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1.
Nat Biomed Eng ; 5(1): 64-76, 2021 01.
Artigo em Inglês | MEDLINE | ID: mdl-33483710

RESUMO

The detection and quantification of protein biomarkers in interstitial fluid is hampered by challenges in its sampling and analysis. Here we report the use of a microneedle patch for fast in vivo sampling and on-needle quantification of target protein biomarkers in interstitial fluid. We used plasmonic fluor-an ultrabright fluorescent label-to improve the limit of detection of various interstitial fluid protein biomarkers by nearly 800-fold compared with conventional fluorophores, and a magnetic backing layer to implement conventional immunoassay procedures on the patch and thus improve measurement consistency. We used the microneedle patch in mice for minimally invasive evaluation of the efficiency of a cocaine vaccine, for longitudinal monitoring of the levels of inflammatory biomarkers, and for efficient sampling of the calvarial periosteum-a challenging site for biomarker detection-and the quantification of its levels of the matricellular protein periostin, which cannot be accurately inferred from blood or other systemic biofluids. Microneedle patches for the minimally invasive collection and analysis of biomarkers in interstitial fluid might facilitate point-of-care diagnostics and longitudinal monitoring.


Assuntos
Biomarcadores/análise , Líquido Extracelular/química , Microtecnologia/instrumentação , Agulhas , Animais , Cocaína/análise , Citocinas/análise , Desenho de Equipamento , Feminino , Corantes Fluorescentes/química , Técnicas de Imunoadsorção/instrumentação , Limite de Detecção , Masculino , Camundongos , Camundongos Endogâmicos BALB C , Camundongos Endogâmicos C57BL
2.
J Anal Toxicol ; 44(8): 851-860, 2020 Dec 10.
Artigo em Inglês | MEDLINE | ID: mdl-33313888

RESUMO

Spectroscopic techniques combined with chemometrics are a promising tool for analysis of seized drug powders. In this study, the performance of three spectroscopic techniques [Mid-InfraRed (MIR), Raman and Near-InfraRed (NIR)] was compared. In total, 364 seized powders were analyzed and consisted of 276 cocaine powders (with concentrations ranging from 4 to 99 w%) and 88 powders without cocaine. A classification model (using Support Vector Machines [SVM] discriminant analysis) and a quantification model (using SVM regression) were constructed with each spectral dataset in order to discriminate cocaine powders from other powders and quantify cocaine in powders classified as cocaine positive. The performances of the models were compared with gas chromatography coupled with mass spectrometry (GC-MS) and gas chromatography with flame-ionization detection (GC-FID). Different evaluation criteria were used: number of false negatives (FNs), number of false positives (FPs), accuracy, root mean square error of cross-validation (RMSECV) and determination coefficients (R2). Ten colored powders were excluded from the classification data set due to fluorescence background observed in Raman spectra. For the classification, the best accuracy (99.7%) was obtained with MIR spectra. With Raman and NIR spectra, the accuracy was 99.5% and 98.9%, respectively. For the quantification, the best results were obtained with NIR spectra. The cocaine content was determined with a RMSECV of 3.79% and a R2 of 0.97. The performance of MIR and Raman to predict cocaine concentrations was lower than NIR, with RMSECV of 6.76% and 6.79%, respectively and both with a R2 of 0.90. The three spectroscopic techniques can be applied for both classification and quantification of cocaine, but some differences in performance were detected. The best classification was obtained with MIR spectra. For quantification, however, the RMSECV of MIR and Raman was twice as high in comparison with NIR. Spectroscopic techniques combined with chemometrics can reduce the workload for confirmation analysis (e.g., chromatography based) and therefore save time and resources.


Assuntos
Cocaína/análise , Cromatografia Gasosa-Espectrometria de Massas , Pós/análise , Análise Espectral
3.
J Chromatogr A ; 1633: 461629, 2020 Dec 06.
Artigo em Inglês | MEDLINE | ID: mdl-33128968

RESUMO

In this paper, a low-cost, rapid, easy, and potentially portable tool for the identification of cocaine and its semi-quantitative determination in oral fluid has been proposed. A field collection device has been designed, based on a cotton pad with an indicator and a molecularly imprinted polymer (MIP) sorbent, to selective retain cocaine from oral fluid components. After sample collection, cocaine is transferred by using phosphate buffer to the MIP and then eluted with 2-propanol. The obtained extract is analysed by ion mobility spectrometry (IMS), providing a cut-off value of 20 µg L-1 that identifies 100 % true-positive and 95 % true-negative samples. The MIP-IMS procedure has been validated by the analysis of oral fluid samples, collected from cocaine users at recreation environments, by comparing the results with lateral flow immunoassay and chromatographic reference methods. Thus, the proposed methodology allows a simple and fast cocaine identification that can be carried out in field by non-specialized personnel, such as health personnel, law enforcement bodies, and customs staff.


Assuntos
Cocaína/análise , Impressão Molecular , Saliva/química , Detecção do Abuso de Substâncias/instrumentação , Detecção do Abuso de Substâncias/métodos , Humanos , Espectrometria de Mobilidade Iônica , Polímeros/química
4.
Environ Sci Pollut Res Int ; 27(36): 45063-45075, 2020 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-32779066

RESUMO

The occurrence of pharmaceuticals and illicit drugs in water resources is widely documented in Europe, North America and Asia. However, in South America, these studies are still incipient. The objective of this study was to screen and identify the presence of pharmaceuticals of various therapeutic classes, including illicit drugs such as cocaine and its metabolite benzoylecgonine, in urban drainage channels that flow into the bathing waters of Guarujá city, State of São Paulo, Brazil. Moreover, the ecological potential risks to the aquatic biota were also assessed. The water samples were collected from four beaches of Guarujá in two different points: in the urban drainage channels and in the nearby coast line. A total of 16 compounds were detected using liquid chromatography coupled with tandem mass spectrometry: carbamazepine (0.1-8.0 ng/L), caffeine (33.5-6550.0 ng/L), cocaine (0.2-30.3 ng/L), benzoylecgonine (0.9-278.0 ng/L), citalopram (0.2-0.4 ng/L), acetaminophen (18.3-391.0 ng/L), diclofenac (0.9-79.8 ng/L), orphenadrine (0.2-1.5 ng/L), atenolol (0.1-140.0 ng/L), propranolol (limit of detection: LOD-0.9 ng/L), enalapril (2.2-3.8 ng/L), losartan (3.6-548.0 ng/L), valsartan (19.8-798.0 ng/L), rosuvastatin (2.5-38.5 ng/L), chlortalidone (0.1-0.4 ng/L) and clopidogrel (0.1-0.2 ng/L). The hereby data also showed that five of these compounds, namely caffeine, acetaminophen, diclofenac, losartan and valsartan, could raise moderate to severe risks to aquatic organisms (algae, crustaceans and fishes). This study is the first report of the occurrence of several pharmaceuticals and illicit drugs in urban drainage channels that flow to the bathing waters in South America, and it is the first quantification of rosuvastatin, chlortalidone and clopidogrel in environmental marine waters of Latin America.


Assuntos
Cocaína , Preparações Farmacêuticas , Poluentes Químicos da Água , Ásia , Brasil , Cidades , Cocaína/análise , Monitoramento Ambiental , Europa (Continente) , América do Norte , Medição de Risco , Poluentes Químicos da Água/análise
5.
Chemosphere ; 261: 127628, 2020 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-32731016

RESUMO

BACKGROUND: Polycyclic aromatic hydrocarbons (PAHs) are the risk factors for workers' neurological performance, which were widely exist in the occupational environment. OBJECTIVE: We aimed to investigate the dose-response relationship between various PAH metabolites and workers' neurobehavioral changes and to explore whether mitochondrial DNA copy number (mtDNAcn) can be used as a potential biomarker to reflect changes in neurobehavioral behavior. METHOD: A total of 697 workers were recruited from a coke oven plant. The concentrations of eleven PAHs metabolites were determined by HPLC-MS/MS. Peripheral blood mtDNAcn was measured using QPCR. Neurobehavioral function was measured by NCTB questionnaire. The dose-response relationships were evaluated using restricted cubic spline models. Mediation analysis was also carried out. RESULTS: We found dose-response relationships between urinary 2-hydroxynaphthalene (2-OH Nap), sum of PAH metabolites (Æ© -OH PAHs) and total digit span (DSP), backward digit span (DSPB), forward digit span (DSPF) and mtDNAcn. Each one-unit increase in ln-transformed of 2-OH Nap or Æ© -OH PAHs was associated with a 2.64 or 3.22 decrease in DSP, a 1.20 or 1.58 decrease in DSPF, a 1.44 or 1.62 decrease in DSPB and a 0.13 or 0.12 decrease in mtDNAcn. However, we did not find a significant mediation effect of mtDNAcn between PAHs metabolites and DSP, DSPF, or DSPB. CONCLUSION: Our data indicated that workers urinary 2-hydroxynaphthalene and sum of PAH metabolites levels were inversely associated with mtDNAcn and neurobehavior, especially their auditory memory. However, there was no significant mediation effect of mtDNAcn between urinary PAHs metabolites and neurobehavior.


Assuntos
Exposição Ocupacional/análise , Hidrocarbonetos Policíclicos Aromáticos/urina , Adulto , Biomarcadores , Cocaína/análise , Coque/análise , Variações do Número de Cópias de DNA , DNA Mitocondrial/genética , Feminino , Humanos , Masculino , Mitocôndrias/metabolismo , Hidrocarbonetos Policíclicos Aromáticos/análise , Espectrometria de Massas em Tandem
6.
Biosensors (Basel) ; 10(3)2020 Mar 04.
Artigo em Inglês | MEDLINE | ID: mdl-32143406

RESUMO

The development of a sensor based on molecularly imprinted polymer nanoparticles (nanoMIPs) and electrochemical impedance spectroscopy (EIS) for the detection of trace levels of cocaine is described in this paper. NanoMIPs for cocaine detection, synthesized using a solid phase, were applied as the sensing element. The nanoMIPs were first characterized by Transmission Electron Microscopy (TEM) and Dynamic Light Scattering and found to be ~148.35 ± 24.69 nm in size, using TEM. The nanoMIPs were then covalently attached to gold screen-printed electrodes and a cocaine direct binding assay was developed and optimized, using EIS as the sensing principle. EIS was recorded at a potential of 0.12 V over the frequency range from 0.1 Hz to 50 kHz, with a modulation voltage of 10 mV. The nanoMIPs sensor was able to detect cocaine in a linear range between 100 pg mL-1 and 50 ng mL-1 (R2 = 0.984; p-value = 0.00001) and with a limit of detection of 0.24 ng mL-1 (0.70 nM). The sensor showed no cross-reactivity toward morphine and a negligible response toward levamisole after optimizing the sensor surface blocking and assay conditions. The developed sensor has the potential to offer a highly sensitive, portable and cost-effective method for cocaine detection.


Assuntos
Técnicas Biossensoriais/métodos , Cocaína/química , Técnicas Eletroquímicas/métodos , Impressão Molecular/métodos , Nanopartículas/química , Cocaína/análise , Humanos
7.
Talanta ; 211: 120662, 2020 May 01.
Artigo em Inglês | MEDLINE | ID: mdl-32070623

RESUMO

The aim of the current study was to develop and validate an analytical method to determine whether drugs of abuse (DOA) were present in oral fluid (OF) using a newly-developed, portable capillary electrophoresis (CE) instrument coupled to a deep ultra-violet fluorescence detector (FD). The performance of this portable CE-FD DOA analyser was tested at the Weekend Festival Baltic (Pärnu, Estonia) between 2016 and 2018 as well as on the roadside OF samples collected by the police. The study reported 128 analysed cases in which persons were allegedly found to have been under the influence of DOA. The samples were analysed for amphetamine (AMP), methamphetamine (METH), 3,4-methylenedioxy-methamphetamine (MDMA), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxy-N-ethylamphetamine (MDEA), cocaine (COC) and cocaethylene (COET). Subsequent toxicological reports revealed that 26% cases were negative, and 74% were positive. The most frequently detected and quantified DOA was MDMA (68 cases, 62%). A comparative study was conducted to validate the accuracy of using the CE-FD DOA analyser versus classic high-performance liquid chromatography coupled to mass spectrometry (HPLC-ESI-MS). Diagnostic statistics for CE-FD DOA were also evaluated and were higher than 99.5%. In addition, all zeta-scores were lower than 2 when both methods were compared, showing that the CE-FD analyser can be implemented as a reliable, sensitive and convenient tool for roadside and workplace testing for DOA.


Assuntos
Anfetaminas/análise , Cocaína/análogos & derivados , Drogas Ilícitas/análise , Saliva/química , Detecção do Abuso de Substâncias/métodos , Adulto , Idoso , Cocaína/análise , Feminino , Fluorescência , Humanos , Masculino , Pessoa de Meia-Idade , Adulto Jovem
8.
J Environ Sci Health B ; 55(5): 455-461, 2020.
Artigo em Inglês | MEDLINE | ID: mdl-31941387

RESUMO

The use and abuse of prescription and illicit drugs are on the rise worldwide and as a result residue of these drugs and their metabolites are continually being disposed into the environment through sewage system and other means. Therefore, this paper reports on the development of a cost-effective, simple and sensitive approach that involved the fabrication of an electrochemical sensor from exfoliated graphite (EG) and gold nanoparticles (AuNPs) for the detection of selected psychoactive drugs in water. The fabricated electrochemical sensor was characterized using scanning electron microscopy coupled with energy dispersive X-ray spectroscopy (SEM-EDS) to ascertain its surface morphology characteristics and cyclic voltammetry (CV) for ascertaining the redox potential peak. The EG-AuNPs sensor was able to detect cocaine in water with limit of detection (LOD) and limit quantification (LOQ) of 0.82 and 2.74 µg/L, respectively under the pH of 12.25. The sensor was extended on other psychoactive drugs (methylphenidate, amphetamine and heroin) and one metabolite (6-acetylmorphine) to examine its applicability. The drugs were distinctively detected, and thus making EG-AuNPs electrode a possible alternative sensor for electrochemical detection of psychoactive drugs and their metabolites in synthetic and real water samples.


Assuntos
Técnicas Eletroquímicas/instrumentação , Eletrodos , Nanopartículas Metálicas/química , Psicotrópicos/análise , Técnicas Biossensoriais , Cocaína/análise , Técnicas Eletroquímicas/métodos , Ouro/química , Grafite/química , Concentração de Íons de Hidrogênio , Limite de Detecção , Microscopia Eletrônica de Varredura , Espectrometria por Raios X , Poluentes Químicos da Água/análise
9.
Nanomedicine (Lond) ; 15(4): 325-335, 2020 02.
Artigo em Inglês | MEDLINE | ID: mdl-31976806

RESUMO

Aim: The current work highlighted a novel colorimetric sensor based on aptamer and molybdenum disulfide (MoS2)-gold nanoparticles (AuNPs) that was developed for cocaine detection with high sensitivity. Materials & methods: Due to the presence of the plasmon resonance band on the surface of AuNPs, AuNPs aggregated and the color was changed from red to blue after adding a certain concentration of NaCl. We used MoS2 to optimize the sensing system of AuNPs. The folded conformation of the aptamer in combination with cocaine enhanced the salt tolerance of the MoS2-AuNPs, effectively preventing their aggregation. Results & conclusion: The detection limit of cocaine was 7.49 nM with good selectivity. The method based on MoS2-AuNPs colorimetry sensor is simple, quick, label-free and low cost.


Assuntos
Aptâmeros de Nucleotídeos/química , Cocaína/análise , Dissulfetos/química , Ouro/química , Nanopartículas Metálicas/química , Molibdênio/química , Técnicas Biossensoriais/métodos
10.
Mikrochim Acta ; 187(2): 104, 2020 01 08.
Artigo em Inglês | MEDLINE | ID: mdl-31912290

RESUMO

Authors report on a new fluoro-graphene-plasmonic nanohybrid aptamer-based fluorescent nanoprobe for cocaine. To construct the nanoprobe, newly synthesized glutathione-capped ZnS/Ag2Se quantum dots (QDs) were first conjugated to graphene oxide (GO) to form a QD-GO nanocomposite. The binding interaction resulted in a fluorescence turn-ON. Thereafter, cetyltrimethylammonium bromide (CTAB)-gold nanoparticles (AuNPs) were directly adsorbed on the QD-GO nanocomposite to form a novel QD-GO-CTAB-AuNP nanohybrid assembly that resulted in a fluorescence turn-OFF. Streptavidin (strep) was then adsorbed on the QDs-GO-CTAB-AuNP nanohybrid assembly which allowed binding to a biotinylated MNS 4.1 anticocaine DNA aptamer (B) receptor. The addition of cocaine into the strep-B-QDs-GO-CTAB-AuNP aptamer nanoprobe system aided affinity to the aptamer receptor and in turn turned on the fluorescence of the nanoprobe in a concentration-dependent manner. Under optimum experimental conditions, we found the strep-B-QD-GO-CTAB-AuNP to be far superior in its sensitivity to cocaine than the tested strep-B-QDs (no GO and CTAB-AuNPs), strep-B-QD-CTAB-AuNP (no GO) and strep-B-QD-GO (no CTAB-AuNP). In addition, the investigation of localized surface plasmon resonance (LSPR) amplified signal from tested plasmonic NPs shows that CTAB-AuNPs was far superior in amplifying the fluorescence signal of the nanoprobe. A detection limit of 4.6 nM (1.56 ng.mL-1), rapid response time (~2 min) and excellent selectivity against other drugs, substances and cocaine metabolites was achieved. The strep-B-QD-GO-CTAB-AuNP aptamer-based fluorescent nanoprobe was successfully applied for the determination of cocaine in seized adulterated cocaine samples. Graphical abstractSchematic representation of the streptavidin-biotin-quantum dot-graphene oxide-cetyltrimethylammonium bromide-gold nanoparticle aptamer-based fluorescent nanoprobe for cocaine.


Assuntos
Aptâmeros de Nucleotídeos/química , Técnicas Biossensoriais/métodos , Cocaína/análise , Pontos Quânticos/química , Compostos de Selênio/química , Compostos de Prata/química , Sulfetos/química , Compostos de Zinco/química , Inibidores da Captação de Dopamina/análise , Contaminação de Medicamentos , Corantes Fluorescentes/química , Glutationa/química , Ouro/química , Grafite/química , Drogas Ilícitas/análise , Limite de Detecção , Nanopartículas Metálicas/química , Nanocompostos/química , Espectrometria de Fluorescência/métodos
11.
Sci Total Environ ; 698: 134207, 2020 Jan 01.
Artigo em Inglês | MEDLINE | ID: mdl-31499350

RESUMO

This study used wastewater-based epidemiology (WBE) to investigate the lifestyle of the inhabitants of Malé, the capital of the Republic of Maldives. Raw wastewater 12-h composite samples were collected from nine pumping stations serving the city area - thus representative of the whole Malé population. Samples were analysed by liquid chromatography coupled to mass spectrometry for estimating the profile of use of a large number of substances including illicit drugs, alcohol, caffeine, tobacco and pharmaceuticals. The illicit drugs most used were cannabis (THC) and heroin (700 and 18 g/day), with lower consumption of cocaine and amphetamines (0.1-1.2 g/day). It is important to note that the consumption of cannabis in Malé was comparable to that measured in other countries, while the consumption of heroin was higher. Among cathinones, mephedrone was detected at the highest levels similar to other countries. Consumption of alcohol, which is not allowed in Maldives, was found (1.3 L/day/1000 inhabitants), but at a low level compared with other countries (6-44 L/day/1000 inhabitants), while the consumption of caffeine and tobacco was generally in line with reports from other countries. Unique information on pharmaceuticals use was also provided, since no official data were available. Human lifestyle was evaluated by applying for the first time the full set of WBE methodologies available in our laboratory. Results provided valuable epidemiological information, which may be useful for national and international agencies to understand population lifestyles better, including illicit drug issues, and for planning and evaluation of drug prevention programs in Malé.


Assuntos
Drogas Ilícitas/análise , Águas Residuárias/química , Poluentes Químicos da Água/análise , Anfetaminas/análise , Cafeína/análise , Cocaína/análise , Humanos , Ilhas do Oceano Índico , Detecção do Abuso de Substâncias , Transtornos Relacionados ao Uso de Substâncias/epidemiologia
12.
Anal Chim Acta ; 1096: 89-99, 2020 Feb 01.
Artigo em Inglês | MEDLINE | ID: mdl-31883595

RESUMO

We report the on-line coupling of a monolithic molecularly imprinted polymer to nano-liquid chromatography for the selective analysis of cocaine and its main metabolite, benzoylecgonine, in complex biological samples. After the screening of different synthesis conditions, a monolithic molecularly imprinted polymer was in situ synthesized into a 100 µm internal diameter fused-silica capillary using cocaine as template, methacrylic acid as functional monomer, and trimethylolpropane trimethacrylate as cross-linker. Scanning electron microscopy was used to assess the homogeneous morphology of the molecularly imprinted polymer and its permeability was measured. Its selectivity was evaluated by nano-liquid chromatography-ultraviolet, leading to imprinting factors of 3.2 ±â€¯0.5 and 2.2 ±â€¯0.3 for cocaine and benzoylecgonine, respectively, on polymers resulting from three independent syntheses, showing the high selectivity and the repeatability of the synthesis. After optimizing the extraction protocol to promote selectivity, the monolithic molecularly imprinted polymer was successfully on-line coupled with nano-liquid chromatography-ultraviolet for the direct extraction and analysis of cocaine present in spiked human plasma and saliva samples. The repeatability of the obtained extraction recovery, between 85.4 and 98.7% for a plasma sample spiked at 100 ng mL-1, was high with relative standard deviation values lower than 5.8% for triplicate analyses on each of the three independently synthesized molecularly imprinted polymers. A linear calibration range was achieved between 100 and 2000 ng mL-1 (R2 = 0.999). Limits of quantification of 14.5 ng mL-1 and 6.1 ng mL-1 were achieved in plasma and urine samples, respectively. The very clean-baseline of the resulting chromatogram illustrated the high selectivity brought by the monolithic molecularly imprinted polymer that allows the removal of a huge peak corresponding to the elution of interfering compounds and the easy determination of the target analyte in these complex biological samples.


Assuntos
Anestésicos Locais/isolamento & purificação , Cromatografia Líquida/métodos , Cocaína/isolamento & purificação , Metacrilatos/química , Impressão Molecular/métodos , Anestésicos Locais/análise , Anestésicos Locais/sangue , Cromatografia Líquida/instrumentação , Cocaína/análise , Cocaína/sangue , Reagentes para Ligações Cruzadas/química , Desenho de Equipamento , Humanos , Limite de Detecção , Impressão Molecular/instrumentação , Saliva/química , Extração em Fase Sólida/instrumentação , Extração em Fase Sólida/métodos
13.
Talanta ; 208: 120353, 2020 Feb 01.
Artigo em Inglês | MEDLINE | ID: mdl-31816720

RESUMO

A porous and hydrophilic sorbent material was used in an extraction system, assisted by electric fields, for the extraction of cocaine in saliva and subsequent determination by ultra-high-performance liquid chromatography associated with sequential triple quadrupole mass spectrometry (UHPLC-MS/MS). The cellulose-based material was characterized by scanning electron microscopy, infrared spectroscopy, thermogravimetric analysis, and X-ray diffraction. The time and voltage variables applied in the extraction process were investigated through a Doehlert experimental design, and with the best conditions found (35min and 300 V) some validation parameters were evaluated. The established working range was 1-100 µg L-1 (R2 > 0.99), and the detection and quantification limits determined were 0.3 and 0.8 µg L-1, respectively. Recoveries from 80 to 115% and coefficient of variation ≤15 and 16% for intra-day and inter-day assays, respectively, were obtained for sample concentrations of LOQ, 5, 25, and 75 µg L-1, indicating satisfactory accuracy and precision for the proposed method. In addition, the method presented no matrix effect, and the extraction efficiency was between 56 and 70%. The results showed that the material used has adequate physicochemical characteristics and can be applied as a sorbent and electrolyte support in multiphase extractions using electric fields.


Assuntos
Celulose/química , Cromatografia Líquida de Alta Pressão/métodos , Cocaína/análise , Cocaína/isolamento & purificação , Saliva/metabolismo , Extração em Fase Sólida/métodos , Espectrometria de Massas em Tandem/métodos , Fenômenos Eletromagnéticos , Humanos , Interações Hidrofóbicas e Hidrofílicas , Saliva/química , Saliva Artificial/química , Saliva Artificial/metabolismo , Extração em Fase Sólida/instrumentação
14.
J Forensic Sci ; 65(2): 563-569, 2020 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-31498435

RESUMO

A method using liquid chromatography-tandem mass spectrometry (LC-MS/MS) to simultaneously quantify amphetamines, opiates, ketamine, cocaine, and metabolites in human hair is described. Hair samples (50 mg) were extracted with methanol utilizing cryogenic grinding. Calibration curves for all the analytes were established in the concentration range 0.05-10 ng/mg. The recoveries were above 72%, except for AMP at the limit of quantification (LOQ), which was 48%. The accuracies were within ±20% at the LOQ (0.05 ng/mg) and between -11% and 13.3% at 0.3 and 9.5 ng/mg, respectively. The intraday and interday precisions were within 19.6% and 19.8%, respectively. A proficiency test was applied to the validated method with z-scores within ±2, demonstrating the accuracy of the method for the determination of drugs of abuse in the hair of individuals suspected of abusing drugs. The hair concentration ranges, means, and medians are summarized for abused drugs in 158 authentic cases.


Assuntos
Cromatografia Líquida , Cabelo/química , Entorpecentes/análise , Detecção do Abuso de Substâncias/métodos , Transtornos Relacionados ao Uso de Substâncias/diagnóstico , Espectrometria de Massas em Tandem , Adulto , Anfetaminas/análise , Cocaína/análise , Feminino , Toxicologia Forense/métodos , Humanos , Ketamina/análise , Limite de Detecção , Masculino , Pessoa de Meia-Idade , Alcaloides Opiáceos/análise
15.
Drug Alcohol Depend ; 204: 107508, 2019 11 01.
Artigo em Inglês | MEDLINE | ID: mdl-31670189

RESUMO

BACKGROUND: The aim of the present study is to describe the prevalence of NPS and conventional DOA in Paris and its suburbs over a six-year period using hair testing approach. METHOD: Hair was sampled in patients admitted to different departments of Paris hospitals between 2012 and 2017. Two high-risk populations were mainly considered: 1) drug-dependent and 2) acutely intoxicated patients. Segmental hair analysis was performed by validated LC-MS/MS method to screen for DOA and 83 NPS. RESULTS: 480 patients (280 M/200 F, 15-70 years) were included. 141 patients tested positive for NPS (99 M/42 F; median age: 33). NPS prevalence was 29%, that of amphetamines, cocaine and opioids were 32%, 38.5% and 52%, respectively. 27 NPS were identified, 4-MEC and mephedrone (number of cases n = 24 each) were the most detected cathinones. JWH-122 (n = 1) was the only detected synthetic cannabinoid while ketamine (n = 104) was present in numerous NPS users (67%). 3-fluorofentanyl (n = 1), furanylfentanyl (n = 1), N-ethylpentylone (n = 2), pentedrone (n = 2), mexedrone (n = 1), methcathinone (n = 3), 6-APDB (n = 2), TFMPP (n = 2), 2-CE (n = 1), 3,4-MD-αPHP (n = 1) and dextromethorphan (n = 27) were identified for the first time in hair. Users were found to have more than one NPS in 53% of cases, mostly in combination with conventional DOA. The number of detected NPS rose from 5 in 2012 to 42 in 2017. A broad range of hair concentrations (0.001-318 ng/mg) was found, but the low median concentrations seem to show an occasional exposure more than chronic use. CONCLUSION: NPS screening should be assessed in routine clinical practice, especially in high-risk populations.


Assuntos
Drogas Ilícitas/análise , Detecção do Abuso de Substâncias/métodos , Transtornos Relacionados ao Uso de Substâncias/epidemiologia , Adulto , Anfetaminas/análise , Analgésicos Opioides/análise , Cromatografia Líquida/métodos , Cocaína/análise , Estudos Transversais , Feminino , Cabelo/química , Humanos , Masculino , Paris/epidemiologia , Prevalência , Transtornos Relacionados ao Uso de Substâncias/diagnóstico , Espectrometria de Massas em Tandem/métodos
17.
Rev Esp Salud Publica ; 932019 Nov 26.
Artigo em Espanhol | MEDLINE | ID: mdl-31767827

RESUMO

OBJECTIVE: The basic sources of information on drug use are epidemiological surveys, although they have some limitations: their results may be conditioned by the lack of veracity of the responses and the sampling method makes it difficult to detect lowprevalence behaviours in target populations. This study aimed to establish the epidemiological pattern of drug use in the population undergoing drug testing in hair, in the framework of judicial investigations, in order to provide an additional approach to the knowledge of high-risk drug use. METHODS: A cross-sectional study on drug use was conducted on the population subjected to drug testing in hair (N=5,292) in the forensic context. Prevalence of cannabis, cocaine, heroin, ketamine, amphetamine (AP), methamphetamine (MA), 3,4-methylenedioxy- methamphetamine (MDMA), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxy-N-ethylamphetamine (MDEA) and methadone uses were obtained. Association between drug use and demographics, and trends of prevalence over the period were analysed using the Pearson Chi-square test. Frequency distribution of drug concentrations in hair was obtained and it was assessed in relation to gender and age using the non-parametric Mann-Whitney U and Kruskal-Wallis H methods. RESULTS: During the period 2013-2015, prevalence of cocaine use was particularly high (49%), rating second among the population studied, after cannabis use (54%). Proportions of heroin, methadone, MDMA and amphetamine use ranged from 10% to 18%. There was a significant increase in prevalence of MDMA, heroin and amphetamine use during the period 2013-2015, as well as a significant decrease in methadone use. The rates of cannabis, cocaine and MDMA use were higher in men, whereas methadone use was higher among women. CONCLUSIONS: Cannabis and cocaine are the most frequently abused drugs among the population undergoing drug testing in hair in the framework of judicial investigations over the three-year period, although the proportions of heroin, MDMA and amphetamine users show an increasing trend. Drug use patterns vary according to age and sex, with a decrease in cannabis and MDMA use and an increase in heroin and methadone use as age increased; cannabis, cocaine and MDMA use are more prevalent among men and methadone use among women.


Assuntos
Cabelo/química , Detecção do Abuso de Substâncias/métodos , Transtornos Relacionados ao Uso de Substâncias/diagnóstico , 3,4-Metilenodioxianfetamina/análogos & derivados , 3,4-Metilenodioxianfetamina/análise , Adolescente , Adulto , Anfetamina/análise , Canabinoides/análise , Cocaína/análise , Estudos Transversais , Feminino , Ciências Forenses , Cromatografia Gasosa-Espectrometria de Massas , Heroína/análise , Humanos , Drogas Ilícitas , Ketamina/análise , Masculino , Metadona/análise , Metanfetamina/análise , Pessoa de Meia-Idade , N-Metil-3,4-Metilenodioxianfetamina/análise , Prevalência , Espanha/epidemiologia , Transtornos Relacionados ao Uso de Substâncias/epidemiologia , Adulto Jovem
18.
Anal Chem ; 91(22): 14514-14521, 2019 11 19.
Artigo em Inglês | MEDLINE | ID: mdl-31614078

RESUMO

Structure-switching aptamers (SSAs) offer a promising recognition element for sensor development. However, the generation of SSAs via in vitro aptamer selection technologies or postselection engineering is challenging. Inspired by the two-domain structure of antibodies, we have devised a simple, universal strategy for engineering aptamers into SSAs with signal reporting functionality. These constructs consist of a "constant" domain, comprising a split DNAzyme G-quadruplex (G4) region for signal transduction, and a "variable" domain, comprising an aptamer sequence capable of specific target binding. In the absence of target, the G4-SSA construct folds into a parallel G4 structure with high peroxidase catalytic activity. Target binding disrupts the G4 structure, resulting in low enzymatic activity. We demonstrate that this change in DNAzyme activity enables sensitive and specific colorimetric detection of diverse targets including Hg2+, thrombin, sulfadimethoxine, cocaine, and 17ß-estradiol. G4-SSAs can also achieve label-free fluorescence detection of various targets using a specific G4-binding dye. We demonstrate that diverse aptamers can be readily engineered into G4-SSA constructs independent of target class, binding affinity, aptamer length, or structure. This design strategy could broadly extend the power, accessibility, and utility of numerous SSA-based biosensors.


Assuntos
Aptâmeros de Nucleotídeos/química , Técnicas Biossensoriais/métodos , DNA Catalítico/química , Benzotiazóis/química , Biocatálise , Cocaína/análise , Cocaína/química , Colorimetria/métodos , DNA Catalítico/genética , Estradiol/análise , Estradiol/química , Corantes Fluorescentes/química , Quadruplex G , Limite de Detecção , Mercúrio/análise , Mercúrio/química , Conformação de Ácido Nucleico , Peroxidase/química , Espectrometria de Fluorescência/métodos , Sulfadimetoxina/análise , Sulfadimetoxina/química , Trombina/análise , Trombina/química
19.
Mar Pollut Bull ; 149: 110545, 2019 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-31543485

RESUMO

Illicit drugs and their metabolites represent a new class of emerging contaminants. These substances are continuously discharged into wastewater which have been detected in the aquatic environment in concentrations ranging from ng.L-1 to µg.L-1. Our study detected the occurrence of cocaine (COC) and benzoylecgonine (BE) in a subtropical coastal zone (Santos Bay, SP, Brazil) within one year. Water samples (surface and bottom) were collected from the Santos Submarine Sewage Outfall (SSOS) area. COC and BE were measured in the samples using ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-ESI-MS/MS). Concentrations ranged from 12.18 to 203.6 ng.L-1 (COC) and 8.20 to 38.59 ng.L-1 (BE). Higher concentrations of COC were observed during the end of spring, following the population increase at summer season. COC and its metabolite occurrence in this coastal zone represent a threat to coastal organisms.


Assuntos
Cocaína/análogos & derivados , Cocaína/análise , Poluentes Químicos da Água/análise , Baías , Brasil , Cromatografia Líquida , Monitoramento Ambiental/métodos , Drogas Ilícitas/análise , Estações do Ano , Esgotos , Espectrometria de Massas por Ionização por Electrospray , Espectrometria de Massas em Tandem , Águas Residuárias
20.
Forensic Sci Int ; 302: 109894, 2019 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-31408788

RESUMO

INTRODUCTION: Currently, hair straightening has become a regular hair treatment for women but likewise for men. Several studies have shown that thermal straightening has an influence on the concentration of ethyl glucuronide and of drugs of abuse content in hair. Heat treatment of hair may decrease concentrations of cocaine (COC) and of cocaethylene (CE) in hair and increase concentrations of benzoylecgonine (BZE). The goal of this study was to evaluate the influence of thermal straightening on anhydroecgonine methyl ester (AEME), a known cocaine smoking marker, in hair. METHOD: 42 positive COC hair samples were treated in vitro with iron plates heated to 200°C. During this treatment one lock of hair was put sequentially 30 times in contact with a hair straightener during 2s, the other lock was not treated. The hair samples were analyzed by a validated GC/MS method for AEME, COC and its metabolites BZE, norcocaine (NC), ecgonine methyl ester (EME) and CE. RESULTS: After treatment, a median increase of concentrations was observed for AEME (110.3%) and BZE (27.6%) whereas a median decrease was found for COC (56.9%), NC (46.7%), EME (33.3%) and CE (41.7%). The median BZE/COC ratio of 0.6 in not treated hair increased to 1.5 in treated hair. CONCLUSION: Regarding our in vitro results, AEME may be produced by thermal hair straightening. Therefore, the presence of AEME in hair should not be used as an irrefutable prove of cocaine smoking. Our study shows that for the interpretation of AEME results in hair, potential heat treatment of hair should be considered. A ratio BZE/COC higher 1 appears to be a good marker to identify thermal treatment of hair before collection. Finally, thermal straightening should be documented during hair collection and should also be considered for the interpretation of COC results in hair.


Assuntos
Cocaína/análogos & derivados , Cocaína/análise , Preparações para Cabelo , Cabelo/química , Entorpecentes/análise , Biomarcadores/análise , Transtornos Relacionados ao Uso de Cocaína/diagnóstico , Toxicologia Forense , Cromatografia Gasosa-Espectrometria de Massas , Humanos , Técnicas In Vitro , Detecção do Abuso de Substâncias
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