Your browser doesn't support javascript.
loading
Mostrar: 20 | 50 | 100
Resultados 1 - 20 de 92
Filtrar
1.
Sci Rep ; 10(1): 1974, 2020 02 06.
Artigo em Inglês | MEDLINE | ID: mdl-32029797

RESUMO

The finding that drugs and metabolites can be detected from fingerprints is of potential relevance to forensic science and as well as toxicology and clinical testing. However, discriminating between dermal contact and ingestion of drugs has never been verified experimentally. The inability to interpret the result of finding a drug or metabolite in a fingerprint has prevented widespread adoption of fingerprints in drug testing and limits the probative value of detecting drugs in fingermarks. A commonly held belief is that the detection of metabolites of drugs of abuse in fingerprints can be used to confirm a drug has been ingested. However, we show here that cocaine and its primary metabolite, benzoylecgonine, can be detected in fingerprints of non-drug users after contact with cocaine. Additionally, cocaine was found to persist above environmental levels for up to 48 hours after contact. Therefore the detection of cocaine and benzoylecgonine (BZE) in fingermarks can be forensically significant, but do not demonstrate that a person has ingested the substance. In contrast, the data here shows that a drug test from a fingerprint (where hands can be washed prior to donating a sample) CAN distinguish between contact and ingestion of cocaine. If hands were washed prior to giving a fingerprint, BZE was detected only after the administration of cocaine. Therefore BZE can be used to distinguish cocaine contact from cocaine ingestion, provided donors wash their hands prior to sampling. A test based on the detection of BZE in at least one of two donated fingerprint samples has accuracy 95%, sensitivity 90% and specificity of 100% (n = 86).


Assuntos
Cocaína/análogos & derivados , Cocaína/metabolismo , Toxicologia Forense/métodos , Pele/química , Detecção do Abuso de Substâncias/métodos , Cocaína/isolamento & purificação , Transtornos Relacionados ao Uso de Cocaína/diagnóstico , Dermatoglifia , Desinfecção das Mãos , Humanos , Irlanda , Espectrometria de Massas , Sensibilidade e Especificidade , Pele/metabolismo , Fatores de Tempo
2.
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
3.
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 de 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
4.
Drug Test Anal ; 11(10): 1542-1555, 2019 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-31407511

RESUMO

The effectiveness of decontamination procedures used for the removal of external drug contamination in forensic hair analysis is an ongoing debate. This investigation evaluated wash methods complying with Society of Hair Testing (SoHT) guidelines and their capacity to remove cocaine (COC) and methamphetamine (MA) from artificially contaminated hair. The most effective decontamination method was determined using a systematic approach, involving (1) an initial washing solvent screen, (2) optimization of wash duration, (3) comparison of sequential wash methods, and (4) reanalysis of clinical hair samples. For analysis, hair was subjected to micro-pulverized methanolic extraction prior to quantitation by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Methanol (MeOH) and 0.1 M phosphate buffer (pH 6) were the most effective organic and aqueous solvents, respectively, removing 28%-38% of COC and 16%-31% of MA. Wash durations longer than 30-60 minutes did not remove additional amounts, and a more efficient sequential wash method was subsequently developed. Despite this, the interpretation of reportable results relative to the SoHT cut-off levels was unchanged for most clinical hair samples reanalyzed after washing by agitation for 30 minutes with MeOH. These findings highlight the inability of decontamination solvents to completely remove external COC and MA contamination from hair, including wash methods adhering to SoHT guidelines.


Assuntos
Anestésicos Locais/isolamento & purificação , Estimulantes do Sistema Nervoso Central/isolamento & purificação , Cocaína/isolamento & purificação , Cabelo/química , Metanfetamina/isolamento & purificação , Anestésicos Locais/análise , Estimulantes do Sistema Nervoso Central/análise , Cromatografia Líquida de Alta Pressão/métodos , Cocaína/análise , Descontaminação/métodos , Toxicologia Forense/métodos , Humanos , Metanfetamina/análise , Solventes/química , Detecção do Abuso de Substâncias/métodos , Espectrometria de Massas em Tandem/métodos
5.
J Chromatogr A ; 1603: 23-32, 2019 Oct 11.
Artigo em Inglês | MEDLINE | ID: mdl-31230878

RESUMO

The analyses of drugs and metabolites in complex matrices have been widely studied in recent years. However, due to high levels endogenous compounds and matrix complexity, these analyses require a sample pre-treatment step. To this aim, two lab-made extractive phases were integrated to probe electrospray ionization mass spectrometry (PESI-MS) technique for direct analysis of illicit drugs in biological fluids and phorbol esters in Jatropha curcas extract. The polypyrrole (PPy) phase was electropolymerized onto a platinum wire surface by cyclic voltammetry. The molecularly imprinted polymer (MIP) was synthesized and adhered onto a stainless-steel needle with epoxy resin. The PPy-PESI-MS method showed to be linear in a concentration range from 1 to 500 µg L-1, with accuracy values between -2.1 and 14%, and precision values between 0.8 and 10.8%. The MIP-PESI-MS method showed to be linear in a concentration range from 0.9 to 30 mg L-1, with accuracy values between -1.6 and -15.3%, and precision values between 4.1 and 13.5%.


Assuntos
Impressão Molecular/métodos , Preparações Farmacêuticas/análise , Preparações Farmacêuticas/isolamento & purificação , Polímeros/química , Pirróis/química , Microextração em Fase Sólida/métodos , Espectrometria de Massas por Ionização por Electrospray/métodos , Cocaína/análise , Cocaína/isolamento & purificação , Voluntários Saudáveis , Humanos , Jatropha/química , Dietilamida do Ácido Lisérgico/análise , Dietilamida do Ácido Lisérgico/isolamento & purificação , Metanfetamina/análise , Metanfetamina/isolamento & purificação , N-Metil-3,4-Metilenodioxianfetamina/análise , N-Metil-3,4-Metilenodioxianfetamina/isolamento & purificação , Ésteres de Forbol/análise , Ésteres de Forbol/isolamento & purificação , Extratos Vegetais/análise , Extratos Vegetais/isolamento & purificação , Saliva/metabolismo , Aço Inoxidável/química , Urinálise
6.
Chemosphere ; 222: 83-90, 2019 May.
Artigo em Inglês | MEDLINE | ID: mdl-30690404

RESUMO

The present study focused on 11-nor-9carboxy-Δ9-THC (THC-COOH) and Benzoylecgonine (BE), the most common metabolites of cannabis and cocaine, respectively, present in the domestic sewage entering the wastewater treatment plants. The aims of the study were: (1) to validate the analytical method of detection in wastewater and sludge; (2) to determine contribution of biodegradation and other processes to the removal in the biological reactor of the wastewater treatment plant (WWTP) and the response of biomass to different drug concentrations. The Ultra-Performance Liquid Chromatography coupled to tandem Mass Spectrometry method showed to be repeatable and reliable (recovery>75%; repeatability<10-15%; bias uncertainty<10) for measurements in wastewater; the ultrasound assisted extraction (USE) demonstrated to be reliable as pre-treatment of activated sludge solid phase. Both drugs were fully removed from the liquid phase in the lab-scale biological reactor within 24 h. Biodegradation was the main BE removal mechanism, and the first order kinetic model provided the best fitting of the experimental data. THC-COOH was mainly removed due to a combination of adsorption and biodegradation; adsorption was better described by the pseudo-second order kinetic model and the Freundlich isotherm. Both drugs at the higher concentrations caused inhibition of nitrogen oxidation and carbon removal.


Assuntos
Biodegradação Ambiental , Cocaína/análogos & derivados , Dronabinol/análogos & derivados , Esgotos/química , Adsorção , Cannabis/química , Cromatografia Líquida , Cocaína/análise , Cocaína/isolamento & purificação , Dronabinol/análise , Dronabinol/isolamento & purificação , Espectrometria de Massas em Tandem , Águas Residuárias/química , Poluentes Químicos da Água/análise
7.
Methods Mol Biol ; 1872: 199-209, 2019.
Artigo em Inglês | MEDLINE | ID: mdl-30350292

RESUMO

Meconium, the first stool of a newborn, can be analyzed to identify prenatal exposure to drugs of abuse. Meconium accumulates in a fetus during the second and third trimesters of pregnancy providing a wide window of exposure. Identification of in utero drug exposure is essential for the diagnosis and treatment of infants for dependency/withdrawal caused from the exposure. However, testing of meconium samples is often cumbersome and time-consuming. Unlike liquid samples, meconium is a viscous, semisolid, tar-like substance that needs to be individually weighed prior to extraction. Additionally, the meconium matrix is not homogeneous and not easily mixed or extracted. A method for analyzing cocaine and metabolites as well as amphetamines in meconium utilizing ceramic homogenizers prior to salt-assisted liquid-liquid extraction and liquid chromatography tandem-mass spectrometry (LC-MS/MS) is presented.


Assuntos
Anfetaminas/farmacocinética , Cromatografia Líquida , Cocaína/farmacocinética , Extração Líquido-Líquido/métodos , Mecônio/química , Detecção do Abuso de Substâncias/métodos , Espectrometria de Massas em Tandem , Anfetaminas/isolamento & purificação , Cocaína/isolamento & purificação , Humanos , Sais
8.
Talanta ; 181: 232-238, 2018 May 01.
Artigo em Inglês | MEDLINE | ID: mdl-29426506

RESUMO

A molecularly imprinted polymer - Mn-doped ZnS quantum dot-based fluorescence probe for cocaine abuse screening has been prepared and applied to complex samples such as serum and oral fluid. The fluorescent sensing material was prepared by anchoring a selective MIP for COC on the surface of polyethylene glycol (PEG) modified Mn-doped ZnS quantum dots (QDs). Simple and low cost methods have thus been optimized for assessing cocaine abuse in serum and oral fluid by monitoring fluorescence quenching when cocaine (COC) is present (optimized operating conditions with 1.5mL of 200mgL-1 MIP-coated QDs solution, pH 5.5, and 15min before fluorescence scanning). The matrix effect was found to be important when analyzing oral fluid and serum, and several strategies based on centrifugation for oral fluid and solid phase extraction (SPE) for serum were explored. Two analytical methods were developed for oral fluid. The first one (direct method) requires a centrifugation step (6°C, 4000rpm, 20min) to avoid the matrix effect, and allows for cocaine determination by using an aqueous calibration (1:20 dilution). The second method was developed for oral fluid sampled by Salivette devices, and also requires a further centrifugation (6°C, 4000rpm, 20min) of the recovered oral fluid. This method, however, requires the standard addition technique (1:20 dilution) because of the existence of the matrix effect. Regarding serum samples, a direct method (serum dilution) was not possible, and an SPE procedure was needed to avoid the matrix effect (use of aqueous calibration). The limits of detection and quantification when using the Salivette method were 0.035mgL-1and 0.117mgL-1, respectively; whereas, 0.015mgL-1 (LOD) and 0.050mgL-1 (LOQ) were obtained for serum.


Assuntos
Cocaína/análise , Impressão Molecular , Polímeros/química , Pontos Quânticos/química , Saliva/química , Espectrometria de Fluorescência/métodos , Cocaína/sangue , Cocaína/isolamento & purificação , Transtornos Relacionados ao Uso de Cocaína/sangue , Transtornos Relacionados ao Uso de Cocaína/diagnóstico , Manganês/química , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Sulfetos/química , Compostos de Zinco/química
9.
Drug Test Anal ; 10(4): 761-767, 2018 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-28815945

RESUMO

Cocaine trafficking in the form of textile impregnation is routinely encountered as a concealment method. Raman spectroscopy has been a popular and successful testing method used for in situ screening of cocaine in textiles and other matrices. Quantitative analysis of cocaine in these matrices using Raman spectroscopy has not been reported to date. This study aimed to develop a simple Raman method for quantifying cocaine using atropine as the model analogue in various types of textiles. Textiles were impregnated with solutions of atropine in methanol. The impregnated atropine was extracted using less hazardous acidified water with the addition of potassium thiocyanate (KSCN) as an internal standard for Raman analysis. Despite the presence of background matrix signals arising from the textiles, the cocaine analogue could easily be identified by its characteristic Raman bands. The successful use of KSCN normalised the analyte signal response due to different textile matrix background interferences and thus removed the need for a matrix-matched calibration. The method was linear over a concentration range of 6.25-37.5 mg/cm2 with a coefficient of determination (R2 ) at 0.975 and acceptable precision and accuracy. A simple and accurate Raman spectroscopy method for the analysis and quantification of a cocaine analogue impregnated in textiles has been developed and validated for the first time. This proof-of-concept study has demonstrated that atropine can act as an ideal model compound to study the problem of cocaine impregnation in textile. The method has the potential to be further developed and implemented in real world forensic cases.


Assuntos
Atropina/análise , Cocaína/análise , Drogas Ilícitas/análise , Análise Espectral Raman/métodos , Têxteis/análise , Atropina/isolamento & purificação , Vestuário , Cocaína/análogos & derivados , Cocaína/isolamento & purificação , Humanos , Drogas Ilícitas/isolamento & purificação , Limite de Detecção , Tiocianatos/química
10.
Bioanalysis ; 9(21): 1655-1666, 2017 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-29095043

RESUMO

AIM: The increasing use of cocaine (COC) during breastfeeding has led to growing concern about exposure of infants. Therefore, to study this exposure, a new method to analyze COC and benzoylecgonine in breast milk was developed. METHODOLOGY: A new extraction method was used for the first time to analyze COC and its major metabolite, benzoylecgonine, in breast milk using magnetic carbon nanotubes partially doped with nitrogen. RESULTS: The calibration curves were linear in the range 5.0-180.0 ng ml-1. The limit of quantification was 5.0 ng ml-1. Coefficients of variation were between 3.2 and 13.9%. Recovery was between 89.6 and 99.2%. CONCLUSION: The proposed method is simple, efficient and suitable to determine analytes in breast milk.


Assuntos
Cocaína/análogos & derivados , Cocaína/análise , Cromatografia Gasosa-Espectrometria de Massas , Leite Humano/química , Adulto , Calibragem , Cocaína/isolamento & purificação , Cocaína/normas , Feminino , Cromatografia Gasosa-Espectrometria de Massas/normas , Humanos , Limite de Detecção , Leite Humano/metabolismo , Nanotubos de Carbono/química , Extração em Fase Sólida
11.
Talanta ; 164: 693-699, 2017 Mar 01.
Artigo em Inglês | MEDLINE | ID: mdl-28107992

RESUMO

A novel and rapid method to detect cocaine in human urine has been developed by using self-assembly ordered two dimensional (2D) gold nanoparticles (GNPs) film as surface-enhanced Raman spectroscopy (SERS) substrates. In order to obtain high sensitivity, uniformity, and reproducibility of SERS platform, quasi-spherical, uniform GNPs were firstly synthesis using seed growth method, in which the GNPs have been functionalized with CTAB to form orderly close-packed GNPs film as SERS substrate. Importantly, the high-performance GNPs on solid substrates can produce a high yield of sub-10-nm gaps which can generate gigantic signals enhancement for analytes adsorbed GNPs surface. In view of the complex component of human urine, we develop a rapid and efficient pretreatment strategy for separation and purification of cocaine by using hexane extraction in real human urine samples within 3min. With the advantages of better extraction rates (>75%) examined by ultraperformance liquid chromatography (UPLC) and the excellent signal-to-noise ratio detected by SERS, our pretreatment procedure can efficiently lower the interference of complex biological components in urine. To reach on-spot analyzer, a handheld Raman spectrometer was used for feasible SERS detection of cocaine in real human urine. The favorable results demonstrated our pretreatment strategy combined with SERS platform will be a great prospective method toward rapid, reliable, and on-spot cocaine detection for public safety.


Assuntos
Cocaína/urina , Ouro/química , Nanopartículas Metálicas/química , Análise Espectral Raman/métodos , Urinálise/métodos , Cocaína/química , Cocaína/isolamento & purificação , Hexanos/química , Humanos
12.
Electrophoresis ; 38(8): 1217-1223, 2017 04.
Artigo em Inglês | MEDLINE | ID: mdl-28130907

RESUMO

A new CE method was here developed, in order to study the stability of cocaine and some of its metabolites in water and in oral fluid. At first, standard mixtures of cocaine (COC), benzoylecgonine (BE) and cocaethylene (COET) in water were used to study the optimal CE parameters to separate the three compounds. Voltage, sample temperature and pH were investigated, and 25 kV, 25°C and a pH of 4.7 were selected to achieve the best separation. The stability of the three compounds in water and oral fluid was then monitored by applying the previously developed method. Three different storage temperatures (8, 25 and 37°C) were selected and analyses during a week were performed. A decrease of COC and COET peak areas and an increase of BE peak area were observed over time at 25 and 37°C. In addition, in oral fluid, the presence of enzymes and other proteins, and the differences in the molecular structures between COC and COET, caused a stronger degradation of the first compound. Instead, when samples were stored at a low temperature (8°C), the peak areas of the compounds did not vary. Thus, the use of this storage temperature is recommended, above all when sample must be analyzed after a relatively long time.


Assuntos
Cocaína/metabolismo , Eletroforese Capilar/métodos , Líquidos Corporais , Cocaína/análogos & derivados , Cocaína/isolamento & purificação , Estabilidade de Medicamentos , Concentração de Íons de Hidrogênio , Saliva , Temperatura , Água
13.
Forensic Sci Int ; 270: 267-274, 2017 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-27836413

RESUMO

The Scott test, widely used as the field test for cocaine, is performed in three steps. If a sample contains cocaine, blue precipitates appear in step 1, the precipitates are dissolved and the solution turns pink in step 2, and the lower layer turns blue in step 3. However, some pyrrolidine-type cathinones produce cocaine-like results when tested, necessitating modification of the test procedure. Filtration of the second-step mixture weakened the blue color in step 3; however, the blue color did not completely disappear. Adding the Chen-Kao reagent to the test procedure enhanced the differentiation: when the reagent was added to cocaine, the solution was initially turbid, but then became clear over time; its addition to cathinones resulted in turquoise or light sky-blue precipitation. These results indicated that the Chen-Kao test was useful for exclusion of cathinones. A combination of the modified Scott test and the Chen-Kao test was successfully applied to the forensic samples containing cocaine or pyrrolidine-type cathinones. In conclusion, a combination of these tests will be the useful field-test procedure for cocaine.


Assuntos
Transtornos Relacionados ao Uso de Cocaína/diagnóstico , Cocaína/isolamento & purificação , Entorpecentes/isolamento & purificação , Detecção do Abuso de Substâncias/métodos , Humanos , Indicadores e Reagentes
14.
Toxicology ; 376: 102-112, 2017 Feb 01.
Artigo em Inglês | MEDLINE | ID: mdl-27142991

RESUMO

A simple method has been proposed for the determination of cocaine's major adulterants (caffeine, levamisole, lidocaine, phenacetin, diltiazem, and hydroxyzine) in human urine by dispersive liquid-liquid microextraction based on solidification of floating organic drop (DLLME-SFO) in combination with high-performance liquid chromatography - photodiode array detector (HPLC-PDA). The reversed-phase chromatographic separation was obtained with a column C18 extended (250×4.6mm; 5µm; 80Å) in gradient elution mode using acetonitrile-trifluoroacetic acid 0.026% (v,v) (pH=2.5) at 1mLmin-1 as mobile phase, at 25°C, and detection at 235nm. The analysis time was 25min. This condition had the best resolution factors (>1.15), retention factors (>0.68), number of plates (>2094.9), and separation factors (>1.05) for all targets, indicating a good separation. The kind of extraction and dispersive solvent were investigated for unifactorial design. The buffer pH, the volume of extraction and disperser solvent, and the amount of salt were optimized for full factorial design. Under optimum conditions, human urine samples were alkalized with 0.5M sodium phosphate buffer (pH 10) and added to sodium chloride (20%m/v). Acetonitrile (150µL) and 1-dodecanol (30µL) were used as dispersive and extraction solvent, respectively. The method presented linear range of 312.5-3125ngmL-1 to caffeine and levamisole and 187.5-1875ngmL-1 to lidocaine, phenacetin, diltiazem, and hydroxyzine. The limit of quantification was 187.5ngmL-1 to lidocaine, phenacetin, diltiazem, and hydroxyzine and 312.5ngmL-1 for caffeine and levamisole. The recovery mean values were between 6.0 and 42.6%. The method showed good precision and accuracy, with within- and between-run relative standard deviation and relative error less than 15%. The samples were stable after freeze-thaw cycle and short-term room temperature stability tests. Besides, this method was satisfactorily applied in urine of cocaine users. It is expected that this method, which was the first to combine the use of DLLME-SFO and HPLC-PDA for the determination of cocaine's major adulterants in human urine, will contribute to the accuracy in the diagnosis of acute intoxication, the proper planning of therapeutic measures, as well as to the favorable prognostic of cocaine intoxicated patients.


Assuntos
Cocaína/isolamento & purificação , Cocaína/urina , Contaminação de Medicamentos , Microextração em Fase Líquida/métodos , Adulto , Cromatografia Líquida de Alta Pressão/métodos , Feminino , Humanos , Masculino , Pessoa de Meia-Idade , Adulto Jovem
15.
J Hazard Mater ; 318: 515-525, 2016 Nov 15.
Artigo em Inglês | MEDLINE | ID: mdl-27450344

RESUMO

Benzoylecgonine (BE), the main cocaine metabolite, has been detected in numerous surface water and treatment plants effluents in Europe and there is urgent need for effective treatment methods. In this study, the removal of BE by the UV254/H2O2 process from different water matrices was investigated. By means of competition kinetics method, the kinetic constant of reaction between BE and the photogenerated hydroxyl radicals (OH) was estimated resulting in kOH/BE=5.13×10(9)M(-1)s(-1). By-products and water matrices scavengers effects were estimated by numerical modeling of the reaction kinetics for the UV254/H2O2 process and validated in an innovative microcapillary film (MCF) array photoreactor and in a conventional batch photoreactor. The ecotoxicity of the water before and after treatment was evaluated with four organisms Raphidocelis subcapitata, Daphnia magna, Caenorhabditis elegans, and Vicia faba. The results provided evidence that BE and its transformation by-products do not have significant adverse effects on R. subcapitata, while D. magna underwent an increase of lipid droplets. C. elegans was the most sensitive to BE and its by-products. Furthermore, a genotoxicity assay, using V. faba, showed cytogenic damages during the cell mitosis of primary roots.


Assuntos
Cocaína/análogos & derivados , Peróxido de Hidrogênio/química , Mutagênicos/toxicidade , Poluentes Químicos da Água/isolamento & purificação , Poluentes Químicos da Água/toxicidade , Água/química , Animais , Organismos Aquáticos , Cocaína/isolamento & purificação , Cocaína/toxicidade , Ecotoxicologia , Cinética , Plantas , Raios Ultravioleta
16.
Artigo em Inglês | MEDLINE | ID: mdl-26977890

RESUMO

A fluorescence immunoassay (FIA) has been developed for the detection of cocaine using norcocaine labeled with merocyanine dye and a monoclonal antibody specific to cocaine. Using this FIA, the detection range for cocaine was between 20.0 and 1700 µg/L with a limit of detection of 20.0 µg/L. Other cocaine derivatives did not interfere significantly with the detection when using this immunoassay technique with cross-reactivity values of less than 20%. Thus this FIA could be considered a useful tool for the detection of cocaine.


Assuntos
Anticorpos Monoclonais/imunologia , Cocaína/análogos & derivados , Cocaína/isolamento & purificação , Imunoensaio , Benzopiranos/química , Benzopiranos/imunologia , Cocaína/imunologia , Fluorescência , Humanos , Indóis/química , Indóis/imunologia , Limite de Detecção
17.
Sci Rep ; 6: 21024, 2016 Feb 15.
Artigo em Inglês | MEDLINE | ID: mdl-26876971

RESUMO

Illicit drug use has a global concern and effective monitoring and interventions are highly required to combat drug abuse. Wastewater-based epidemiology (WBE) is an innovative and cost-effective approach to evaluate community-wide drug use trends, compared to traditional population surveys. Here we report for the first time, a novel quantitative community sewage sensor (namely DNA-directed immobilization of aptamer sensors, DDIAS) for rapid and cost-effective estimation of cocaine use trends via WBE. Thiolated single-stranded DNA (ssDNA) probe was hybridized with aptamer ssDNA in solution, followed by co-immobilization with 6-mercapto-hexane onto the gold electrodes to control the surface density to effectively bind with cocaine. DDIAS was optimized to detect cocaine at as low as 10 nM with a dynamic range from 10 nM to 5 µM, which were further employed for the quantification of cocaine in wastewater samples collected from a wastewater treatment plant in seven consecutive days. The concentration pattern of the sampling week is comparable with that from mass spectrometry. Our results demonstrate that the developed DDIAS can be used as community sewage sensors for rapid and cost-effective evaluation of drug use trends, and potentially implemented as a powerful tool for on-site and real-time monitoring of wastewater by un-skilled personnel.


Assuntos
Aptâmeros de Nucleotídeos/química , Técnicas Biossensoriais/métodos , Cocaína/isolamento & purificação , Ácidos Nucleicos Imobilizados/química , Aptâmeros de Nucleotídeos/genética , DNA de Cadeia Simples/química , Monitoramento Ambiental , Humanos , Esgotos/química , Transtornos Relacionados ao Uso de Substâncias/epidemiologia , Águas Residuárias/química
18.
Anal Bioanal Chem ; 408(5): 1467-74, 2016 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-26753977

RESUMO

Modern LC-MS/MS instruments have sensitivity and scanning velocity high enough to analyze many different compounds in single runs. Consequently, the sample preparation procedure has become the bottleneck for developing efficient, rapid, and cheap multi-compound methods. Here, we examined one-step sample preparation based on quick, easy, cheap, effective, rugged, and safe (QuEChERS) salts to set up and validate a LC-MS/MS method for the simultaneous determination of 35 drugs of abuse and their metabolites in whole blood. Despite large differences in physicochemical properties, this simplified QuEChERS extraction method yielded satisfactory recoveries (until 96%) for the 35 molecules. The amounts of QuEChERS salts had no influence on extraction yield. Chromatographic separation was obtained in less than 6 min. LLOD and LLOQ were 3 and 5 ng/mL, respectively. The procedure was successfully validated and then applied to 253 cases of driving under the influence of drugs (DUID), collected over a 6-month period.


Assuntos
Anfetaminas/análise , Analgésicos Opioides/análise , Análise Química do Sangue/métodos , Cromatografia Líquida/métodos , Cocaína/análise , Espectrometria de Massas em Tandem/métodos , Anfetaminas/isolamento & purificação , Anfetaminas/metabolismo , Analgésicos Opioides/isolamento & purificação , Analgésicos Opioides/metabolismo , Cocaína/isolamento & purificação , Cocaína/metabolismo , Humanos , Extração em Fase Sólida/métodos , Detecção do Abuso de Substâncias/métodos
19.
Biosens Bioelectron ; 75: 8-14, 2016 Jan 15.
Artigo em Inglês | MEDLINE | ID: mdl-26278045

RESUMO

Mesoporous silica nanoparticles (MSN) based controlled release system had been coupled with diverse detection technologies to establish biosensors for different targets. Chemiluminescence (CL) system of luminol/H2O2 owns the characters of simplicity, low cost and high sensitivity, but the targets of which are mostly focused on some oxidants or which can participate in a chemical reaction that yields a product with a role in the CL reaction. In this study, chemiluminescent detection technique had been coupled with mesoporous silica-based controlled released system for the first time to develop a sensitive biosensor for the target which does not cause effect to the CL system itself. Cocaine had been chosen a model target, the MSN support was firstly loaded with glucose, then the positively charged MSN interacted with negatively charged oligonucleotides (the aptamer cocaine) to close the mesopores of MSN. At the present of target, cocaine binds with its aptamer with high affinity; the flexible linear aptamer structured will become stems structured through currently well-defined non-Waston-Crick interactions and causes the releasing of entrapped glucose into the solution. With the assistant of glucose oxidase (GOx), the released glucose can react with the dissolved oxgen to produce gluconic acid and H2O2, the latter can enhance the CL of luminol in the NaOH solution. The enhanced CL intensity has a relationship with the cocaine concentration in the range of 5.0-60µM with the detection limit of 1.43µM. The proposed method had been successfully applied to detect cocaine in serum samples with high selectivity. The same strategy can be applied to develop biosensors for different targets.


Assuntos
Técnicas Biossensoriais , Cocaína/isolamento & purificação , Nanopartículas/química , Dióxido de Silício/química , Cocaína/química , Enzimas Imobilizadas/química , Glucose , Glucose Oxidase/química , Ouro/química , Humanos , Peróxido de Hidrogênio/química , Limite de Detecção , Luminescência , Luminol/química
20.
Biosens Bioelectron ; 75: 213-21, 2016 Jan 15.
Artigo em Inglês | MEDLINE | ID: mdl-26319164

RESUMO

Mn-doped ZnS quantum dots (QDs) coated with a molecularly imprinted polymer (MIP) material selective toward cocaine and its metabolites have been prepared and applied to cocaine (COC) and metabolites assessment by spectrofluorimetry. Ultrasound irradiation (37kHz) was novelty used for performing the Mn-doped ZnS QDs synthesis as well as for preparing the QD based MIP-coated composite by precipitation polymerization (imprinting process). This fact allowed the synthesis to be accomplished in four hours. In addition, the use of ultrasound irradiation during MIP-QDs synthesis increased the homogeneity of the QDs size, and reduced nanoparticles agglomeration. MIP was synthesized using COC as a template molecule, ethylene dimethacrylate (EDMA) as a functional monomer, divinylbenzene (DVB) as a cross-linker, and 2,2'-azobisisobutyronitrile (AIBN) as an initiator. The fluorescence of MIP-coated QDs was quenched by the template (COC) and also by metabolites from COC such as benzoylecgonine (BZE), and ecgonine methyl ester (EME). Quenching was not observed when performing experiments with non-imprinted polymer (NIP)-coated QDs; and also, fluorescence quenching of MIP-coated QDs was not observed by other drugs of abuse and metabolites (heroin and cannabis abuse). This fact indicates that the prepared material recognize only COC (template) and metabolites.


Assuntos
Técnicas Biossensoriais , Cocaína/isolamento & purificação , Impressão Molecular , Espectrometria de Fluorescência , Humanos , Manganês/química , Polímeros/química , Pontos Quânticos/química , Sulfetos/química , Telúrio/química , Compostos de Zinco/química
SELEÇÃO DE REFERÊNCIAS
DETALHE DA PESQUISA
...