RESUMEN
In this study, tannic acid (TA) was applied as a stabilizing agent for synthesizing bimetallic copper-gold (CuAu) nanoparticles. Cu(NO3)2 and NaAuCl4 were used as the sources of copper and gold ions, respectively, and NaBH4 was employed as a reducing agent. The prepared TA-CuAu nanoparticles were extensively characterized via ultraviolet-visible spectroscopy, Fourier transform infrared spectroscopy, transmission electron microscopy, X-ray diffraction, and zeta potential analyses. To evaluate their catalytic activity, the TA-CuAu nanoparticles and NaBH4 were applied in the degradation of 4-nitrophenol (4-NP) and rhodamine B (RB) individually and in a mixture. The individual degradation of 4-NP and RB was completed within 10 min, and the apparent rate constants were calculated as 0.3046 and 0.2628 min-1, respectively, emphasizing the efficient catalytic activity of the TA-CuAu nanoparticles. Additionally, controlled experiments were performed for the degradation of 4-NP and RB in the absence of catalysts or NaBH4 to investigate the kinetic feasibility of the catalytic reactions. A mixture of 4-NP and RB was successfully degraded within 10 min using the TA-CuAu nanoparticles as catalysts. Furthermore, the reuse of the catalysts after five successive cycles demonstrates an outstanding performance with no significant loss in the catalytic activity. Finally, the successful treatment of the tap and lake water samples spiked with 4-NP and RB using the TA-CuAu nanoparticles further confirmed their application potential as catalysts in environmental water remediation.
RESUMEN
Excessive administration of penicillin G and improper disposal of its residues pose a serious risk to human health; therefore, the development of convenient methods for monitoring penicillin G levels in products is essential. Herein, novel gold-silver nanoclusters (AuAgNCs) were synthesized using chicken egg white and 6-aza-2-thiothymine as dual ligands with strong yellow fluorescence at 509 and 689 nm for the highly selective detection of penicillin G. The AuAgNCs were characterized using transmission electron microscopy, X-ray photoelectron spectroscopy, ultraviolet-visible absorption spectrophotometry, and fluorescence spectrophotometry. Under optimum conditions, the fluorescence intensity decreased linearly with the concentration of penicillin G from 0.2 to 6 µM, with a low detection limit of 18 nM. Real sample analyses indicated that a sensor developed using the AuAgNCs could detect penicillin G in urine and water samples within 10 min, with the recoveries ranging from 99.7 to 104.0%. The particle size of the AuAgNCs increased from 1.80 to 9.06 nm in the presence of penicillin G. We believe the aggregation-induced quenching of the fluorescence of the AuAgNCs was the main mechanism for the detection of penicillin G. These results demonstrate the ability of our sensor for monitoring penicillin G levels in environmental and clinic samples.
RESUMEN
This study developed a facile, highly sensitive technique for extracting and quantifying barbiturates in serum samples. This method combined ultrasound and surfactant-assisted dispersive liquid-liquid microextraction with poly(ethylene oxide)-mediated stacking in capillary electrophoresis. Factors influencing the extraction and stacking performance, such as the type and volume of extraction solvents, the type and concentration of surfactant, extraction time, salt additives, sample matrix, solution pH, and composition of the background electrolyte, were carefully studied and optimized to achieve the optimal detection sensitivity. Under the optimized extraction (injecting 140 µL C2 H4 Cl2 into 1 mL of sample with pH 4 (5 mM sodium phosphate containing 0.05 mM Tween 20 and sonication for 1 min) and separation conditions (150 mM tris(hydroxymethyl)aminomethane-borate with pH 8.5 containing 0.5% (m/v) poly(ethylene oxide)), the limits of detection (signal-to-noise ratio = 3) of five barbiturates ranged from 0.20 to 0.33 ng/mL, and the calculated sensitivity improvement ranged from 868- to 1700-fold. The experimental results revealed excellent linearity (R2 > 0.99), with relative standard deviations of 2.1%-3.4% for the migration time and 4.3%-5.7% for the peak area. The recoveries of the spiked serum samples were 97.1% -110.3%. Our proposed approach offers a rapid and practical method for quantifying barbiturates in biological fluids.
Asunto(s)
Microextracción en Fase Líquida , Tensoactivos , Humanos , Polietilenglicoles , Óxido de Etileno , Microextracción en Fase Líquida/métodos , Solventes/química , Límite de DetecciónRESUMEN
This study proposes the use of thiomalic acid-modified Au and Ag nanoparticle mixtures (TMA-Au/AgNP mixes) for the selective detection of tricyclazole. Upon the addition of tricyclazole, the color of TMA-Au/AgNP mixes solution changes from orange-red to lavender (red-shift). According to the density-functional theory calculations, tricyclazole-induced aggregation of TMA-Au/AgNP mixes through electron donor-acceptor interactions was proved. The sensitivity and selectivity of the proposed method are affected by the amount of TMA, volume ratio of TMA-AuNPs to TMA-AgNPs, pH value, and buffer concentration. The ratio of absorbance (A654/A520) of TMA-Au/AgNP mixes solution is proportional to the concentration of tricyclazole over the range 0.1-0.5 ppm with a linear correlation (R2 = 0.948). Moreover, the limit of detection was estimated at 0.028 ppm. The practicality of TMA-Au/AgNP mixes was validated for the determination of tricyclazole concentration in real samples (spiked recovery was 97.5%-105.2%), demonstrating its advantages of simplicity, selectivity, and sensitivity.
Asunto(s)
Nanopartículas del Metal , Oro , Plata , TiazolesRESUMEN
Green emission carbon dots (CDs) electrochemically prepared from 2,6-pyridinedicarboxylic acid and o-phenyl-enediamine were applied separately for the quantitation of hypochlorite and carbendazim. The characteristic and optical properties of the CDs were studied through fluorescence, UV-vis absorption, X-ray photoelectron spectroscopy, and transmission electron microscopy. The synthesized CDs were mainly 0.8-2.2 nm in size, with an average size of 1.5 nm. The CDs exhibited green luminescence centered at 520 nm when excited by 420 nm light. The green emission of the CDs is quenched after the addition of hypochlorite, mainly through the redox reaction between hypochlorite and hydroxyl groups on the CDs surface. Furthermore, the hypochlorite-induced fluorescence quenched can be prevented in the presence of carbendazim. The sensing approaches exhibit good linear ranges of 1-50 µM and 0.05-5 µM for hypochlorite and carbendazim, respectively, with low detection limits of 0.096 and 0.005 µM, respectively. Practicalities of the luminescent probes were separately validated by the quantitation of the two analytes in real sample matrix with recoveries ranging from 96.3 to 108.9% and the relative standard deviation values below 5.51%. Our results show the potential of the sensitive, selective, and simple CD probe for water and food quality control.
Asunto(s)
Ácido Hipocloroso , Puntos Cuánticos , Puntos Cuánticos/química , Carbono , Espectroscopía de FotoelectronesRESUMEN
Sodium alginate (SA) was used to functionalize the surfaces of silver nanoparticles (AgNPs) to form SA-AgNPs for sensing dimethoate with a rapid and sensitive visual readout. UV-Vis spectrophotometry, Fourier transform infrared spectroscopy, transmission electron microscopy, X-ray photoelectron spectroscopy, and zeta potential measurements were used to characterize SA-AgNPs that were synthesized under the ideal conditions. SA-AgNPs were spherical with an average size of 14.6 nm. The stability of SA-AgNPs was investigated with changes in pH, salinity, and storage time. This colorimetric assay of dimethoate relied on the change in the absorption ratio (A475/A400) of SA-AgNPs, resulting in their aggregation caused by dimethoate, leading to a visual change for SA-AgNPs from yellow to pale yellow. As a result, the absorption ratio (A475/A400) of SA-AgNPs showed good linearity in the range of 0.05 to 2.0 ppm (R2 = 0.9986) with a limit of detection (LOD) of 30 ppb. Adding other pesticides did not significantly change the absorption ratio of SA-AgNPs, indicating its high selectivity as a colorimetric assay. The sensor was successfully used to detect dimethoate in actual water samples.
Asunto(s)
Dimetoato , Nanopartículas del Metal , Colorimetría/métodos , Alginatos , Plata/química , Nanopartículas del Metal/química , Sodio , Espectroscopía Infrarroja por Transformada de FourierRESUMEN
Nitrogen and sulfur codoped carbon dots (NSCDs) were synthesized via a one-pot hydrothermal method, and citric acid, ethylenediamine, and methyl blue were used as precursors. The obtained NSCDs were spherical with an average size of 1.86 nm. The fluorescence emission spectra of the NSCDs were excitation independent and emitted blue fluorescence at 440 nm with an excitation wavelength at 350 nm. The quantum yield of the NSCDs was calculated to be 68.0%. The NSCDs could be constructed as fluorescent probes for highly selective and sensitive sensing mercuric (Hg2+) and hypochlorite (ClO-) ions. As the addition of Hg2+ or ClO- ions to the NSCDs, the fluorescence intensity was effectively quenched due to dynamic quenching. Under the optimal conditions, the linear response of the fluorescence intensity ranged from 0.7 µM to 15 µM with a detection limit of 0.54 µM and from 0.3 µM to 5.0 µM with a limit of detection of 0.29 µM for Hg2+ and ClO- ions, respectively. Finally, the proposed method was successfully used for quantifying Hg2+ and ClO- ions in spiked tap water samples.
RESUMEN
A colorimetric assay for highly selective and sensitive detection of tricyclazole using fluorescein-functionalized silver nanoparticles (F-AgNPs) as sensing probes was investigated. As the addition of tricyclazole to F-AgNPs, a drastic decrease in the absorbance at 394 nm was detected, which was accompanied with a noticeable color change from yellow to gray. The sensing mechanism involved an interaction between tricyclazole and F-AgNPs, which led to aggregation of the latter, inducing a color change from yellow to gray. An excellent linear calibration curve (R2 = 0.9994) was achieved between absorbance at 394 nm and the tricyclazole concentration in the range between 0.06 and 1.0 ppm. Moreover, the detection limit was estimated at 0.051 ppm. The developed colorimetric assay also showed good selectivity and was successfully utilized to quantify tricyclazole in rice samples with satisfactory recoveries. The proposed assay has been successfully applied for monitoring tricyclazole in rice samples.
Asunto(s)
Colorimetría/métodos , Nanopartículas del Metal/química , Plata/química , Tiazoles/análisis , Fluoresceína/química , Límite de Detección , Oryza/química , Oryza/metabolismoRESUMEN
In this study, we developed a facile method for synthesizing dual-emission carbon nanodots (CDs) through trimesic acid and o-phenylenediamine through electrolysis for 2 h. The synthesized CDs were mainly 3-7 nm in size, with an average size of 5.17 nm. The dual-emission fluorescent property of these CDs could be observed under two different excitation wavelengths. The green emission of the CDs could be quenched after the addition of mercury ions or copper ions, and the blue emission of the CDs could be inhibited using hydroxychloroquine (HCQ). Furthermore, the quenched fluorescence of CDs/Cu2+ could be recovered through the addition of glyphosate. We developed a multifunctional chemical sensor by using these special fluorescence materials. Under optimal conditions, the detection limits of mercury ions, glyphosate, and HCQ were 0.42 µM, 1.1 mg L-1, and 0.14 µM, respectively. Moreover, this method can be used to detect mercury ions, glyphosate, and HCQ in environmental water, cereals, and urine samples, respectively.
RESUMEN
In the present article, we report a novel colorimetric probe (TNT@MB) for the detection of the phosphate ion, which is based on the strong binding affinity between the phosphate ion and titanium dioxide nanotubes (TNTs). TNTs were synthesized from TiO2 nanoparticles by hydrothermal treatment. The obtained TNTs had an average length of 200 ± 50 nm and an average width of 12 ± 5 nm. TNT@MB was prepared by adsorbing methyl blue onto TNTs in acidic condition. The optimal synthesis conditions for TNT@MB consisted in having 0.05 g of TNTs react with 1 µmole of methyl blue at pH 2 for 90 min. TNTs and TNT@MB were characterized by UV-vis diffuse reflection spectroscopy, TEM, FTIR, and XPS. The phosphate-ion sensing behavior of TNT@MB was investigated by UV-visible spectroscopy. The phosphate-ion concentration linear range and detection limit of this method based on TNT@MB were 1-40 µM and 0.59 µM, respectively. A sample of lake water was used as a real sample, and analyte recovery rates were measured in the 102.5-103.6% range, with relative standard deviations below 5.6% (n = 3). We also found that this probe could be reused after regeneration in alkaline solution. These results indicate that as a colorimetric probe, TNT@MB has the advantages of being environmentally friendly, inexpensive, and simple to use, as well as giving rise to an easily observable color change.
RESUMEN
Pesticides are a family of non-biodegradable chemical compounds which widely used in agriculture to control pests and increase yield production. However, overuse or abuse of pesticides and their metabolites may cause potential toxicity for the environment as well as human health and all other living organisms, even at deficient concentrations. Consequently, the development of sensors for monitoring these compounds is significant. Recently, nanoparticles-based sensors have been extensively employed as a potential alternative or complementary analytical tool to conventional detection methods for pesticides. Among them, gold nanoparticles (AuNPs) owing to their unique optical properties have been developed as smart sensors with high selectivity, sensitivity, simplicity, and portability. These comprehensive reviews have summarized various studies performed based on different detection strategies, i.e., colorimetric, fluorescence, surface-enhanced Raman scattering, and electrochemical, using AuNPs as sensing probes for pesticide analysis in various matrices. Additionally, the current challenges and future trends for developing novel AuNPs-based sensors for the detection of pesticides are also discussed.
RESUMEN
A novel sensing system has been designed for the detection of cupric ions. It is based on the quenched fluorescence signal of carbon dots (CDs), which were carbonized from poly(vinylpyrrolidone) (PVP) and L-Cysteine (CYS). Cupric ions interact with the nitrogen and sulfur atoms on surface of the CDs to form an absorbed complex; this results in strong quenching of the fluorescence of the CDs via a fast metal-to-ligand binding affinity. The synthesized water-soluble CDs also exhibited a quantum yield of 7.6%, with favorable photoluminescent properties and good photostability. The fluorescence intensity of the CDs was very stable in high ionic strength (up to 1.0 M NaCl) and over a wide range of pH levels (2.0-12.0). This facile method can therefore develop a sensor that offers reliable, fast, and selective detection of cupric ions with a detection limit down to 0.15 µM and a linear range from 0.5 to 7.0 µM (R2 = 0.980). The CDs were used for cell imaging, observed that they were low toxicity to Tramp C1 cells and exhibited blue and green and red fluorescence under a fluorescence microscope. In summary, the CDs exhibited excellent fluorescence properties, and could be applied to the selective and sensitive detection of cupric ion and multicolor cell imaging.
Asunto(s)
Carbono/química , Cobre/análisis , Imagenología Tridimensional/métodos , Sondas Moleculares/síntesis química , Puntos Cuánticos/química , Animales , Carbono/toxicidad , Muerte Celular/efectos de los fármacos , Línea Celular Tumoral , Supervivencia Celular/efectos de los fármacos , Fluorescencia , Iones , Ratones Transgénicos , Sondas Moleculares/química , Espectroscopía de Fotoelectrones , Puntos Cuánticos/toxicidad , Espectrometría de Fluorescencia , Espectrofotometría Ultravioleta , Espectroscopía Infrarroja por Transformada de Fourier , Contaminantes Químicos del Agua/análisisRESUMEN
Generally, metal nanoclusters are synthesized using only a single ligand. Thus, the properties and applications of these nanomaterials are limited by the nature of the ligand used. In this study, we have developed a new synthetic strategy to prepare bi-ligand copper nanoclusters (Cu NCs). These bi-ligand Cu NCs are synthesized from copper ions, thiosalicylic acid, and cysteamine by a simple one-pot method, and they exhibit high quantum yields (>18.9%) and good photostability. Most interestingly, the fluorescence intensities and surface properties of the Cu NCs can be tailored by changing the ratio of the two ligands. Consequently, the bi-ligand Cu NCs show great promise as fluorescent probes. Accordingly, the Cu NCs were applied to the inner-filter-effect-based detection of hexavalent chromium in water. A wide linear range of 0.1-1000 µM and a low detection limit (signal-to-noise ratio = 3) of 0.03 µM was obtained. The recoveries for the real sample analysis were between 98.3 and 105.0% and the relative standard deviations were below 4.54%, demonstrating the repeatability and practical utility of this assay.
RESUMEN
This study developed a sensitive method involving capillary electrophoresis (CE) coupled with ultraviolet absorption for the simultaneous separation of chiral phenothiazine drugs at nanomolar concentration levels. The method consists of hydroxypropyl-γ-cyclodextrin (Hp-γ-CD) as a chiral selector and poly (diallyldimethylammonium chloride) (PDDAC)-based CE. Five pairs of d,l-phenothiazines were baseline separated using a background electrolyte containing 0.9% PDDAC, 5 mM Hp-γ-CD, and 100 mM tris(hydroxymethyl)aminomethane (Tris)-formate (pH 3.0). The five pairs were successfully stacked on the basis of the difference in viscosity between the PDDAC-containing background electrolyte and the sample solution, with almost no loss of resolution. The combination of a solid-phase extraction and PDDAC-mediated CE can efficiently improve the sensitivity of the phenothiazine enantiomers. Under optimal conditions, calibration graphs displayed the linear range between 6 and 1500 nM, with relative standard deviation values lower than 3.5% (n = 5). Detection limit ranged from 2.1 to 6.3 nM for target analytes, and 607- to 1555-fold enhancement was achieved. The practicality of using the proposed method to determine five pairs of d,l-phenothiazines in urine is also validated, in which recoveries between recoveries of all phenothiazines from urine ranged from 89% to 101%.
Asunto(s)
Electroforesis Capilar/métodos , Fenotiazinas/química , Fenotiazinas/aislamiento & purificación , Extracción en Fase Sólida/métodos , Límite de Detección , Polímeros/química , Extracción en Fase Sólida/instrumentación , Estereoisomerismo , gamma-Ciclodextrinas/químicaRESUMEN
A simple approach to fabricate a highly selective and sensitive dimethoate probe was developed based on Rhodamine B (RB)-functionalized gold nanoparticles (AuNPs). The quenching of RB fluorescence in the presence of AuNPs in the solution, mediated by fluorescence resonance energy transfer, was observed. In the presence of dimethoate, the fluorescence intensity of the RB-AuNP solution is gradually recovered when dimethoate molecules displace RB molecules on the surface of the AuNPs, which significantly increased the fluorescence intensity of RB. Fluorescence is proportional to the dimethoate concentration in the range of 0.005-1.0â¯ppm (R2â¯=â¯0.989), and the LOD was 0.004â¯ppm. The recoveries of dimethoate in water and fruit samples were 86-116% with a good RSD (<â¯9.3%). Because of its high sensitivity, excellent selectivity, and convenient fabrication process, this method is a promising candidate for dimethoate screening.
Asunto(s)
Dimetoato/análisis , Transferencia Resonante de Energía de Fluorescencia/métodos , Colorantes Fluorescentes/química , Nanopartículas del Metal/química , Contaminación de Alimentos/análisis , Oro/química , Límite de Detección , Rodaminas/química , Sensibilidad y Especificidad , Agua/química , Contaminantes Químicos del Agua/análisisRESUMEN
In the proposed study, an efficient method for a carbon dot@ß-cyclodextrin (C-dot@ß-CD)-based fluorescent probe was developed for the analyses of catechol (CC) and hydroquinone (HQ) at trace levels in water samples. The properties of C-dot@ß-CD nanocomposites were characterized by Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). The sensing behaviors of C-dot@ß-CD toward CC and HQ were investigated by fluorescence spectroscopy. Based on the host-guest chemistry between C-dot@ß-CD and phenolic compounds, which can quench C-dot@ß-CD fluorescence, the prepared C-dot@ß-CD nanocomposites could be used for the sensitive and selective detection of CC or HQ across a wide linear range (0.1 to 10 µM) with detection limits of 47.9 and 20.2 nM, respectively. These results showed that the synthesized C-dot@ß-CD nanocomposite exhibited strong fluorescence and high degree of water solubility and thus, it is suitable for use as a nanoprobe for detecting CC or HQ in real water samples.
RESUMEN
Carbon quantum dots (CQDs) have attracted enormous interest in recent years owing to their low cytotoxicity, excellent biocompatibility and strong fluorescence. They have been successfully employed in sensor, bio-imaging, and drug carrier applications. A complete understanding of their core-surface structure is essential for tuning their physical and chemical properties for various applications. Conventional characterizations of CQDs are conducted with electron microscopy or spectroscopy, such as transmission electron microscopy, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy and Raman spectroscopy. However, these techniques cannot fully resolve the core-surface structure of CQDs. In this study, we attempt to analyze the structures of CQDs by laser desorption/ionization mass spectrometry (LDI-MS) using three model CQDs synthesized from citric acid (CA-CQDs), diammonium citrate (AC-CQDs) and spermidine trihydrochloride (Spd-CQDs). Both CA-CQDs and AC-CQDs produced anionic carbon cluster ions ([Cn]-, n = 4-9) during the laser desorption/ionization process. Additionally, AC-CQDs produced fragments containing C, N, and O that appeared at m/z values of 41.999, 91.015, and 107.008, which were identified by 15N isotopes as [CNO]-, [CH3N2O3]-, and [CH3N2O4]-, respectively. By contrast, subjecting Spd-CQDs to the same analysis did not yield carbon cluster ions ([Cn]-); instead, strong chlorine-associated ions with a unique isotopic pattern were observed, strongly implying that Spd-CQDs contain chlorine. The lack of carbon cluster ion formation in nitrogen- and chlorine-doped Spd-CQDs indicates that nitrogen and chlorine are abundantly and homogenously doped in the CQDs. We also found a shot-dependent fragmentation behavior for AC-CQDs that produces nitrogen- and oxygen-containing ions and carbon cluster ions ([Cn]-) during initial fragmentation of the surface, with a gradual destruction of the nanocrystalline carbon core after additional shots. These results suggest that LDI-MS can be used as a tool for analyzing the core-surface structure of CQDs, particularly when it contains a heteroatom doped carbon core with various surface functional groups containing nitrogen, oxygen and halogens.
RESUMEN
A novel method for the detection of dimethoate based on the peroxidase-like activity of silver-nanoparticles-modified oxidized multiwalled carbon nanotubes (AgNPs/oxMWCNTs) has been developed. The synthesized AgNPs/oxMWCNTs showed excellent peroxidease-like catalytic activity in hydrogen peroxide-Amplex red (AR) system (AR is oxidized to resorufinat, with the resorufin fluorescence at 584nm being used to monitor the catalytic activity). After dimethoate was added to AgNPs/oxMWCNTs, the interaction between dimethoate and the AgNPs inhibited the catalytic activity of AgNPs/oxMWCNTs. The decrease in fluorescence was used for the detection of dimethoate in the range of 0.01-0.35µgmL-1 (R2=0.998) with a detection limit of 0.003µgmL-1 (signal/noise=3). This method exhibited good selectivity for the detection of dimethoate even in the presence of high concentration of other pesticides. Consequently, the method was applied to measure the concentration of dimethoate residue in lake water and fruit, thus obtaining satisfactory results.
Asunto(s)
Dimetoato/análisis , Nanopartículas del Metal/química , Nanotubos de Carbono/química , Plata/química , Fluorometría , Análisis de los Alimentos , Frutas/química , Peróxido de Hidrógeno/metabolismo , Lagos/química , Límite de Detección , Plaguicidas/análisisRESUMEN
A turn-off fluorescence sensor synthesized by combining copper (II) oxide and multiwall carbon nanotubes (MWCNTs) were used for measuring glyphosate based on the inhibiting the catalytic activity of the CuO/MWCNTs. This sensor was synthesized by precipitating copper ions onto the acidic MWCNTs under basic conditions; the resulting material was characterized by the transmission electron microscopy, X-ray photoelectron spectroscopy, and Fourier transform infrared spectroscopy to confirm its structure. The CuO/MWCNTs nanomaterial was found to exhibit high peroxidase-like catalytic activity toward the reduction of H2O2 to H2O and the oxidation of Amplex Red to resorufin, with a corresponding color change from pink to red and the fluorescence enhancement. However, this activity was inhibited and the fluorescence diminished when glyphosate was added to the system. Using this strategy, we applied this sensor to detect glyphosate. The results indicated that this sensor is not only highly sensitive, with a detection limit of 0.67 ppb and a linear range from 0.002 to 0.01ppm, but also exhibits good selectivity for glyphosate. When this sensor was assessed for detecting glyphosate in real water samples, recoveries of 96-107% were attained. This proposed material and method are a promising approach for rapid screening of glyphosate.
Asunto(s)
Cobre/química , Glicina/análogos & derivados , Herbicidas/análisis , Nanotubos de Carbono/química , Contaminantes Químicos del Agua/análisis , Catálisis , Agua Potable/análisis , Técnicas Electroquímicas , Fluorometría , Glicina/análisis , Glicina/química , Herbicidas/química , Peróxido de Hidrógeno/química , Lagos/química , Límite de Detección , Microscopía Electrónica de Transmisión , Nanotubos de Carbono/ultraestructura , Oxidación-Reducción , Espectroscopía de Fotoelectrones , Espectroscopía Infrarroja por Transformada de Fourier , Contaminantes Químicos del Agua/química , GlifosatoRESUMEN
Dispersive liquid-liquid microextraction was combined with acetonitrile stacking in capillary electrophoresis for the identification of three selective serotonin reuptake inhibitors (citalopram, fluoxetine, and fluvoxamine) in human fluids such as urine and plasma. Parameters that affect the extraction and stacking efficiency, such as the type and volume of the extraction and disperser solvent, extraction time, salt addition for dispersive liquid-liquid microextraction, and sample matrices, pH, and concentration of the separation buffer for stacking, were investigated and optimized. Under optimum conditions, the enrichment factors were in the range of 1195-1441. Limits of detection ranged from 1.4 to 1.7 nM for the target analytes. Calibration graphs displayed satisfied linearity with R2 greater than or equal to 0.9978, and relative standard deviations of the peak area analysis were in the range of 2.9-5.0% (n = 3). The recoveries of all tricyclic antidepressant drugs from urine and plasma were in the range of 77-117 and 79-106%, respectively. The findings of this study show that dispersive liquid-liquid microextraction acetonitrile-stacking capillary electrophoresis is a rapid and convenient method for identifying tricyclic antidepressant drugs in urine and plasma.