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1.
Biosens Bioelectron ; 147: 111790, 2020 Jan 01.
Artigo em Inglês | MEDLINE | ID: mdl-31669805

RESUMO

In this study, modified hollow titanium dioxide and SnS2 quantum dots (SnS2 QDs) were used to build a novel electrochemiluminescence immunoassay (ECLIA) for ultrasensitive detection of chloramphenicol (CAP). The titanium dioxide hollow spheres (THS) modified with polyethyleneimine (PEI) and gold nanoparticles (Au NPs) was synthesized as a probe material for the novel ECLIA, meanwhile it also could be a coreaction accelerator which could greatly improve the interaction efficiency between SnS2 QDs and S2O82-. Then the modified THS was combined with chloramphenicol antibody to form ECLIA probes, and colloidal gold synthesized as a platform for an ECLIA by ascorbic acid (AA) reduction. A competitive immunoassay strategy was used for the detection of CAP, where CAP in the sample would compete with the coating antigen for the limited antibodies. The proposed ECLIA for CAP detection exhibited high sensitivity with a wide linear range from 0.01 ng mL-1 to 100 ng mL-1 and a low detection limit at 3.1 pg mL-1. Furthermore, it could be seen from electrochemical analysis that the effect of THS on the enhancement of ECL signal is about twice as high as that of ordinary titanium dioxide. Importantly, this work not only successfully applied THS to amplify electrochemical-luminescence signal in the ECLIA, but also successfully prepared a stable and highly selective sensor for ultrasensitive detection of CAP.


Assuntos
Técnicas Biossensoriais , Cloranfenicol/isolamento & purificação , Técnicas Eletroquímicas , Nanopartículas Metálicas/química , Cloranfenicol/química , Dissulfetos/química , Medições Luminescentes , Pontos Quânticos/química , Estanho/química , Titânio/química
2.
Biosens Bioelectron ; 149: 111801, 2020 Feb 01.
Artigo em Inglês | MEDLINE | ID: mdl-31726276

RESUMO

An ultrasensitive and rapid detection of trace antibiotics is imperative for food safety and public health. Herein, we present a ratiometric fluorescent sensing strategy based on an aptamer labeled with a fluorescent dye and a highly stable zirconium-porphyrin MOF (PCN-222) as a fluorescence quencher for the high-efficiency detection of chloramphenicol (CAP). PCN-222 exhibits a strong adsorption ability toward the dye-labeled aptamer through π-π stacking, electrostatic, hydrogen bond, and coordination interactions. Experimental and simulation studies confirm that PCN-222 demonstrates a high quenching efficiency via fluorescence resonance energy transfer (FRET) and photoinduced electron transfer (PET) processes. In the presence of CAP, dye-labeled aptamers are released from the PCN-222 surface, resulting in the recovery of fluorescence. This proposed biosensor allows the complete detection of CAP within 26 min. For ratiometric measurement, its detection limit is as low as 0.08 pg mL-1 with a wide detection range from 0.1 pg mL-1 to 10 ng mL-1. It is successfully applied to analyze CAP in milk and shrimp samples, and its results are consistent with those of the commercial ELISA kit. This biosensor not only enables the rapid, ultrasensitive, and highly specific detection of CAP but also reveals excellent universality and multiplexed analysis performance.


Assuntos
Técnicas Biossensoriais , Cloranfenicol/isolamento & purificação , Leite/química , Animais , Cloranfenicol/química , Ensaio de Imunoadsorção Enzimática , Transferência Ressonante de Energia de Fluorescência , Corantes Fluorescentes/química , Humanos , Limite de Detecção , Porfirinas/química , Zircônio/química
3.
J Food Sci ; 84(12): 3624-3633, 2019 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-31762030

RESUMO

An aptamer-functionalized Fe3 O4 /graphene oxide was synthesized by chemical co-precipitation method and then employed in the magnetic solid-phase extraction for selective enrichment of chloramphenicol before HPLC. The aptamer was covalently bonded to the Fe3 O4 /graphene oxide complex by 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride and N-hydroxysuccinimide. Parameters affecting extraction efficiency including solution pH, extraction time and temperature, types and volume of elution solvent, and elution time were investigated in detail. Under the optimal conditions, good linearity was obtained between the peak area and analyte concentration in the range of 7.0 to 1.0 × 103  µg/L with the correlation coefficient of 0.9994. The limit of detection and quantitation were 0.24 µg/L and 0.79 µg/L, respectively. The developed method was employed to the analysis of chloramphenicol in honey and milk samples. The recoveries ranged from 80.5% to 105.0% with relative standard deviations less than 8.9%. PRACTICAL APPLICATION: An aptamer-functionalized Fe3 O4 /graphene oxide was synthesized and employed in magnetic solid phase extraction for the enrichment of chloramphenicol before HPLC. The presented assay was employed for the determination of chloramphenicol in honey and milk with satisfactory results.


Assuntos
Antibacterianos/análise , Antibacterianos/isolamento & purificação , Cloranfenicol/análise , Cloranfenicol/isolamento & purificação , Cromatografia Líquida de Alta Pressão/métodos , Mel/análise , Leite/química , Extração em Fase Sólida/métodos , Animais , Bovinos , Resíduos de Drogas/análise , Resíduos de Drogas/isolamento & purificação , Contaminação de Alimentos/análise , Grafite/química , Limite de Detecção , Fenômenos Magnéticos , Extração em Fase Sólida/instrumentação
4.
Biosens Bioelectron ; 145: 111711, 2019 Dec 01.
Artigo em Inglês | MEDLINE | ID: mdl-31563801

RESUMO

Although aptamer has been demonstrated as an important probe for antibiotic determination, the selective sensing of different antibiotics is still a challenge due to their structure similarities and wide folding degrees of aptamer. Herein, a field-effect transistor using MoS2 nanosheet as the channel and an aptamer DNA (APT) with its configuration shaped by a complementary strand DNA (CS) is employed for kanamycin (KAN) determination. This probe structure contributes to an enhanced selectivity and reliability with reduced device-to-device variations. This MoS2/APT/CS sensor shows time-dependent performance in antibiotic sensing. Prolonged detection time (20 s-300 s) leads to an enhanced sensitivity (1.85-4.43 M-1) and a lower limit of detection (1.06-0.66 nM), while a shorter detection time leads to a broader linear working range. A new sensing mechanism relying on charge release from probe is proposed, which is based on the "replacement reaction" between KAN and APT-CS. This sensor exhibits an extremely high selectivity (selectivity coefficient of 12.8) to kanamycin over other antibiotics including streptomycin, tobramycin, amoxicillin, ciprofloxacin and chloramphenicol. This work demonstrates the merits of probe engineering in label-free antibiotic detection with FET sensor, which presents significant promises in sensitive and selective chemical and biological sensing.


Assuntos
Antibacterianos/isolamento & purificação , Aptâmeros de Nucleotídeos/química , Técnicas Biossensoriais , Leite/química , Animais , Antibacterianos/química , Bovinos , Cloranfenicol/química , Cloranfenicol/isolamento & purificação , DNA Complementar/química , Dissulfetos/química , Ouro/química , Humanos , Canamicina/química , Canamicina/isolamento & purificação , Nanopartículas Metálicas/química , Molibdênio/química , Estreptomicina/química , Estreptomicina/isolamento & purificação , Tobramicina/química , Tobramicina/isolamento & purificação
5.
Chemosphere ; 226: 298-306, 2019 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-30933739

RESUMO

As a natural organic carbon skeleton, humic acid (HA) was loaded with nanoscale zero-valent iron (nZVI) Particles to remove chloramphenicol (CAP) from aqueous solution. The pore morphology and structure, the type, the distribution and valence state of element, and the class of functional groups on the surface of the material were shown by SEM/EDS, XPS, BET and FTIR. When the load ratio of nZVI on HA was 1:30, the iron content in the material was minimized, the specific gravity of the economic material-HA was increased, and the removal efficiency of CAP was 80.0% or higher. In addition, the mass ratio of nZVI on HA, the dosage of nZVI/HA-30, the initial pH and CAP concentration of the solution, these four general factors, played an important role in the efficiency and equilibrium time of the CAP removal. The removal efficiency of CAP by nZVI/HA-30 was 84.2% when the dosage was 1.0 g (100 mL)-1, the initial concentration of CAP was 30 mg L-1 and the pH was 3. The reaction pathway and removal mechanism of ZVI/HA-30 were studied by the concentration of total and ferrous iron ions in the solution, UV-Vis and MS. The CAP was continuously denitrified and dechlorinated, decomposed into easily degradable substances by nZVI particles supported on HA, which was consistent with the first-order kinetic model within 5 min. This newly synthesized material was economical and efficient, easy to store, effectively prevented agglomeration and passivation of nZVI, and had a good application prospect for removing contaminants from water.


Assuntos
Cloranfenicol/isolamento & purificação , Substâncias Húmicas , Ferro/química , Poluentes Químicos da Água/isolamento & purificação , Purificação da Água/métodos , Adsorção , Cinética , Água , Poluentes Químicos da Água/análise
6.
Biosens Bioelectron ; 131: 79-87, 2019 Apr 15.
Artigo em Inglês | MEDLINE | ID: mdl-30826654

RESUMO

A novel p-type semiconductor-based cathodic "signal-on" photoelectrochemical (PEC) aptasensor was proposed for highly sensitive and selective detection of chloramphenicol (CAP). The photocathode was fabricated with hierarchical porous flower-like Bi-BiOI@C composite synthesized via a one-pot solvothermal method using glucose as both green reductant and carbon precursor. Due to the surface plasmon resonance (SPR) effect of Bi and high-conductivity of carbon, the composite exhibited an enhanced cathodic photocurrent as compared with pure BiOI or Bi-BiOI. When CAP-binding aptamer was immobilized as recognition element on Bi-BiOI@C modified electrode, a cathodic PEC aptasensor showing specific "signal-on" response to CAP was constructed. Some influencing factors such as coating amount of Bi-BiOI@C suspension, applied bias potential, and aptamer concentration were studied. Under the optimum conditions, the cathodic photocurrent of the constructed PEC aptasensor increased linearly with CAP concentration from 2 to 250 nM, with a detection limit (3S/N) of 0.79 nΜ. The proposed sensor was successfully applied to the determination of CAP in pharmaceutical tablet, eye drop and lake water samples.


Assuntos
Aptâmeros de Nucleotídeos/química , Técnicas Biossensoriais , Cloranfenicol/isolamento & purificação , Técnicas Eletroquímicas , Carbono/química , Cloranfenicol/química , Eletrodos , Ouro/química , Grafite/química , Limite de Detecção , Porosidade , Semicondutores , Ressonância de Plasmônio de Superfície , Titânio/química
7.
Anal Bioanal Chem ; 411(10): 2131-2140, 2019 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-30719563

RESUMO

Herein, we developed a sensitive and quantitative flow assay for simultaneous detection of amantadine (AMD) and chloramphenicol (CAP) in chicken samples based on different CdSe/ZnS quantum dots (QDs). In contrast to other reports, the QDs could be excited by the same excitations that lowered the requirements for the matching instruments. Under the optimal conditions, the strategy permitted sensitive detection of AMD and CAP in a linear range of 0.23 to 1.02 ng/g and 0.02 to 0.66 ng/g. The limits of detection were 0.18 ng/g and 0.016 ng/g, respectively. Moreover, the whole detection process could be completed within 20 min with no additional sophisticated instruments and complicated operations. Spiked samples were analyzed using both QD-based lateral flow immunoassay (QD-LFIA) and commercial ELISA kits with good correlation (R2 = 0.96). Moreover, this study laid the foundation and simplified the development of the requisite instrument. Graphical abstract ᅟ.


Assuntos
Amantadina/análise , Anti-Infecciosos/análise , Cloranfenicol/análise , Análise de Alimentos/métodos , Imunoensaio/métodos , Carne/análise , Pontos Quânticos/química , Amantadina/isolamento & purificação , Animais , Anti-Infecciosos/isolamento & purificação , Compostos de Cádmio/química , Galinhas , Cloranfenicol/isolamento & purificação , Desenho de Equipamento , Análise de Alimentos/instrumentação , Imunoensaio/instrumentação , Limite de Detecção , Modelos Moleculares , Fitas Reagentes/análise , Compostos de Selênio/química , Sulfetos/química , Compostos de Zinco/química
8.
Biosens Bioelectron ; 130: 139-146, 2019 Apr 01.
Artigo em Inglês | MEDLINE | ID: mdl-30735947

RESUMO

Microchip electrophoresis (MCE) was a good available method for high-throughput and rapid detecting chemical pollutants in food samples. However, many of the reported MCE assays involve complex design of microchip, laborious operation and poor universality which limited its promotion in multiple antibiotics' detection. Herein, a multiplexed aptasensor was developed based on a universal double-T type microchip to one-step and simultaneously detect several antibiotics within 3 min using chloramphenicol (CAP) and kanamycin (Kana) as representatives. Besides, a novel stir-bar assisted DNA multi-arm junctions recycling (MAJR) strategy was designed for transducing and amplifying the signal. The brief detection mechanism was as following: the added CAP and Kana can specifically react with their aptamer probes on the stir-bar and produce different single-stranded DNA primer, respectively. Afterwards, the primers can trigger MAJR to form a lot of three- and four-arm DNA junctions corresponding to different targets. The DNA multi-arm junctions can be easily separated and detected by MCE for quantification. Moreover, the stir-bar can facilitate phase separation and obviously eliminate matrix interference in food. The assay was successfully applied in milk and fish samples, showing excellent selectivity and sensitivity with a detection limits of 0.52 pg mL-1 CAP and 0.41 pg mL-1 Kana (S/N = 3). Thus, the assay holds a great potential application for screening of antibiotics in food.


Assuntos
Antibacterianos/isolamento & purificação , Técnicas Biossensoriais , Análise de Alimentos , Contaminação de Alimentos , Animais , Antibacterianos/química , Aptâmeros de Nucleotídeos/química , Cloranfenicol/química , Cloranfenicol/isolamento & purificação , Eletroforese em Microchip , Peixes , Humanos , Canamicina/química , Canamicina/isolamento & purificação , Leite/química
9.
Molecules ; 24(3)2019 Jan 22.
Artigo em Inglês | MEDLINE | ID: mdl-30678224

RESUMO

A simple method for the determination of chloramphenicol in 22 matrices was prepared based on the QuEChERS and HPLC-MS/MS combination. Following a hydrolysis step, the homogenized samples were extracted and partitioned after adding sodium chloride with acetonitrile. Chloramphenicol was analysed by HPLC-MS/MS in negative electrospray mode by monitoring the daughter ions m/z: 321→194 and 321→152. The limit of decision (CCα) was calculated at the range of 0.10 µg kg-1 to 0.15 µg kg-1 and detection capability (CCß) from 0.12 µg kg-1 to 0.18 µg kg-1. Validation results showed that this method is suitable for the determination and confirmation of chloramphenicol in various matrices.


Assuntos
Cloranfenicol/análise , Cromatografia Líquida de Alta Pressão , Extração Líquido-Líquido , Espectrometria de Massas em Tandem , Cloranfenicol/química , Cloranfenicol/isolamento & purificação , Cromatografia Líquida de Alta Pressão/métodos , Resíduos de Drogas/análise , Resíduos de Drogas/química , Extração Líquido-Líquido/métodos , Reprodutibilidade dos Testes , Solventes , Espectrometria de Massas em Tandem/métodos
10.
Biosens Bioelectron ; 128: 113-121, 2019 Mar 01.
Artigo em Inglês | MEDLINE | ID: mdl-30641453

RESUMO

Ion-selective electrodes (ISE) can rapidly, sensitively detect their corresponding ions and are suitable for field testing. However, most ISE methods cannot detect other targets directly which limits their practice application. Herein, we established an aptamer-sensing platform to detect organic small molecule using a portable fluoride-selective electrode (FSE). To achieve the purpose, novel signal tags were fabricated based on nano metal-organic frameworks (NMOF) encapsulating F- and labeling aptamers. They were then immobilized on one stir-bar. Subsequently, a double stir-bars (bar-a and b) assisted target recycling strategy was designed to convert organic small molecular target to F- for signal development and amplification. The movement of tags from bar-a to b can be triggered by the analytes. After reaction, the transferred signal tags in bar-b were washed and released F- which can be measured by FSE for qualification of the target. The assay was evaluated to detect kanamycin or chloramphenicol which was employed as the representatives of organic small molecular with a low detection limit of 0.35 nmol L-1 or 0.46 nmol L-1, respectively. Satisfactory performance was observed in complex sample analysis of kanamycin (milk, fish, urine and serum) with a recovery of 91-108% and an RSD (n = 6) <5%. The proposed method broadens the application of traditional FSE to the detection of organic small molecule. And the employment of NMOF which has higher encapsulating capacity of F- for preparing signal tags can be extended to FSE based aptasensors.


Assuntos
Antibacterianos/isolamento & purificação , Técnicas Biossensoriais , Análise de Alimentos , Leite/química , Animais , Antibacterianos/química , Aptâmeros de Nucleotídeos/química , Cloranfenicol/química , Cloranfenicol/isolamento & purificação , Canamicina/química , Canamicina/isolamento & purificação , Limite de Detecção , Estruturas Metalorgânicas/química
11.
Biosens Bioelectron ; 126: 463-469, 2019 Feb 01.
Artigo em Inglês | MEDLINE | ID: mdl-30472443

RESUMO

Constructing junctions between semiconductors is an effective way to promote charge separation and thus to improve the photoelectrochemical (PEC) performances, and specifically, p-n heterojunction is considered as a very promising structure. Herein, we designed and fabricated MoS2/nitrogen doped graphene hydrogels (MoS2/NGH) p-n heterojunction by a facile one-pot hydrothermal route. The as-fabricaterd MoS2/NGH heterostructures demonstrated the excellent PEC activity, exhibiting enhanced photocurrent intensity by the fast transfer and separation rate of photogenerated electron-hole owing to the construction of p-n heterojunction. Based on the high PEC performances of the MoS2/NGH heterostructure, a novel sensitive PEC sensor was developed for the determination of chloramphenicol (CAP) with the assistance of aptamer. In the presence of target molecules, the as-fabricated PEC sensor could recognize the CAP quickly and then consume the holes in the interface of heterostructures, inhibiting the recombination of photogenerated electron-hole pairs, resulting the enhanced photocurrent. Specially, with the concentration of CAP increased, the photocurrent enhanced gradually. Excellent linearity was obtained in the concentration range from 32.3 ng/L to 96.9 µg/L, and the limit of detection was 3.23 ng/L. Moreover, the as-fabricated PEC sensor exhibited rapid response, high stability, low-cost and high selectivity, which could be successfully applied to the analysis of CAP in honeycomb samples.


Assuntos
Aptâmeros de Nucleotídeos/química , Técnicas Biossensoriais , Cloranfenicol/isolamento & purificação , Grafite/química , Cloranfenicol/química , Hidrogéis/química , Limite de Detecção , Molibdênio/química , Nitrogênio/química , Semicondutores , Sulfetos/química
12.
Anal Bioanal Chem ; 411(4): 803-812, 2019 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-30542815

RESUMO

A simple and efficient method combining solid-phase extraction (SPE) with homogeneous liquid-liquid microextraction (HLLME) has been developed for fast pretreatment of chloramphenicol (CAP) from water samples prior to determination by high-performance liquid chromatography-ultraviolet detection. Oasis HLB sorbent was chosen for SPE. In HLLME, N,N-dimethylcyclohexylamine was used as a CO2-triggered switchable solvent that could switch reversibly between hydrophilic and hydrophobic forms. The parameters influencing both SPE and HLLME were investigated and optimized. Under the optimal conditions, the method exhibited low limit of detection (0.1 ng/mL), good linearity (0.5-50 ng/mL), acceptable precision (RSD <5.0%) and accuracy (RE <4.0%). An enrichment factor of 340 was obtained. The proposed method is simple, fast, cost-effective, and suitable for the determination of trace chloramphenicol in water matrices. Graphical abstract ᅟ.


Assuntos
Cloranfenicol/análise , Cloranfenicol/isolamento & purificação , Microextração em Fase Líquida/métodos , Extração em Fase Sólida/métodos , Solventes/química , Poluentes Químicos da Água/isolamento & purificação , Antibacterianos/análise , Antibacterianos/isolamento & purificação , Antibacterianos/normas , Cloranfenicol/normas , Cromatografia Líquida de Alta Pressão , Concentração de Íons de Hidrogênio , Interações Hidrofóbicas e Hidrofílicas , Limite de Detecção , Padrões de Referência , Reprodutibilidade dos Testes , Análise Espectral/métodos , Poluentes Químicos da Água/análise
13.
Biosens Bioelectron ; 127: 45-49, 2019 Feb 15.
Artigo em Inglês | MEDLINE | ID: mdl-30590222

RESUMO

We here report a novel method for antibiotic detection by making use of DNA/metal ion interaction coupled with Ag-DNAzyme cleavage-mediated signal amplification. Taking the analysis of chloramphenicol (CAP) as an example, upon the specific recognition between the antibiotic CAP and its aptamer, the secondary structure of the DNA aptamer shaped by C-Ag+-C base mismatches will be altered, liberating the pre-captured Ag+. Subsequently, the free Ag+ provided as a cofactor can activate the Ag-DNAzyme, which behaves recycled cleavage of substrate DNA on the electrode surface for signal amplification. The more CAP is present, the more Ag+ is released, thus more Ag-DNAzyme can be activated to achieve a higher electrochemical signal. Therefore, the target-responsive variation of electrochemical signal enables the sensitive detection of CAP. The proposed method is cost-effective only with plain metal ion as modulator. It has also been challenged with real food samples, indicating the potential to be a promising tool for food safety detection.


Assuntos
Antibacterianos/isolamento & purificação , Técnicas Biossensoriais , Cloranfenicol/isolamento & purificação , DNA/química , Antibacterianos/química , Cloranfenicol/química , DNA Catalítico/química , Análise de Perigos e Pontos Críticos de Controle , Íons/química , Limite de Detecção , Metais/química , Prata/química
14.
Biosens Bioelectron ; 124-125: 167-175, 2019 Jan 15.
Artigo em Inglês | MEDLINE | ID: mdl-30388558

RESUMO

Graphene has emerged as a novel material with enhanced electrical and structural properties that can be used for a multitude of applications from super-capacitors to biosensors. In this context, an ultra-sensitive biosensor was developed using a low-cost, simple and mask-free method based on laser-induced graphene technique for electrodes patterning. The graphene was produced on a polyimide substrate, showing a porous multi-layer structure with a resistivity of 102.4 ±â€¯7.3 Ω/square. The biosensor was designed as a 3-electrode system. Auxiliary and working electrodes were made of graphene by laser patterning and the reference electrode was handmade by casting a silver ink. A molecularly-imprinted polymer (MIP) was produced at the working electrode by direct electropolymerization of eriochrome black T (EBT). As proof-of-concept, the MIP film was tailored for chloramphenicol (CAP), a common contaminant in aquaculture. The resulting device was evaluated by cyclic voltammetry and electrochemical impedance spectroscopy readings against a redox standard probe. The limit of detection (LOD) was 0.62 nM and the linear response ranged from 1 nM to 10 mM. These analytical features were better than those produced by assembling the same biorecognition element on commercial graphene- and carbon-based screen-printed electrodes. Overall, the simplicity and quickness of the laser-induced graphene technique, along with the better analytical features obtained with the graphene-based electrodes, shows the potential to become a commercial approach for on-site sensing.


Assuntos
Técnicas Biossensoriais , Cloranfenicol/isolamento & purificação , Grafite/química , Impressão Molecular , Espectroscopia Dielétrica , Técnicas Eletroquímicas , Lasers , Polímeros/química
15.
Anal Chim Acta ; 1047: 231-237, 2019 Jan 24.
Artigo em Inglês | MEDLINE | ID: mdl-30567655

RESUMO

Removal of organic solvent from sample extracts is required before analysis by reversed phase HPLC to preserve chromatographic performance and allow for bigger injection volumes, boosting sensitivity. Herein, an automated on-line extraction evaporation procedure is integrated with HPLC analysis. The evaporation occurs inside a 200 µm microfluidic channel confined by a vapor permeable membrane. A feedback control algorithm regulates evaporation rate keeping the output flow rate constant. The evaporation process across this membrane was firstly characterized with water/solvent mixtures showing organic solvent removal capabilities. This system allowed continuous methanol, ethanol and acetonitrile removal from samples containing up to 80% organic solvent. An evaporative injection procedure was developed demonstrating the use of the device for fully integrated extract reconstitution coupled to HPLC analysis, applied to analysis of the antibiotic chloramphenicol in milk samples. Sample reconstitution and collection was performed in less than 10 min and can be executed simultaneously to HPLC analysis of the previous sample in a routine workflow, thus having minimal impact on the total sample analysis time when run in a sequence.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Solventes/química , Acetonitrilas/química , Animais , Cloranfenicol/isolamento & purificação , Etanol/química , Metanol/química , Microfluídica/métodos , Leite/química , Sistemas On-Line
16.
Molecules ; 23(11)2018 Nov 16.
Artigo em Inglês | MEDLINE | ID: mdl-30453532

RESUMO

A great deal of attention has been focused on the secondary metabolites produced by marine endophytic fungi, which can be better alternatives to chemicals, such as biopesticides, for control of polyphagous pests. On the basis of its novel biocontrol attributes, chemical investigation of a marine alga-derived endophytic fungus, Acremonium vitellinum, resulted in the isolation of three chloramphenicol derivatives (compounds 1⁻3). Their chemical structures were elucidated by detailed analysis of their nuclear magnetic resonance spectra, high-resolution electrospray ionization mass spectrometry, and by comparison with the data available in the literature. In this paper, compound 2 was firstly reported as the natural origin of these fungal secondary metabolites. The insecticidal activities of compounds 1⁻3 against the cotton bollworm, Helicoverpa armigera, were evaluated. The natural compound 2 presented considerable activity against H. armigera, with an LC50 value of 0.56 ± 0.03 mg/mL (compared to matrine with an LC50 value of 0.24 ± 0.01 mg/mL). Transcriptome sequencing was used to evaluate the molecular mechanism of the insecticidal activities. The results presented in this study should be useful for developing compound 2 as a novel, ecofriendly and safe biopesticide.


Assuntos
Acremonium/fisiologia , Cloranfenicol/farmacologia , Regulação da Expressão Gênica/efeitos dos fármacos , Inseticidas/farmacologia , Larva/crescimento & desenvolvimento , Lepidópteros/crescimento & desenvolvimento , Controle Biológico de Vetores , Animais , Cloranfenicol/química , Cloranfenicol/isolamento & purificação , Proteínas de Insetos/genética , Inseticidas/química , Inseticidas/isolamento & purificação , Larva/efeitos dos fármacos , Larva/genética , Lepidópteros/efeitos dos fármacos , Lepidópteros/genética
17.
J Chromatogr B Analyt Technol Biomed Life Sci ; 1100-1101: 113-121, 2018 Nov 15.
Artigo em Inglês | MEDLINE | ID: mdl-30308418

RESUMO

In this study, an efficient, selective, and simple analytical method for the extraction of chloramphenicol (CAP) from food using magnetic molecularly imprinted polymers (MMIPs) as the solid-phase extraction (SPE) sorbent was successfully developed. MMIPs with varying ratios of methacrylic acid to acrylamide were prepared by suspension polymerization on the surface of double-bond-modified Fe3O4 magnetic nanoparticles. Further, these MMIPs were characterized by Fourier transform infrared spectroscopy and scanning electron microscopy, as well as using a vibrating sample magnetometer. Furthermore, the adsorption capacities of MMIPs and MNIPs were investigated by binding experiments. Methodology evaluation for the detection of CAP from food was carried out using MMIPs as the SPE sorbent. By using an external magnetic field, MMIPs were separated by a simple and rapid method. The diameter of the so-obtained MMIPs, exhibiting good monodispersity, was 400-700 nm. The MMIPs exhibited the maximum apparent adsorption capacity of up to 42.60 mg g-1 with good selectivity. For the detection of food samples, the linear response range was 0.02-10.00 mg L-1, with a detection limit of 10 µg L-1, and intra- and inter-day stabilities ranged from 1.34% to 1.89% and from 1.76% to 2.77%, respectively, with good recoveries (95.31%-106.89%) and satisfactory relative standard deviations (1.21%-2.60%).


Assuntos
Cloranfenicol/análise , Resíduos de Drogas/análise , Contaminação de Alimentos/análise , Nanopartículas de Magnetita/química , Impressão Molecular/métodos , Animais , Cloranfenicol/química , Cloranfenicol/isolamento & purificação , Cromatografia Líquida de Alta Pressão/métodos , Resíduos de Drogas/química , Resíduos de Drogas/isolamento & purificação , Mel/análise , Limite de Detecção , Modelos Lineares , Carne/análise , Reprodutibilidade dos Testes , Suínos
18.
Food Chem ; 269: 542-548, 2018 Dec 15.
Artigo em Inglês | MEDLINE | ID: mdl-30100471

RESUMO

A widely applicable method involving liquid chromatography-electrospray ionization tandem triple quadrupole mass spectrometry (LC-ESI/MS/MS) was developed for the simultaneous determination of chloramphenicol, thiamphenicol, florfenicol, and florfenicol amine in eggs. Samples were extracted with ethyl acetate-acetonitrile-ammonium hydroxide (49:49:2, v/v) and defatted with hexane saturated with acetonitrile. The analysis was carried out on a mass spectrometer via an electrospray interface operated in the positive and negative ionization modes using deuterated chloramphenicol-d5 as the internal standard. The limits of detection and limits of quantification were 0.04-0.5 µg/kg and 0.1-1.5 µg/kg in eggs, respectively. The average recoveries of the four analytes from egg samples were 90.84-108.23%, with relative standard deviations of less than 9.61%. The corresponding intra-day and inter-day variations were found to be less than 8.11% and 11.30%, respectively. Finally, the new approach was successfully applied to the quantitative determination of these analytes in 50 commercial eggs from local supermarkets.


Assuntos
Resíduos de Drogas/análise , Ovos/análise , Contaminação de Alimentos/análise , Espectrometria de Massas por Ionização por Electrospray/métodos , Espectrometria de Massas em Tandem/métodos , Cloranfenicol/isolamento & purificação , Cromatografia Líquida , Reprodutibilidade dos Testes , Tianfenicol/análogos & derivados , Tianfenicol/isolamento & purificação
19.
Mar Pollut Bull ; 133: 750-755, 2018 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-30041372

RESUMO

This study highlights an efficient sample pre-treatment method for preconcentration and detection of chloramphenicol in marine water using molecularly imprinted solid-phase extraction (MISPE). Chloramphenicol molecularly imprinted microspheres were prepared and evaluated on the base of morphology, capacity and selectivity. The imprinted microspheres exhibited specific recognition and high retention capability to chloramphenicol and were applied as special solid-phase extraction adsorbents. An off-line MISPE protocol has been optimized and a creative analytical method coupled to HPLC-DAD was successfully developed for the cleanup and determination of chloramphenicol in seawater samples. Method performance was satisfactory with recoveries ranging from 81 to 90% and relative standard deviation (RSD) was <4.93% (n = 3). Accuracy of the method was assessed at three spiking concentration levels and the limit of detection was 5 ng L-1. Finally, five seawater samples from Jiaozhou Bay of China were determined and the results showed that there was no chloramphenicol detected.


Assuntos
Antibacterianos/isolamento & purificação , Cloranfenicol/isolamento & purificação , Polímeros/química , Água do Mar/química , Extração em Fase Sólida/métodos , Poluentes Químicos da Água/isolamento & purificação , Antibacterianos/química , Baías/química , China , Cloranfenicol/análise , Cromatografia Líquida de Alta Pressão , Impressão Molecular , Polímeros/síntese química , Extração em Fase Sólida/instrumentação , Poluentes Químicos da Água/análise
20.
Water Res ; 128: 383-392, 2018 01 01.
Artigo em Inglês | MEDLINE | ID: mdl-29126034

RESUMO

Hospital effluents are a major source for the occurrence of pharmaceuticals in the environment. In this work, the treatment of synthetic urine polluted with chloramphenicol is studied by using three different conductive-diamond electrochemical oxidation technologies: electrolysis (single electrolysis), photoelectrolysis and high-frequency ultrasound sonoelectrolysis. These technologies were evaluated at 10 and 100 mA cm-2. Results shows that not only chloramphenicol but also other organics contained in urine are completely mineralized by electrolysis. Ammonium is the main inorganic nitrogen species formed and it can react with the electrogenerated hypochlorite, favouring the formation of chloramines. These species prevent the potential formation of perchlorate from chlorides contained in urine at low current densities (10 mA cm-2) and delay its occurrence at high current densities (100 mA cm-2). On the other hand, irradiation of ultraviolet (UV) light or high-frequency ultrasound (US) produce changes in the performance of the electrolytic treatment, but these changes are not as important as in other cases of study shown in the literature. Nonetheless, the effect of electroirradiated technologies seems to be higher and depends on the type of pollutant when working at low current densities (10 mA cm-2). It is positive in the case of the degradation of the antibiotic and the uric acid and negative in the case of urea where there is a clear antagonistic effect. Production of oxidants increases with the current density although in lower ratio than expected. These results are of great importance because clearly point out that electrolytic technologies can be applied to minimize the diffuse pollution associated to pharmaceuticals before discharge into municipal sewers.


Assuntos
Antibacterianos/isolamento & purificação , Cloranfenicol/isolamento & purificação , Eletrólise/métodos , Eliminação de Resíduos Líquidos/métodos , Cloretos , Diamante , Eletrodos , Eletrólitos , Hospitais , Oxidantes , Oxirredução , Percloratos , Tecnologia , Urina
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