquisition schemes-including classical 1D, fast 2D based on non-uniform sampling or ultrafast schemes-are evaluated and compared. Finally, as a proof of concept, the developed workflow is applied to characterize lipid profiles disruption in serum from ß-agonists diet fed pigs. RESULTS: Our results show the ability of the workflow to discriminate efficiently sample groups based on their lipidic profile, while using fast 2D NMR methods in an automated acquisition framework. CONCLUSION: This work demonstrates the potential of fast multidimensional 1H NMR-suited with an appropriate sample preparation-for lipidomics fingerprinting as well as its applicability to address chemical food safety issues.


Asunto(s)
Lípidos/química , Espectroscopía de Resonancia Magnética/métodos , Metabolómica/métodos , Animales , Femenino , Alimentos , Inocuidad de los Alimentos/métodos , Imagen por Resonancia Magnética , Fenetilaminas/análisis , Fenetilaminas/sangre , Porcinos/sangre , Flujo de Trabajo
13.
Mikrochim Acta ; 185(4): 210, 2018 03 07.
Artículo en Inglés | MEDLINE | ID: mdl-29594705

RESUMEN

The work describes a gold nanoparticle-based colorimetric enzyme-linked immunosorbent assay (ELISA) for ractopamine. The ELISA is based on an indirect competitive approach. In the presence of ractopamine, gold(III) ions are oxidized by H2O2 to form red AuNPs. On the other hand, the AuNP in solution are purple-blue due to aggregation if the sample does not contain ractopamine. The absorption, best measured at 560 nm, increases linearly in the 2 to 512 ng·mL-1 ractopamine concentration range, and the detection limit is as low as 0.35 ng·mL-1 in urine. Ractopamine can also be detected visually, even in the presence of other ß-agonists and antibiotics. The results obtained by this method are consistent with those obtained by LC-MS/MS as demonstrated by analysis of sheep urine. The ELISA method described here is inexpensive, easy-to-use, and suitable for rapid screening of ractopamine in animal samples. Graphical abstract Schematic presentation of a colorimetric indirect competitive immunoassay for ractopamine. It is based on the use of catalase labeled IgG and the measurement of the absorption of red gold nanoparticles (AuNPs) that are generated by the reaction of gold ions with H2O2. In the absence of ractopamine, the solution becomes blue.


Asunto(s)
Colorimetría/métodos , Ensayo de Inmunoadsorción Enzimática/métodos , Oro/química , Nanopartículas del Metal/química , Fenetilaminas/análisis , Animales , Catalasa/metabolismo , Peróxido de Hidrógeno/química , Fenetilaminas/orina , Estreptavidina/metabolismo
14.
Fed Regist ; 83(170): 44474-8, 2018 Aug 31.
Artículo en Inglés | MEDLINE | ID: mdl-30198687

RESUMEN

The Acting Administrator of the Drug Enforcement Administration is issuing this temporary scheduling order to schedule the synthetic cathinone, 1- (1,3-benzodioxol-5-yl)-2-(ethylamino)- pentan-1-one (N-ethylpentylone, ephylone) and its optical, positional, and geometric isomers, salts, and salts of isomers in schedule I. This action is based on a finding by the Acting Administrator that the placement of Nethylpentylone in schedule I of the Controlled Substances Act (CSA) is necessary to avoid an imminent hazard to the public safety. As a result of this order, the regulatory controls and administrative, civil, and criminal sanctions applicable to schedule I controlled substances will be imposed on persons who handle (manufacture, distribute, reverse distribute, import, export, engage in research, conduct instructional activities or chemical analysis, or possess), or propose to handle N-ethylpentylone.


Asunto(s)
Alcaloides/clasificación , Control de Medicamentos y Narcóticos/legislación & jurisprudencia , Fenetilaminas/clasificación , Drogas de Diseño/clasificación , Etiquetado de Medicamentos/legislación & jurisprudencia , Humanos , Drogas Ilícitas , Fenetilaminas/análisis , Estados Unidos
15.
J Am Chem Soc ; 139(20): 6851-6854, 2017 05 24.
Artículo en Inglés | MEDLINE | ID: mdl-28481522

RESUMEN

The rate of hydrogen-deuterium exchange (HDX) in aqueous droplets of phenethylamine has been determined with submillisecond temporal resolution by mass spectrometry using nanoelectrospray ionization with a theta-capillary. The average speed of the microdroplets is measured using microparticle image velocimetry. The droplet travel time is varied from 20 to 320 µs by changing the distance between the emitter and the heated inlet to the mass spectrometer and the voltage applied to the emitter source. The droplets were found to accelerate by ∼30% during their observable travel time. Our droplet imaging shows that the theta-capillary produces two Taylor cone-jets (one per channel), causing mixing to take place from droplet fusion in the Taylor spray zone. Phenethylamine (ϕCH2CH2NH2) was chosen to study because it has only one functional group (-NH2) that undergoes rapid HDX. We model the HDX with a system of ordinary differential equations. The rate constant for the formation of -NH2D+ from -NH3+ is 3660 ± 290 s-1, and the rate constant for the formation of -NHD2+ from -NH2D+ is 3330 ± 270 s-1. The observed rates are about 3 times faster than what has been reported for rapidly exchangeable peptide side-chain groups in bulk measurements using stopped-flow kinetics and NMR spectroscopy. We also applied this technique to determine the HDX rates for a small 10-residue peptide, angiotensin I, in aqueous droplets, from which we found a 7-fold acceleration of HDX in the droplet compared to that in bulk solution.


Asunto(s)
Medición de Intercambio de Deuterio , Fenetilaminas/análisis , Agua/química , Nanotecnología , Tamaño de la Partícula , Espectrometría de Masa por Ionización de Electrospray
16.
Anal Chem ; 89(3): 1445-1452, 2017 02 07.
Artículo en Inglés | MEDLINE | ID: mdl-28059498

RESUMEN

The NBOMe derivatives are phenethylamines derived from the 2C class of hallucinogens. Only a few human pharmacologic studies have been conducted on these drugs, and several cases of intoxication and deaths have been reported. Presently, NBOMe are not a part of the routine drugs-of-abuse screening procedure for many police forces, and there are no rapid immunoassay screening tests that can detect the presence of those compounds. In this Article, the voltammetric behavior of 25B NBOMe and 25I NBOMe were investigated and their electroanalytical characteristics determined for the first time. A novel, fast, and sensitive screening method for the identification of the two most common NBOMes (25B-NBOMe and 25I-NBOMe) in real samples is reported. The method uses the electrochemical oxidation of these molecules to produce an analytical signal that can be related to the NBOMe concentration with an average lower limit of quantitation of 0.01 mg/mL for both of them. The method is selective enough to identify the two compounds individually, even given the great similarity in their structure.


Asunto(s)
Técnicas Electroquímicas/métodos , Fenetilaminas/análisis , Psicotrópicos/análisis , Anisoles/análisis , Dimetoxifeniletilamina/análogos & derivados , Dimetoxifeniletilamina/análisis , Medicina Legal , Concentración de Iones de Hidrógeno , Límite de Detección , Fenetilaminas/química , Psicotrópicos/química
17.
Rapid Commun Mass Spectrom ; 30 Suppl 1: 141-6, 2016 08.
Artículo en Inglés | MEDLINE | ID: mdl-27539429

RESUMEN

RATIONALE: With the amounts and types of new psychoactive substances (NPSs) increasing rapidly in recent years, an excellent high-throughput method for the analysis of these compounds is urgently needed. In this article, a rapid screening method and a quantitative analysis method for 11 NPSs are described and compared, respectively. METHOD: A simple direct analysis in real time mass spectrometry (DART-MS) method was developed for the analysis of 11 NPSs including three categories of these substances present on the global market such as four cathinones, one phenylethylamine, and six synthetic cannabinoids. In order to analyze these compounds quantitatively with better accuracy and sensitivity, another rapid analytical method with a low limit of detection (LOD) was also developed using liquid chromatography/electrospray ionization quadrupole time-of-flight mass spectrometry (LC/QTOFMS). RESULTS: The 11 NPSs could be determined within 0.5 min by DART-MS. Furthermore, they could also be separated and determined within 5 min by the LC/QTOFMS method. The two methods both showed good linearity with correlation coefficients (r(2) ) higher than 0.99. The LODs for all these target NPSs by DART-MS and LC/QTOFMS ranged from 5 to 40 ng mL(-1) and 0.1 to 1 ng mL(-1) , respectively. Confiscated samples, named as "music vanilla" and "bath salt", and 11 spiked samples were firstly screened by DART-MS and then determined by LC/QTOFMS. CONCLUSIONS: The identification of NPSs in confiscated materials was successfully achieved, and the proposed analytical methodology could offer rapid screening and accurate analysis results. Copyright © 2016 John Wiley & Sons, Ltd.


Asunto(s)
Cromatografía Liquida/métodos , Espectrometría de Masas/métodos , Psicotrópicos/análisis , Cannabinoides/análisis , Ensayos Analíticos de Alto Rendimiento/métodos , Límite de Detección , Fenetilaminas/análisis , Reproducibilidad de los Resultados , Espectrometría de Masa por Ionización de Electrospray/métodos
18.
Anal Bioanal Chem ; 408(24): 6703-9, 2016 Sep.
Artículo en Inglés | MEDLINE | ID: mdl-27438720

RESUMEN

The use of potential mutagenic nitrofuran antibiotic in food animal production has been banned world-wide. Common methods for nitrofuran detection involve complex extraction procedures. In the present study, magnetic beads functionalized with antibody against nitrofuran derivative were used as both the extraction and color developing media in lateral flow biosensor. Derivatization reagent carboxybenzaldehyde is firstly modified with ractopamine. After reaction with nitrofuran metabolites, the resultant molecule has two functional groups: the metabolite moiety and the ractopamine moiety. Metabolite moiety is captured by the antibody that is coated on magnetic beads. This duplex is then loaded onto biosensor and ractopamine moiety is further captured by the antibody immobilized on the test zone of nitrocellulose membrane. Without tedious organic reagent-based extraction procedure, this biosensor was capable of visually detecting four metabolites simultaneously with a detection limit of 0.1 µg/L. No cross-reactivity was observed in the presence of 50 µg/L interferential components. Graphical abstract Derivatization of nitrofuran metabolites (AHD, AOZ, SEM, or AMOZ) and LFA detection of the derivative products.


Asunto(s)
Anticuerpos Inmovilizados/química , Técnicas Biosensibles/instrumentación , Nitrofuranos/análisis , Tiras Reactivas/análisis , Animales , Anticuerpos Monoclonales/química , Diseño de Equipo , Cabras , Límite de Detección , Imanes/química , Ratones , Nitrofuranos/metabolismo , Fenetilaminas/análisis
19.
J Nanosci Nanotechnol ; 16(1): 548-54, 2016 Jan.
Artículo en Inglés | MEDLINE | ID: mdl-27398486

RESUMEN

In this paper, a sensitive method for the colorimetric detection of clenbuterol and ractopamine using citrate-stabilized gold nanoparticles (AuNPs) as probe was developed. The concentration of clenbuterol and ractopamine could be determined with naked eyes or a UV-vis spectrometer. By optimizing the influence of NaHSO4 and incubation time, clenbuterol could be detected in the linear range of 0.1-4 µg/mL with the detection limit of 0.0158 µg/mL, and ractopamine could be detected in the linear range of 1-9 µg/mL with the detection limit of 0.0229 µg/mL. The proposed method could be successfully applied to detect clenbuterol and ractopamine in pig urines by a simple pre-treatment with excellent recoveries. The proposed colorimetric assay exhibits good reproducibility and accuracy, providing a simple and rapid method for the analysis of clenbuterol and ractopamine.


Asunto(s)
Clenbuterol/análisis , Oro/química , Nanopartículas del Metal/química , Fenetilaminas/análisis , Colorimetría/métodos
20.
J Environ Sci (China) ; 45: 40-8, 2016 Jul.
Artículo en Inglés | MEDLINE | ID: mdl-27372117

RESUMEN

The feed additive ractopamine hydrochloride was fortified at four concentrations into batch vials containing soils that differed in both biological activity and organic matter (OM). Sampling of the liquid layer for 14days demonstrated that ractopamine rapidly dissipated from the liquid layer. Less than 20% of the fortified dose remained in the liquid layer after 4hr, and recoveries of dosed ractopamine ranged from 8 to 18% in the liquid layer at 336hr. Sorption to soil was the major fate for ractopamine in soil:water systems, i.e., 42%-51% of the dose at 14days. The major portion of the sorbed fraction was comprised of non-extractables; a smaller fraction of the sorbed dose was extracted into water and acetone, portions which would be potentially mobile in the environment. Partitioning coefficients for all soils suggested strong sorption of ractopamine to soil which is governed by hydrophobic interactions and cation exchange complexes within the soil OM. Ractopamine degradation was observed, but to mostly non-polar compounds which had a higher potential than ractopamine to sorb to soil. The formation of volatiles was also suggested. Therefore, despite rapid and extensive soil sorption, these studies indicated a portion of ractopamine, present in manures used to fertilize soils, may be mobile in the environment via water-borne events.


Asunto(s)
Agonistas Adrenérgicos/análisis , Modelos Químicos , Fenetilaminas/análisis , Contaminantes del Suelo/análisis , Monitoreo del Ambiente , Interacciones Hidrofóbicas e Hidrofílicas , Suelo/química , Agua/química
SELECCIÓN DE REFERENCIAS
DETALLE DE LA BÚSQUEDA