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1.
Bioelectrochemistry ; 158: 108725, 2024 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-38714062

RESUMO

An enzymatic amperometric uric acid (UA) biosensor was successfully developed by modifying a screen-printed carbon electrode (SPCE) with Prussian blue-poly(3,4-ethylene dioxythiophene) polystyrene sulfonate composite (PB-PEDOT:PSS). The modified SPCE was coated with gold nanoparticles-graphene oxide-chitosan composite cryogel (AuNPs-GO-CS cry). Uricase (UOx) was directly immobilized via chemisorption on AuNPs. The nanocomposite was characterized by scanning electron microscopy, transmission electron microscopy, ultraviolet-visible spectroscopy, and Fourier transform infrared spectroscopy. The electrochemical characterization of the modified electrode was performed by cyclic voltammetry and electrochemical impedance spectroscopy. UA was determined using amperometric detection based on the reduction current of PB which was correlated with the amount of H2O2 produced during the enzymatic reaction. Under optimal conditions, the fabricated UA biosensor in a flow injection analysis (FIA) system produced a linear range from 5.0 to 300 µmol L-1 with a detection limit of 1.88 µmol L-1. The proposed sensor was stable for up to 221 cycles of detection and analysis was rapid (2 min), with good reproducibility (RSDs < 2.90 %, n = 6), negligible interferences, and recoveries from 94.0 ± 3.9 to 101.1 ± 2.6 %. The results of UA detection in blood plasma were in agreement with the enzymatic colorimetric method (P > 0.05).


Assuntos
Técnicas Biossensoriais , Criogéis , Eletrodos , Ouro , Grafite , Limite de Detecção , Nanopartículas Metálicas , Ácido Úrico , Técnicas Biossensoriais/métodos , Ácido Úrico/sangue , Ácido Úrico/análise , Ouro/química , Grafite/química , Criogéis/química , Nanopartículas Metálicas/química , Carbono/química , Polímeros/química , Porosidade , Análise de Injeção de Fluxo , Compostos Bicíclicos Heterocíclicos com Pontes/química , Quitosana/química , Poliestirenos/química , Enzimas Imobilizadas/química , Enzimas Imobilizadas/metabolismo , Humanos , Urato Oxidase/química , Técnicas Eletroquímicas/métodos , Nanocompostos/química , Ferrocianetos/química
2.
Anal Chim Acta ; 1302: 342516, 2024 May 08.
Artigo em Inglês | MEDLINE | ID: mdl-38580411

RESUMO

Conventional plate electrodes were commonly used in electrochemical flow injection analysis and only part of molecules diffused to the plane of electrodes could be detected, which would limit the performance of electrochemical detection. In this study, a low-cost native stainless steel wire mesh (SSWM) electrode was integrated into a 3D-printed device for electrochemical flow injection analysis with a pass-through mode, which is different compared with previous flow-through mode. This strategy was applied for sensitive analysis of hydrogen peroxide (H2O2) released from cells. Under the optimal conditions (the applied potentials, the flow rate and the sample volume), the device exhibits high sensitivity toward H2O2. Linear relationships could be achieved between electrochemical responses and the concentration of H2O2 ranging from 1 nM to 1 mM. The excellent analytical performance of the SSWM-based device could be attributed to the pass-through mode based on the mesh microstructure and intrinsic catalytic properties for H2O2 by stainless steel. This approach could be further successfully extended for screening of H2O2 released from HeLa cells with electrochemical responses linear to the number of cells in a range of 3 - 1.35 × 104 cells with an injection volume of 30 µL. This study revealed the potential of mesh electrodes in electrochemical flow injection analysis for cellular function and pathology and its possible extension in cell counting and on-line analysis.


Assuntos
Análise de Injeção de Fluxo , Peróxido de Hidrogênio , Humanos , Células HeLa , Peróxido de Hidrogênio/análise , Aço Inoxidável , Técnicas Eletroquímicas , Eletrodos
3.
Talanta ; 275: 125963, 2024 Aug 01.
Artigo em Inglês | MEDLINE | ID: mdl-38643712

RESUMO

This work introduces an innovative gold-leaf flow cell for electrochemical detection in flow injection (FI) analysis. The flow cell incorporates a hammered custom gold leaf electrochemical sensor. Hammered gold leaves consist of pure gold and are readily available in Thailand at affordable prices (approximately $0.085 for a sheet measuring 40 mm × 40 mm). Four sensing devices can be made from a single sheet of this gold leaf, resulting in a production cost of approximately $0.19 per sensor. Each electrochemical sensor has the gold leaf as the working electrode, together with a printed carbon strip, and a printed silver/silver chloride strip as the counter and reference electrodes, respectively. Initial investigations using cyclic voltammetry of a standard 1000 µmol L⁻1 iodide solution in 60 mmol L⁻1 phosphate buffer (PB) solution at pH 5, demonstrated performance comparable to that of a commercial screen-printed gold electrode. The hammered gold leaf electrode was then installed in a commercial flow cell as part of an FI system. A sample or standard iodide solution (100 µL) is injected into the first carrier stream of phosphate buffer (PB) solution, which then merges to mix with the second stream of the same buffer solution before flowing into the flow cell for amperometric detection of iodide. The optimized operating conditions include a fixed potential of +0.39 V (vs Ag/AgCl), and a total flow rate of 3 mL min⁻1. A linear calibration is obtained in the concentration range of 1 to 1000 µmol L⁻1 I- with a typical equation of µA = (0.00299 ± 0.00004) × (µmol L-1 I-) + (0.021 ± 0.020), and R2 = 0.9994. Analysis of iodide using this gold leaf-FI system is rapid with sample throughput of 86 samples h⁻1 and %RSD of a sample of 100 µmol L⁻1 I⁻ of 1.2 (n = 29). The limit of detection, (calculated as 2.78 × SD of regression line/slope), is 27 µmol L⁻1 I-. This method was successfully applied to determine iodide in nuclear emergency tablets.


Assuntos
Técnicas Eletroquímicas , Eletrodos , Ouro , Iodetos , Comprimidos , Iodetos/análise , Ouro/química , Comprimidos/análise , Técnicas Eletroquímicas/métodos , Técnicas Eletroquímicas/instrumentação , Análise de Injeção de Fluxo/métodos , Limite de Detecção
4.
Anal Methods ; 16(4): 589-598, 2024 01 25.
Artigo em Inglês | MEDLINE | ID: mdl-38193655

RESUMO

Efficient evaluation of adsorption kinetics of plant total polyphenols is essential for the design of adsorption separation of bioactive compounds. The conventional method uses manual sampling with poor reproducibility. Here, we developed a new method for on-line determination of total polyphenol content (TPC) in plant extracts by applying the Folin-Ciocalteu method in flow-injection analysis (FIA). The FIA parameters were optimized and a standard curve with excellent linearity was established. Precise determination of TPC with a satisfactory sample throughput of 20 h-1 was achieved for the adsorption kinetic study. The pseudo-second-order kinetic model was found to better describe the kinetic parameters of the batch adsorption/desorption process. The developed method proved to be accurate compared with the conventional method. The FIA method holds significant promise for studying and monitoring adsorption processes, due to its automatic on-line nature, low consumption of reagents and samples, and the ability to generate large quantities of highly accurate adsorption data.


Assuntos
Análise de Injeção de Fluxo , Polifenóis , Polifenóis/análise , Adsorção , Reprodutibilidade dos Testes , Análise de Injeção de Fluxo/métodos , Plantas
5.
Anal Chim Acta ; 1280: 341857, 2023 Nov 01.
Artigo em Inglês | MEDLINE | ID: mdl-37858551

RESUMO

A thin-layer flow cell of low internal volume (12 µL) is incorporated in a flow injection analysis (FIA) system for simultaneous and real-time photoelectrochemical (PEC) immunoassay of anti-SARS-CoV-2 spike 1 (S1) and anti-SARS-CoV-2 nucleocapsid (N) antibodies. Covalent linkage of S1 and N proteins to two separate polyethylene glycol (PEG)-covered gold nanoparticles (AuNPs)/TiO2 nanotube array (NTA) electrodes affords 10 consecutive analyses with surface regenerations in between. An indium tin oxide (ITO) allows visible light to impinge onto the two electrodes. The detection limits for anti-S1 and anti-N antibodies were estimated to be 177 and 97 ng mL-1, respectively. Such values compare well with those achieved with other reported methods and satisfy the requirement for screening convalescent patients with low antibody levels. Additionally, our method exhibits excellent intra-batch (RSD = 1.3%), inter-batch (RSD = 3.4%), intra-day (RSD = 1.0%), and inter-day (RSD = 1.6%) reproducibility. The obviation of an enzyme label and continuous analysis markedly decreased the assay cost and duration, rendering this method cost-effective. The excellent anti-fouling property of PEG enables accuracy validation by comparing our PEC immunoassays of patient sera to those of ELISA. In addition, the simultaneous detection of two antibodies holds great potential in disease diagnosis and immunity studies.


Assuntos
COVID-19 , Nanopartículas Metálicas , Humanos , SARS-CoV-2 , COVID-19/diagnóstico , Ouro , Reprodutibilidade dos Testes , Análise de Injeção de Fluxo , Proteínas do Nucleocapsídeo , Nucleocapsídeo/química , Anticorpos Antivirais , Imunoensaio/métodos
6.
Clin Chim Acta ; 549: 117551, 2023 Sep 01.
Artigo em Inglês | MEDLINE | ID: mdl-37683717

RESUMO

BACKGROUND: Dried Blood Spot (DBS) analysis has been used for identification and quantification of diseases and disorders in large populations. Simply collecting blood or plasma samples on cotton paper, followed with an organic solvent extraction, many small molecules can be detected and quantified. In a typical procedure of DBS analysis in newborn screening, stable isotope internal standards (SIIS) are added to extraction solvent as a reference. However, this way of employing SIIS does not reflect extraction efficiency, or protein binding issues, nor does it reflect potential degradation that could occur. In addition, punched-out discs from larger DBS are known to have imprecision typically ≥ 15%. METHODS: We developed and tested an approach, internal quantitative DBS (iqDBS), which delivers an exact volume of whole blood or plasma to a paper disc that is impregnated with a dried concentration of SIIS for quantitation. Amino acids were derivatized to make butyl esters and measured using Flow Injection Analysis with Selected Reaction Monitoring (FIA-SRM). RESULTS: We demonstrated with phenylalanine and tyrosine improved sensitivity and accuracy by applying iqDBS. CONCLUSIONS: We established a new method for quantitative analysis of small molecules from dried blood spots that incorporates stable isotope internal standard at the time of blood collection.


Assuntos
Fenilalanina , Tirosina , Humanos , Recém-Nascido , Análise de Injeção de Fluxo , Teste em Amostras de Sangue Seco/métodos , Isótopos , Solventes
7.
Anal Methods ; 15(38): 5071-5077, 2023 10 05.
Artigo em Inglês | MEDLINE | ID: mdl-37743796

RESUMO

This works presents a novel screen-printed carbon electrode modified with nickel hydroxide nanoparticles and chitosan (Ni(OH)2/CS/SPCE) for the non-enzymatic flow injection amperometric detection of glucose. The electrode was modified by drop-casting a suspension of the synthesised nanocomposite onto the screen-printed electrode and dried for 1 hour at room temperature. EDX analysis was used to investigate the chemical composition of the electrode before and after modifying. The electrochemical response of the unmodified SPCE and modified electrode was initially investigated by cyclic voltammetry (CV) using 0.1 M NaOH as the supporting electrolyte. CVs showed catalytic activity for glucose oxidation using the Ni(OH)2/CS/SPCE at 0.55 V. During flow injection analysis (FIA), 0.60 V and 1.5 mL min-1 were identified as the optimal potential and flow rate, respectively. A wide linear range of detection was observed (0.2 to 10.0 mM) with a sensitivity and limit of detection of 913 µA mM-1 cm-2 and 0.0174 mM, respectively. The modified electrode also displayed excellent repeatability (RSD = 0.47%, n = 20) and good reproducibility (RSD = 2.52%, n = 6). The modified electrode was shown to be very selectivity for glucose over other interferences commonly found in human blood samples. The practicality of the developed flow injection-amperometric system (FIA-Amp) was validated by the quantification of glucose in real serum samples, where results were in close agreement with those obtained from the local hospital.


Assuntos
Quitosana , Humanos , Níquel/química , Análise de Injeção de Fluxo , Reprodutibilidade dos Testes , Glucose/análise , Hidróxidos , Eletrodos
8.
Sensors (Basel) ; 23(12)2023 Jun 07.
Artigo em Inglês | MEDLINE | ID: mdl-37420564

RESUMO

Sumatriptan is an organic chemical compound from the tryptamine group. It is used as a medicine for migraine attacks and in the treatment of cluster headaches. In this work, a new voltammetric method is proposed for highly sensitive SUM determination, using glassy carbon electrodes modified with carbon black and titanium dioxide suspension. The novelty of the presented work is the usage of the mixture of carbon black and TiO2 as glassy carbon electrode modifier for the first time for SUM determination. The mentioned sensor was characterized by great repeatability and sensitivity of measurements, which resulted in the obtention of a wide range of linearity and a low detection limit. The electrochemical properties of the CB-TiO2/GC sensor was characterized using the LSV and EIS method. The effect of different factors on the SUM peak, such as supporting electrolyte type, preconcentration time and potential, or influence of interferents, were tested using the square wave voltammetry technique. The linear voltammetric response for the analyte was obtained in the concentration range of 5 nmol L-1 to 150 µmol L-1 with a detection limit of 2.9 nmol L-1 for a preconcentration time of 150 s in the 0.1 mol L-1 phosphate buffer pH 6.0. The proposed method was successfully applied for highly sensitive sumatriptan determination in complex matrices, such as tablets, urine, and plasma, with a good recovery parameter (94-105%). The presented CB-TiO2/GC electrode is characterized by great stability, it was used for 6 weeks without significant changes in the SUM peak current. Amperometric and voltammetric measurements of SUM under the flow injection conditions were also performed to indicate the possibility of its fast and accurate determination with a time of single analysis of approx. 30 s.


Assuntos
Carbono , Sumatriptana , Carbono/química , Análise de Injeção de Fluxo , Fuligem , Eletrodos , Fosfatos , Técnicas Eletroquímicas
9.
Phytochem Anal ; 34(8): 1009-1021, 2023 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-37518673

RESUMO

INTRODUCTION: Dahlia pinnata Cav. is a flower native to Mexico that has many applications; in particular, its petals have been used for ornamental, food, and medicinal purposes, for example to treat skin rashes and skin cracks. It has been reported that the medicinal properties of plants are generally related to the phytochemical constituents they possess. However, there are few studies on black D. pinnata. OBJECTIVES: The present study was aimed at qualitatively and quantitatively determining the phytochemical profile of petals from black D. pinnata. METHODOLOGY: Phytochemicals from Dahlia petals were extracted by consecutive maceration (hexane, dichloromethane, and methanol); then, the extracts were analyzed through colorimetric assays and UV-Vis spectroscopy for qualitative identification and quantification of phytochemical compounds, respectively. The methanolic extract was analyzed by flow injection analysis-electrospray ionization-Fourier transform ion cyclotron resonance mass spectrometry (FIA-ESI-FTICR-MS) in negative and positive mode. RESULTS: Quantitative phytochemical profiling of the methanolic extract by UV-Vis spectroscopy indicated high contents of phenolic compounds (34.35 ± 3.59 mg EQ/g plant) and sugars (23.91 ± 1.99 mg EQ/g plant), while the qualitative profiling by FIA-ESI-FTICR-MS allowed the tentative identification of several flavonoids and phenolic acids. Kaempferol-3-rutinoside, pelargonidin-3-(6″-malonylglucoside)-5-glucoside, rutin, kaempferol-3-(2″,3″-diacetyl-4″-p-coumaroylrhamnoside), and myricetin-3-(2‴-galloylrhamnoside) were the main compounds detected. CONCLUSION: The results expand our knowledge of the phytochemical constituents of petals from black D. pinnata.


Assuntos
Dahlia , Espectrometria de Massas por Ionização por Electrospray , Espectrometria de Massas por Ionização por Electrospray/métodos , Quempferóis , Ciclotrons , Análise de Injeção de Fluxo , Análise de Fourier , Extratos Vegetais/química , Metanol , Compostos Fitoquímicos/análise
10.
Luminescence ; 38(6): 680-691, 2023 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-36995153

RESUMO

The online photoreaction of the rose bengal photosensitized luminol-copper (II) chemiluminescence (CL) system was used for the determination of ß-nicotinamide adenine dinucleotide (NADH) and ethanol (EtOH) in pharmaceutical formulations combined with a flow injection technique. NADH can significantly enhance the CL emission of the reaction. For EtOH, alcohol dehydrogenase in soluble form was utilized in the presence of nicotinamide adenine dinucleotide resulting in NADH production. The limit of detection (3σ blank, 𝑛 = 3) of 4.0 × 10-8 and 2.17 × 10-5  M, and linear range 1.3 × 10-7 to 2.5 × 10-5  M (R2  = 0.9998, n = 6) and 0.11-2.17 × 10-3  M (R2  = 0.9996, n = 6) were obtained for NADH and EtOH respectively. The injection rate was 100 h-1 with a relative standard deviation (n = 3) of 1.5-4.8% in the range studied for both analytes. The procedure was satisfactorily applied to pharmaceutical formulations with recoveries in the range 91.6 ± 3.0% to 110 ± 2.0% for NADH and 88 ± 3.0% to 95.4 ± 4.0% for EtOH. The results obtained were very consistent and did not differ considerably from the reported approaches at a 95% confidence limit. The possible mechanism of the CL reaction is also explained briefly.


Assuntos
Luminol , NAD , Cobre , Rosa Bengala , Luminescência , Medições Luminescentes/métodos , Análise de Injeção de Fluxo/métodos , Preparações Farmacêuticas
11.
Luminescence ; 38(5): 647-661, 2023 May.
Artigo em Inglês | MEDLINE | ID: mdl-36967642

RESUMO

A flow injection (FI) methodology using the acidic potassium permanganate (KMnO4 )-rhodamine-B (Rh-B) reaction with chemiluminescence (CL) detection was established to determine acetochlor and cartap-HCl pesticides in freshwater samples. Experimental parameters were optimized, and Chelex-100 cationic exchanger mini column and solid-phase extraction (SPE) were used as phase separation techniques. Linear calibration curves were observed for the standard solutions of acetochlor and cartap-HCl over the ranges 0.005-2.0 mg L-1 [y = 1155.8x + 57.551, R2  = 0.9999 (n = 8)] and 0.005-1.0 mg L-1 [y = 979.76x + 14.491, R2  = 0.9998 (n = 8)] with LODs and LOQs of 7.5 × 10-4 and 8.0 × 10-4  mg L-1 (3σ blank) and 2.5 × 10-3 and 2.7 × 10-3  mg L-1 (10σ blank), respectively, with an injection throughput of 140 h-1 . These methods were used to estimate acetochlor and cartap-HCl with or without the SPE procedure, respectively, in spiked freshwater samples. Results obtained were not significantly different at a 95% confidence level to those of other reported methods. Recoveries for acetochlor and cartap-HCl were obtained over the ranges 93-112% (RSD = 1.9-3.6%) and 98-109% (RSD = 1.7-3.8%), respectively. The most probable CL reaction mechanism was explored.


Assuntos
Ácidos , Luminescência , Rodaminas , Permanganato de Potássio , Água Doce , Análise de Injeção de Fluxo/métodos , Medições Luminescentes/métodos
12.
Clin Chem ; 69(5): 470-481, 2023 04 28.
Artigo em Inglês | MEDLINE | ID: mdl-36920064

RESUMO

BACKGROUND: Classical homocystinuria (HCU) results from deficient cystathionine ß-synthase activity, causing elevated levels of Met and homocysteine (Hcy). Newborn screening (NBS) aims to identify HCU in pre-symptomatic newborns by assessing Met concentrations in first-tier screening. However, unlike Hcy, Met testing leads to a high number of false-positive and -negative results. Therefore, screening for Hcy directly in first-tier screening would be a better biomarker for use in NBS. METHODS: Dried blood spot (DBS) quality control and residual clinical specimens were used in analyses. Several reducing and maleimide reagents were investigated to aid in quantification of total Hcy (tHcy). The assay which was developed and validated was performed by flow injection analysis-tandem mass spectrometry (FIA-MS/MS). RESULTS: Interferents of tHcy measurement were identified, so selective derivatization of Hcy was employed. Using N-ethylmaleimide (NEM) to selectively derivatize Hcy allowed interferent-free quantification of tHcy by FIA-MS/MS in first-tier NBS. The combination of tris(2-carboxyethyl)phosphine (TCEP) and NEM yielded significantly less matrix effects compared to dithiothreitol (DTT) and NEM. Analysis of clinical specimens demonstrated that the method could distinguish between HCU-positive, presumptive normal newborns, and newborns receiving total parenteral nutrition. CONCLUSIONS: Here we present the first known validated method capable of screening tHcy in DBS during FIA-MS/S first-tier NBS.


Assuntos
Homocistinúria , Triagem Neonatal , Humanos , Recém-Nascido , Triagem Neonatal/métodos , Espectrometria de Massas em Tandem/métodos , Homocistinúria/diagnóstico , Controle de Qualidade , Análise de Injeção de Fluxo , Homocisteína
13.
Anal Bioanal Chem ; 415(5): 935-951, 2023 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-36598539

RESUMO

Direct infusion of lipid extracts into the ion source of a mass spectrometer is a well-established method for lipid analysis. In most cases, nanofluidic devices are used for sample introduction. However, flow injection analysis (FIA) based on sample infusion from a chromatographic pump can offer a simple alternative to shotgun-based approaches. Here, we describe important modification of a method based on FIA and tandem mass spectrometry (MS/MS). We focus on minimizing contamination of the FIA/MS both to render the lipidomic platform more robust and to increase its capacity and applicability for long-sequence measurements required in clinical applications. Robust validation of the developed method confirms its suitability for lipid quantitation in human plasma analysis. Measurements of standard human plasma reference material (NIST SRM 1950) and a set of plasma samples collected from kidney cancer patients and from healthy volunteers yielded highly similar results between FIA-MS/MS and ultra-high-performance supercritical fluid chromatography (UHPSFC)/MS, thereby demonstrating that all modifications have practically no effect on the statistical output. Newly modified FIA-MS/MS allows for the quantitation of 141 lipid species in plasma (11 major lipid classes) within 5.7 min. Finally, we tested the method in a clinical laboratory of the General University Hospital in Prague. In the clinical setting, the method capacity reached 257 samples/day. We also show similar performance of the classification models trained based on the results obtained in clinical settings and the analytical laboratory at the University of Pardubice. Together, these findings demonstrate the high potential of the modified FIA-MS/MS for application in clinical laboratories to measure plasma and serum lipid profiles.


Assuntos
Lipidômica , Espectrometria de Massas em Tandem , Humanos , Espectrometria de Massas em Tandem/métodos , Lipidômica/métodos , Análise de Injeção de Fluxo , Plasma/química , Lipídeos/análise
14.
Talanta ; 254: 124172, 2023 Mar 01.
Artigo em Inglês | MEDLINE | ID: mdl-36535211

RESUMO

A certain group of mycotoxins, the ergot alkaloids, has caused countless deaths throughout human history. They are found in rye and other cereals and ingesting contaminated foods can cause serious health problems. To identify contaminated food exceeding the legal limits for ergot alkaloids, a portable and cost-effective test system is of great interest to the food industry. Rapid analysis can be achieved by screening for a marker compound, for which we chose ergometrine. We developed a magnetic bead-based immunoassay for ergometrine with amperometric detection in a flow injection system using a handheld potentiostat and a smartphone. With this assay a limit of detection of 3 nM (1 µg L-1) was achieved. In spiked rye flour, ergometrine levels from 25 to 250 µg kg-1 could be quantified. All results could be verified by optical detection. The developed assay offers great promise to meet the demand for on-site ergometrine detection in the food industry.


Assuntos
Ergonovina , Alcaloides de Claviceps , Humanos , Ergonovina/análise , Secale , Farinha/análise , Análise de Injeção de Fluxo , Alcaloides de Claviceps/análise , Imunoensaio , Fenômenos Magnéticos , Contaminação de Alimentos/análise
15.
Luminescence ; 38(2): 99-108, 2023 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-36494159

RESUMO

A novel flow injection-chemiluminescence (FI-CL) approach is proposed for the assay of pioglitazone hydrochloride (PG-HCl) based on its enhancing influence on the tris(2,2'-bipyridyl)ruthenium(II)-silver(III) complex (Ru(bipy)3 2+ -DPA) CL system in sulfuric acid medium. The possible CL reaction mechanism is discussed with CL and ultraviolet (UV) spectra. The optimum experimental conditions were found as: Ru(bipy)3 2+ , 5.0 × 10-5  M; sulfuric acid, 1.0 × 10-3  M; diperiodatoargentate(III) (DPA), 1.0 × 10-4  M; potassium hydroxide, 1.0 × 10-3  M; flow rate 4.0 ml min-1 for each flow stream and sample loop volume, 180 µl. The CL intensity of PG-HCl was linear in the range of 1.0 × 10-3 to 5.0 mg L-1 (R2 = 0.9998, n = 10) with limit of detection [LOD, signal-to-noise ratio (S/N) = 3] of 2.2 × 10-4  mg L-1 , limit of quantification (LOQ, S/N = 10) of 6.7 × 10-4  mg L-1 , relative standard deviation (RSD) of 1.0 to 3.3% and sampling rate of 106 h-1 . The methodology was satisfactorily used to quantify PG-HCl in pharmaceutical tablets with recoveries ranging from 93.17 to 102.77 and RSD from 1.9 to 2.8%.


Assuntos
Rutênio , Prata , Pioglitazona , 2,2'-Dipiridil , Luminescência , Medições Luminescentes/métodos , Análise de Injeção de Fluxo/métodos
16.
Molecules ; 27(24)2022 Dec 08.
Artigo em Inglês | MEDLINE | ID: mdl-36557822

RESUMO

Biogenic amines (BAs) occur in a wide variety of foodstuffs, mainly from the decomposition of proteins by the action of microorganisms. They are involved in several cellular functions but may become toxic when ingested in high amounts through the diet. In the case of oenological products, BAs are already present in low concentrations in must, and their levels rise dramatically during the fermentation processes. This paper proposes a rapid method for the determination of BAs in wines and related samples based on precolumn derivatization with dansyl chloride and further detection by flow injection analysis with tandem mass spectrometry. Some remarkable analytes such as putrescine, ethanolamine, histamine, and tyramine have been quantified in the samples. Concentrations obtained have shown interesting patterns, pointing out the role of BAs as quality descriptors. Furthermore, it has been found that the BA content also depends on the vinification practices, with malolactic fermentation being a significant step in the formation of BAs. From the point of view of health, concentrations found in the samples are, in general, below 10 mg L-1, so the consumption of these products does not represent any special concern. In conclusion, the proposed method results in a suitable approach for a fast screening of this family of bioactive compounds in wines to evaluate quality and health issues.


Assuntos
Vinho , Vinho/análise , Espectrometria de Massas em Tandem , Análise de Injeção de Fluxo , Aminas Biogênicas/análise , Histamina/análise , Cromatografia Líquida de Alta Pressão/métodos
17.
Luminescence ; 37(12): 2041-2049, 2022 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-36150887

RESUMO

This study developed a simple flow injection (FI) method based on diperiodatonickelate(IV)-sulfuric acid reaction using chemiluminescence (CL) detection for the determination of thiram (THI) fungicide in fresh water using quinine as the sensitizer. The possible mechanism of the CL reaction was described using UV-Vis. absorption and CL spectra. Experimental variables were optimized by applying a univariate approach, and a linear calibration curve was obtained in the range of 1.0 × 10-3 -2.0 mg L-1 (R2 = 0.9994, n = 9) with a limit of detection of 5.0 × 10-4  mg L-1 (S/N = 3) and an injection throughput of 200 h-1 . This approach was successfully applied to determine THI in fresh water by using solid-phase extraction and achieved a good recovery rate of 94%-110% with a relative standard deviation of 1.9%-3.7% (n = 4). The results obtained were compared with the reported FI-CL and high-performance liquid chromatography-ultraviolet methods, and the three methods did not differ significantly at the 95% confidence limit.


Assuntos
Análise de Injeção de Fluxo , Tiram , Análise de Injeção de Fluxo/métodos , Quinina/química , Medições Luminescentes/métodos , Água Doce
18.
J Am Soc Mass Spectrom ; 33(10): 1865-1873, 2022 Oct 05.
Artigo em Inglês | MEDLINE | ID: mdl-36129040

RESUMO

Ion signals in electrospray ionization (ESI) mass spectrometry (MS) are affected by addition of acid or base. Acids or bases are typically added to samples to enhance detection of analytes in positive- or negative-ion mode, respectively. To carry out simultaneous monitoring of analytes with different ionogenic moieties by ESI-MS, a rapid acid/base switching system was developed. The system was further coupled with flow injection analysis (FIA) and liquid chromatography (LC) MS. The two variants enable detection of separated analytes immediately after alternating addition of acid and base. The methods were tested using a set of phospholipids (PLs) as analytes. The rapid acid/base switching enhanced signals of some of the PL analytes in both ion modes of MS. Both FIA-MS and LC-MS with acid/base switching show signal enhancements (∼1.3-23.2 times) of some analyte signals when compared with analysis conducted without acid/base switching. The proposed methods are suitable for simultaneous analysis of cationic and anionic analytes. The FIA-MS and LC-MS methods with acid/base switching were also applied in analysis of lipid extract from real samples (sausage and porcine liver). However, the FIA-MS results were affected by ionization competition and isobaric interference due to the complexity of the sample matrix and diversity of PL species. In contrast, the LC-MS mode provides adequate selectivity to observe signal enhancement for specific analyte ions. Overall, alternating addition of acid and base immediately before the ESI source can improve analytical performance without the need to carry out separate analyses targeting different types of analytes.


Assuntos
Análise de Injeção de Fluxo , Espectrometria de Massas por Ionização por Electrospray , Ácidos , Animais , Cromatografia Líquida de Alta Pressão/métodos , Cromatografia Líquida/métodos , Íons , Fosfolipídeos , Espectrometria de Massas por Ionização por Electrospray/métodos , Suínos
19.
Spectrochim Acta A Mol Biomol Spectrosc ; 283: 121713, 2022 Dec 15.
Artigo em Inglês | MEDLINE | ID: mdl-35952592

RESUMO

Inorganic arsenic especially As(III) is considered a carcinogenic substance and its measurement is important in water samples. In this work, an inexpensive flow injection analysis system was designed for the photometric determination of As(III) at low concentrations. For this purpose, a light-emitting diode (LED) based photometer with a miniaturized detector, was fabricated and used as a determination apparatus and methyl orange was used as a detecting reagent. The fabricated photometer employed the LEDs, as a light source and the light detector. The λmax of emission for emitter and detector LEDs were 525 and 625 nm, respectively. Determination of As (III) was based on its inhibition effect on the redox reaction between methyl orange and X2 (Cl2 or Br2). The decolorization of the reaction products in the FIA system was monitored using the homemade flow cell detector. Analytical figures of merit including linear responses ranging from 0.03 to 3.0 mg/l of As(III) (r = 0.994), detection limits of 0.007 mg/l As(III), RSD% of 1.5% (n = 7), low reagent consumption per determination, and sampling throughput of 50 determinations per hour were achieved.


Assuntos
Análise de Injeção de Fluxo , Fotometria , Compostos Azo , Indicadores e Reagentes
20.
J AOAC Int ; 106(1): 205-211, 2022 Dec 22.
Artigo em Inglês | MEDLINE | ID: mdl-35904530

RESUMO

BACKGROUND: Scientific, accurate, and rapid detection of the composition and content of tea polyphenols is an important basis for their rational use and giving full play to their physiological effect. The spectrophotometric assays for total polyphenols have poor selectivity. Therefore, there is a need to develop a simple and reliable method for the determination of the total polyphenolic level in tea products. OBJECTIVE: The aim of this research was to develop a flow injection chemiluminescence (FI-CL) method based on the Ag(III)-luminol system for the total polyphenol content analysis of tea and substitute tea. METHOD: Through Box-Behnken experimental design, we selected the optimum determination condition. The Ag(III) concentration was 5 × 10-5 mol/L, and the luminol concentration was 3 × 10-7 mol/L (including 0.15 mol/L NaOH). The peristaltic pump is 25 r/min, and the photomultiplier voltage is 600 v. Sample extracts were diluted 100 000 times for the FI-CL assay. RESULTS: Under optimal conditions, CL intensities were proportional to total polyphenol content (in terms of gallic acid concentrations) in the range of 0.1∼100 µg/L. The LOD and LOQ were 0.03 µg/L and 0.1 µg/L. The recovery values were in the range of 86.3-111.0% with a RSD of 1.04∼2.62%. The polyphenolic content of 12 teas and 6 substitute teas was determined, and the results of the developed method and Folin-Ciocalteu method were highly correlated (r = 0.9493 for tea and r = 0.8533 for substitute tea). CONCLUSIONS: The proposed method is better than the Folin-Ciocalteu method in terms of selectivity, sensitivity, and accuracy. It is suitable for the determination of polyphenol content not only in tea, but also in substitute tea. HIGHLIGHTS: We developed a new flow-injection analysis method for polyphenolic content determination based on the Ag(III)-luminol chemiluminescence system. It is simple, rapid, sensitive, and accurate. It is suitable for the determination of polyphenols content not only in tea, but also in substitute tea.


Assuntos
Luminol , Polifenóis , Polifenóis/análise , Luminol/análise , Luminescência , Medições Luminescentes/métodos , Análise de Injeção de Fluxo/métodos , Chá
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