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A core-shell-derived structural magnetic zeolite imidazolate framework-67 (Fe3O4-COOH@ZIF-67) nanocomposite was fabricated through a single-step coating of zeolite imidazolate framework-67 on glutaric anhydride-functionalized Fe3O4 nanosphere for the magnetic solid-phase extraction (MSPE) of theophylline (TP). The Fe3O4-COOH@ZIF-67 nanocomposite was characterized through scanning electron microscopy, transmission electron microscopy, energy dispersive X-ray spectrometry, Fourier transform infrared spectroscopy, Zeta potential analysis, X-ray diffraction, Brunauer-Emmett-Teller, and vibrating sample magnetometer. The material has a high specific surface area and good magnetism, which maintains the regular dodecahedron structure of ZIF-67 without being destroyed by the addition of Fe3O4-COOH nanospheres. The Fe3O4-COOH@ZIF-67 can rapidly adsorb TP mainly through the strong coordination interaction between undercoordinated Co2+ on ZIF-67 and -NH from imidazole of TP. The adsorption and desorption conditions, such as the amount of adsorbent, adsorption time, pH value, and elution solvent, were optimized. The kinetics of TP adsorption on Fe3O4-COOH@ZIF-67 was found to follow pseudo-second-order kinetics. The Langmuir model fits the adsorption data well and the maximum adsorption capacity is 1764 mg/g. Finally, the developed MSPE-HPLC method was applied in the enrichment and analysis of TP in four tea samples and rabbit plasma. TP was not detected in oolong tea and rabbit plasma, and its contents in jasmine tea, black tea, and green tea are 5.80, 4.31, and 1.53 µg/g, respectively. The recoveries of spiked samples are between 74.41% and 86.07% with RSD in the range of 0.81-3.83%. The adsorption performance of Fe3O4-COOH@ZIF-67 nanocomposite was nearly unchanged after being stored at room temperature for at least 80 days and two consecutive adsorption-desorption cycles. The results demonstrate that Fe3O4-COOH@ZIF-67 nanocomposite is a promising magnetic adsorbent for the preconcentration of TP in complex samples.
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A simple and time-saving colorimetric method was developed to quantify sulfonamides (SAAs) in milk via inhibition of the human carbonic anhydrase II (hCAII)-like activity of ZIF-8 that can hydrolyze p-nitrophenyl acetate (pNPA) to p-nitrophenol (pNP), following the color change from yellow to colorless. Effects of different reaction conditions, including pH, temperature, amount of ZIF-8, and incubation time, were investigated. The value of Michaelis-Menten constant (Km) is measured to be 0.15 mM, which exhibits high affinity to pNPA. The IC50 (0.17, 0.24, and 0.60 mM) and inhibition constant (Ki) (0.09, 0.13, and 0.33 mM) of sulfamethazine (SD), sulfadimethoxine (SDM), and sulfathiazole (ST) on ZIF-8 were measured, respectively. Moreover, the activity of ZIF-8 remains more than 90.0% of its initial activity after 30 days' storage. The colorimetric method for SD, SDM, and ST determination was established at the linear ranges of 6.3-750.0 µM (1.75-208.75 mg/kg), 6.3-750.0 µM (1.96-232.75 mg/kg), and 5.0-1250.0 µM (1.28-319.15 mg/kg) with limit of detection of 4.3, 3.2, and 3.9 µΜ (1.2, 0.99, and 0.96 mg/kg), respectively. In addition, the spiked recoveries of SAAs in milk sample are in the range of 81.6%-106.7% with RSD less than 6.5%. In short, the developed colorimetric method can achieve rapid analysis of SAAs in milk with simple operations.
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Colorimetria , Leite , Animais , Anidrase Carbônica II , Colorimetria/métodos , Leite/química , Sulfadimetoxina/análise , Sulfonamidas/análiseRESUMO
In this work, a magnetic octahedral metal-organic framework (Fe3 O4 @NH2 -MIL-101(Fe)) was synthesized for the magnetic solid-phase extraction of three anthraquinones, including aloe-emodin, emodin, and physcion, in rhubarb. The Fe3 O4 @NH2 -MIL-101(Fe) exhibits a high specific surface area of 259.2 m2 /g with an average pore size of 6.0 nm and high magnetic responsivity of 23.4 emu/g, which may be used as an adsorbent for rapid preconcentration and separation of target analytes. The main parameters for magnetic solid-phase extraction of anthraquinones, including the amount of adsorbent, extraction time, extraction temperature, extraction pH, elution solvent, and elution time, were systematically optimized. The whole extraction process requires a very low amount of adsorbent and a small volume of the sample. Besides, under the optimized conditions, the method shows satisfactory spiked recovery for anthraquinones in the range of 93.3-109.1% and the limits of detection are 1.7-3.4 ng/mL. The relative standard deviations for intra- and inter-day precision are 0.2-1.3% and 0.2-0.6%, respectively. The experimental results indicate that the developed method is feasible for the analysis of anthraquinones in rhubarb.
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Emodina , Estruturas Metalorgânicas , Rheum , Antraquinonas/análise , Cromatografia Líquida de Alta Pressão/métodos , Fenômenos Magnéticos , Extração em Fase Sólida/métodosRESUMO
In this study, 3,3',5,5'-tetramethylbenzidine (TMB) was selected as a chromogenic substrate to evaluate the light-responsive oxidase-like activity of different zeolitic imidazolate frameworks (ZIFs). The synthesized ZIFs were systematically characterized by scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, and X-ray diffraction analysis. Several main operational parameters, including ZIFs and TMB concentrations, pH value, radiation time, and working current, in the reaction process were optimized. The kinetic measurement results show that ZIF-90 exhibits higher affinity to the substrate than horseradish peroxidase. Furthermore, given that adenosine triphosphate (ATP) can specifically combine with Zn2+ binding site and destroy the structure of ZIF-90, a specific and sensitive colorimetric method was established for the quantitative detection of ATP within the range 10 - 240 µM. In addition, on the basis that phenolic pollutants can impact the reaction kinetics diversely on different ZIFs, a sensor array was constructed and successfully applied to differentiate five phenolic pollutants in lake water samples. This work is expected to shed light on the establishment of ZIF-based light-responsive oxidase-like nanozymes for the highly selective colorimetric detection and sensor array.
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Poluentes Ambientais , Zeolitas , Zeolitas/química , Trifosfato de Adenosina , OxirredutasesRESUMO
In this study, a simple colorimetric method was established to detect copper ion (Cu2+), sulfathiazole (ST), and glucose based on the acetylcholinesterase (AChE)-like activity of zeolitic imidazolate framework-8 (ZIF-8). The AChE-like activity of ZIF-8 can hydrolyze acetylthiocholine chloride (ATCh) to thiocholine (TCh), which will further react with 5,5'-dithiobis (2-nitrobenzoic acid) (DTNB) to generate 2-nitro-5-thiobenzoic acid (TNB) that has a maximum absorption peak at 405 nm. The effects of different reaction conditions (buffer pH, the volume of ZIF-8, reaction temperature and time, and ATCh concentration) were investigated. Under the optimized conditions, the value of the Michaelis-Menten constant (Km) is measured to be 0.83 mM, which shows a high affinity toward the substrate (ATCh). Meanwhile, the ZIF-8 has good storage stability, which can maintain more than 80.0% of its initial activity after 30 days of storage at room temperature, and the relative standard deviation (RSD) of batch-to-batch (n = 3) is 5.1%. The linear dependences are obtained based on the AChE-like activity of ZIF-8 for the detection of Cu2+, ST, and glucose in the ranges of 0.021-1.34 and 5.38-689.66 µM, 43.10-517.24 µM, and 0.0054-1.40 mM, respectively. The limit of detections (LODs) are calculated to be 20.00 nM, 9.25 µM, and 5.24 µM, respectively. Moreover, the sample spiked recoveries of Cu2+ in lake water, ST in milk, and glucose in strawberry samples were measured, and the results are in the range of 98.4-115.4% with the RSD (n = 3) lower than 3.3%. In addition, the method shows high selectivity in the real sample analysis.
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Acetilcolinesterase , Zeolitas , Colorimetria , Acetiltiocolina , GlucoseRESUMO
Profiling of lipid-water partition coefficients (KL/W ) of drugs is an essential issue during the early stage of drug development. In this study, two liposomes, including 1,2-distearoyl-sn-glycero-3-phosphocholine (DSPC) + cholesterol (Chol) (DSPC/Chol liposomes) and soybean lecithin (SPC) + Chol (SPC/Chol liposomes), were prepared for the liposome electrokinetic chromatography (LEKC) analysis, and the logarithm of lipid-water partition coefficients (log KL/W ) of neutral and ionic drugs were determined based on an iterative method. The log KL/W values determined by the SPC/Chol or DSPC/Chol liposomes LEKC were linearly fitted, which showed a good fitting coefficient (R2 = 0.89). Furthermore, the linear relationship between the data obtained from LEKC system and octanol-water system, immobilized artificial membrane, Caco-2 cell model, and software prediction was analyzed, respectively. Results illustrated that DSPC/Chol liposomes or SPC/Chol liposomes had a good linear relationship with Caco-2 cell model, and R2 was 0.81 and 0.72, respectively. Moreover, the linear free energy relationship analysis suggested that the solute volume, hydrogen bond basicity, and J- were the main descriptors that drove the partition process of solutes in the SPC/Chol or DSPC/Chol LEKC system. In addition, the normalized properties of the SPC/Chol and DSPC/Chol LEKC systems through linear free energy relationship analysis were very close. In short, DSPC/Chol liposomes are more suitable for simulating cell membranes than SPC/Chol liposomes, and the developed LEKC is an effective partitioning model for measuring the log KL/W of drugs.
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Cromatografia , Células CACO-2 , Colesterol , Humanos , Íons , Cinética , Lipossomos , Membranas Artificiais , Soluções , ÁguaRESUMO
In this study, a magnetic yolk-shell structured metal-organic framework material (Fe3O4@YS-UiO-66-NH2) is prepared by the directional etching of Co2+/peroxymonosulfate and in situ magnetization. The characteristic properties of the material were investigated by using field emission scanning electron microscopy, transmission electron microscopy, energy-dispersive X-ray spectroscopy, X-ray powder diffraction, Fourier transform infrared spectroscopy, vibrating sample magnetometer, Brunauer-Emmett-Teller, and contact angle test. The Fe3O4@YS-UiO-66-NH2 shows the advantages of large surface area, good magnetic property, and satisfactory stability, as well as giving high affinity to alkaloids (ALs) via hydrophilic interaction, hydrogen bonding, and π-π interaction. The results of static adsorption experiment indicate that the Fe3O4@YS-UiO-66-NH2 possesses high adsorption capacity towards ALs and the adsorption behaviors are fitted with Langmuir adsorption isotherm model. Furthermore, a magnetic solid-phase extraction using Fe3O4@YS-UiO-66-NH2 and HPLC method was developed for the analysis of ALs in spiked samples with the recovery of 89.6-100.8%. In addition, the proposed method was successfully applied in the pharmacokinetics study of berberine, coptisine, and palmatine in the rat. In short, the developed method might be used for high-efficient recognition and determination of ALs in plasma sample, which would also provide a new way to fabricate magnetic functionalized metal-organic framework in separation science.
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Alcaloides/farmacocinética , Magnetismo , Estruturas Metalorgânicas/química , Alcaloides/sangue , Animais , Feminino , Limite de Detecção , Masculino , Microscopia Eletrônica de Varredura/métodos , Microscopia Eletrônica de Transmissão/métodos , Ratos , Ratos Sprague-Dawley , Reprodutibilidade dos Testes , Análise Espectral/métodos , Zircônio/químicaRESUMO
In this study, a zirconium terephthalate metal-organic framework-coated magnetic nanoparticle (UiO-66@PA@PEI@Fe3 O4 ) was synthesized for the extraction of berberine prior to high-performance liquid chromatography analysis. The phytic acid, which could be grafted onto the magnetic nanoparticle through electrostatic interaction with the abundant amino groups of polyethylenimine, possesses outstanding metal ion coordination ability for the immobilization of metal-organic frameworks UiO-66. The physicochemical properties of the obtained nanoparticle were thoroughly investigated by a series of characterization techniques. Then, the factors that will affect the extraction efficiency and recovery of berberine were investigated. Results indicated that the material had good stability and reusability, and high adsorption capacity (50.01 mg/g) to berberine through single-layer adsorption. In addition, a molecular docking study indicated that the interactions between the material and berberine were mainly π-π stacking and hydrophobic interaction. Finally, the material was successfully applied to the extraction of berberine in Rhizoma Coptidis and Cortex Phellodendri extracts with the recoveries of 76.1% and 71.6%, respectively.
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Yolk-shell structure magnetic metal-organic framework nanoparticles were prepared via post solvothermal method and employed as a magnetic solid-phase extraction adsorbent for selective pre-concentration of 5'-ribonucleotides by π stacking interaction, hydrogen bonding, and the strong interaction between titanium ions (Ti4+) and phosphate group. The properties of the materials were confirmed by scanning electron microscopy, transmission electron microscopy, X-ray diffraction, X-ray photoelectron spectrometry, vibrating sample magnetometer, infrared spectroscopy, thermogravimetric analysis, and Brunauer-Emmett-Teller analysis. The main parameters affecting the adsorption-desorption process, including adsorbent amount, incubation time, incubation temperature, sample pH, shaking speed, elution solution, and elution time, were systematically optimized. Finally, 1.0 mg of adsorbent mixed with 1.0 mL sample solution (10.0 mmolâ L-1 NaCl, pH 3.0) and shaken at 135 rpm for 5 min at 40 °C, washed with 1.0 mL Na3PO4-NH3âH2O under vortex for 5 min were selected as optimized adsorption-desorption conditions. The binding performance of adsorbent towards five nucleotides was evaluated by static adsorption experiments. The data are well-fitted to the Langmuir isotherm model and the maximum adsorption capacity is 27.8 mg g-1 for adenosine 5'-monophosphate. The limit of detection of the method is 19.44-38.41 ng mL-1. Under the optimal conditions, the adsorbent was successfully applied to magnetic solid-phase extraction and high performance liquid chromatography determination of five nucleotides in octopus, chicken, fish, and pork samples.
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Cromatografia Líquida de Alta Pressão/métodos , Dietilamida do Ácido Lisérgico/análogos & derivados , Nanopartículas de Magnetita/química , Estruturas Metalorgânicas/química , Nucleotídeos/química , Dietilamida do Ácido Lisérgico/químicaRESUMO
In this study; a spectrum-effect relationship analysis combined with a high-performance liquid chromatography-mass spectrometry (LC-MS) analysis was established to screen and identify active components that can inhibit thrombin and factor Xa (THR and FXa) in Salviae Miltiorrhizae Radix et Rhizoma-Chuanxiong Rhizoma (Danshen-Chuanxiong) herbal pair. Ten potential active compounds were predicted through a canonical correlation analysis (CCA), and eight of them were tentatively identified through an LC-MS analysis. Furthermore; the enzyme inhibitory activity of six available compounds; chlorogenic acid; Z-ligustilide; caffeic acid; ferulic acid; tanshinone I and tanshinone IIA; were tested to verify the feasibility of the method. Among them; chlorogenic acid was validated to possess a good THR inhibitory activity with IC50 of 185.08 µM. Tanshinone I and tanshinone IIA are potential FXa inhibitors with IC50 of 112.59 µM and 138.19 µM; respectively. Meanwhile; molecular docking results show that tanshinone I and tanshinone IIA; which both have binding energies of less than -7.0 kcal·mol-1; can interact with FXa by forming H-bonds with residues of SER214; GLY219 and GLN192. In short; the THR and FXa inhibitors in the Danshen-Chuanxiong herbal pair have been successfully characterized through a spectrum-effect relationship analysis and an LC-MS analysis.
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Antitrombinas/farmacologia , Medicamentos de Ervas Chinesas/farmacologia , Inibidores do Fator Xa/farmacologia , Trombina/antagonistas & inibidores , Antitrombinas/química , Avaliação Pré-Clínica de Medicamentos , Medicamentos de Ervas Chinesas/química , Inibidores do Fator Xa/química , Humanos , Simulação de Acoplamento Molecular , Salvia miltiorrhiza/químicaRESUMO
Capillary electrochromatography, which combined the high selectivity of high-performance liquid chromatography and the high separation efficiency of capillary electrophoresis, is an attractive separation tool. In this review, the developments on monolithic and open tubular capillary electrochromatography during 2017 to August 2019 are summarized. Considering the development of novel stationary phases is the most active research field in capillary electrochromatography, monolithic capillary electrochromatography is classified according to the polymer-based and hybrid monolithic columns, while open-tubular capillary electrochromatography is categorized by cyclodextrin, silica, polymer, nanomaterials, microporous materials, and biomaterials-based open tubular columns.
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A core-shell structure UiO-66-(OH)2@UiO-66-NH2 (MOF@MOF) nanoparticle was synthesized through a simple hydrothermal method and employed as an adsorbent and laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) matrix for the quantitative analysis of rhubarb anthraquinones (RAs). The properties of the materials were characterized by ï¬eld emission scanning electron microscopy, transmission electron microscopy, energy-dispersive X-ray spectroscopy, X-ray powder diffraction, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, thermogravimetric analysis, and Brunauer-Emmett-Teller. The results indicate that MOF@MOF is regular octahedral structure with a size distribution of about 100 nm, having large BET specific surface area (920 m2/g). Using the MOF@MOF as a matrix shows lower background interference, higher sensitivity, and better storage stability than that of traditional matrices. The MOF@MOF matrix exhibits excellent salt tolerance even under a NaCl concentration of 150 mM. Then, the enrichment conditions were optimized, and the adsorption time of 10 min, adsorption temperature of 40 °C and adsorbent amount of 100 µg were selected. In addition, the possible mechanism of MOF@MOF as an adsorbent and matrix was discussed. Finally, the MOF@MOF nanoparticle was employed as a matrix for the sensitive MALDI-TOF-MS analysis of RAs in spiked rabbit plasma, and the recoveries are in the range of 88.3-101.5% with RSD ≤9.9%. In short, the novel MOF@MOF matrix has demonstrated its potential in the analysis of small-molecule compounds in biological samples.
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Two liposomes, including 1,2-distearoyl-sn-glycero-3-phosphocholine (DSPC) + 1,2-dimyristoyl-sn-glycero-3-phosphoethanolamine (PE) + cholesterol (Chol) (DSPC/PE/Chol liposomes) and soybean lecithin (SPC) + PE + Chol (SPC/PE/Chol liposomes), were prepared and fixed on the inner wall of capillary column by using the adhesion of polydopamine (PDA) membrane and the cross-linking property of glutaraldehyde (GA). The immobilized liposome capillary column (ILCC) has good repeatability and stability based on the electrophoretic mobility of analyte. A CE method based on the immobilized liposome capillary column chromatography (ILCCC) was successfully developed to study the retention behavior of drugs on ILCC, and the logarithm of retention factor (log k) of neutral and ionic drugs were determined. The results show that the log k measured by the ILCCC based on two liposomes have a good linear fitting (R2 = 0.86). Moreover, the linear relationship between ILCCC system and other related research systems (octanol-water system and immobilized artificial membrane (IAM)) was analyzed, and the results indicate that SPC/PE/Chol ILCCC, DSPC/PE/Chol ILCCC and IAM systems have good fitting results, R2 values are 0.86 and 0.78, respectively. In addition, the normalization coefficients of ILCCC and IAM systems obtained by the linear free energy relationship (LFER) analysis are close and the d value is small. In short, the ILCCC is a simple and feasible method for studying drug membrane permeability.
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Lipossomos , Fosfatidiletanolaminas , Permeabilidade da Membrana Celular , Colesterol , PermeabilidadeRESUMO
A novel MOF@HOF composite that can serve as a matrix for analysis of small molecules by MALDI-TOF-MS was fabricated through a simple solvothermal method. Taking falvonoids as an example, this composite/matrix presents high desorption/ionization efficiency, low background interference, high salt tolerance, and satisfactory signal reproducibility for MALDI-TOF-MS analysis.
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Estruturas Metalorgânicas , Hidrogênio , Reprodutibilidade dos Testes , Espectrometria de Massas por Ionização e Dessorção a Laser Assistida por Matriz/métodosRESUMO
In this study, the alkaline phosphatase (ALP)-like activity of zeolitic-imidazolate framework-8 (ZIF-8) is reported for the first time. Then, colorimetric sensors for the ascorbic acid oxidase (AAO) and copper ion (Cu2+) detection were developed based on the acetylcholinesterase (AChE)- and ALP-like activities of ZIF-8. The ZIF-8 has good mimetic enzyme activity and exhibits high affinity to the substrates. Its AChE- and ALP-like activities also have good reusability and storage stability. Good linear dependences are obtained in the range of 1.3-250.0 µM (AChE-like activity-based) and 4.5-454.5 µM (ALP-like activity based) for Cu2+ detection. Furthermore, good linear dependence is also obtained based on the ALP-like activity of ZIF-8 for AAO detection in the range of 2.3-454.5 U/L. Their limits of detection (LODs) are calculated to be 0.7 µM, 2.8 µM, and 1.8 U/L, respectively. Finally, the sample spiked recoveries of Cu2+ in tap water, Cu2+, and AAO in human serum and rabbit plasma were measured, and the results are in the range of 80.0-119.3%. In short, the preparation of ZIF-8 is simple, environmentally friendly, and harmless, and can realize highly selective detection of AAO and Cu2+ in an efficient and fast process.
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Nanoporos , Zeolitas , Animais , Humanos , Coelhos , Fosfatase Alcalina , Cobre , Acetilcolinesterase , Oxirredutases , Ácido Ascórbico , ÍonsRESUMO
An innovative sandwich-structural Fe-based metal-organic framework magnetic material (Fe3O4@SW-MIL-101-NH2) was fabricated using a facile solvothermal method. The characteristic properties of the material were investigated by ï¬eld emission scanning electron microscopy, transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy, X-ray powder diffraction, vibrating sample magnetometry, and Brunauer-Emmett-Teller measurements. Fe3O4@SW-MIL-101-NH2 is associated with advantages, such as robust magnetic properties, high specific surface area, and satisfactory storage stability, as well as good selective recognition ability for chlorogenic acid (CA) and its metabolites via chelation, hydrogen bonding, and π-interaction. The results of the static adsorption experiment indicated that Fe3O4@SW-MIL-101-NH2 possessed a high adsorption capacity toward CA and its isomers, cryptochlorogenic acid (CCA) and neochlorogenic acid (NCA), and the adsorption behaviors were fitted using the Langmuir adsorption isotherm model. Then, a strategy using magnetic solid-phase extraction (MSPE) and ultra-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (UPLC-Q-TOF MS/MS) was developed and successfully employed for the selective pre-concentration and rapid identiï¬cation of CA metabolites in rat plasma, urine, and feces samples. This work presents a prospective strategy for the synthesis of magnetic adsorbents and the high-efficiency pretreatment of CA metabolites.
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In this study, a highly sensitive visual colorimetric sensor was designed for the detection of trichlorfon based on inhibiting ascorbate oxidase (AAO)-induced metallization of gold nanorods (Au NRs). Ascorbic acid (AA) can reduce silver ion (Ag+) to metal silver (Ag) that will be deposited on the surface of Au NRs, which results in the blue shift of longitudinal localized surface plasmon resonance (LSPR) peak of Au NRs, accompanying by perceptible color changes from red to cyan to red to yellow. In the presence of trichlorfon, the activity of AAO will be inhibited, resulting in less AA is hydrolyzed to dehydroascorbic acid (DHA), and therefore more Ag+ is reduced to Ag by AA. Under the optimized conditions, detection of trichlorfon has a wide linear range of 27.8-11111.1 µg/L with a limit of detection as low as 132.6 ng/L. Moreover, the sensor has a good sample spiked recovery (84.7-96.8%) for the determination of trichlorfon in lake water samples. The proposed method can achieve rapid analysis (about 10 min) of trichlorfon with simple operation when there are no other types of organophosphorus pesticides in the real samples.
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Nanopartículas Metálicas , Nanotubos , Praguicidas , Colorimetria , Ouro , Limite de Detecção , Compostos Organofosforados , TriclorfonRESUMO
Sample preparation such as isolation and pre-concentration is a crucial step for the phytochemical analysis. Magnetic solid-phase extraction (MSPE) has received considerable attention, mainly due to its phase separation more conveniently by facile magnetic decantation as compared to traditional SPE. This review focused on the recent applications of MSPE in sample preparation for the analysis of phytochemical compounds in plants, biological samples and Chinese herbal preparations. In addition, the enzymes immobilized on the magnetic materials and used for the biospecific extraction of enzyme inhibitors were also discussed. The information summarized in this article may provide a reference to the further applications of MSPE in phytochemical analysis.
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Magnetismo , Extração em Fase Sólida , Fenômenos Magnéticos , Compostos FitoquímicosRESUMO
In this study, a method based on adsorbed hollow fiber immobilized tyrosinase (TYR) was developed to screening potential TYR inhibitors from Pueraria lobate extract. Kojic acid and ranitidine were used as positive and negative control to verify the reliability of the proposed method, respectively. Several significant parameters of the screening process, including the amount of P. lobata extract, adsorption time and incubation time, were optimized. After investigating the repeatability of the developed method, seven potential active compounds in P. lobata extract were successfully detected and their chemical structures were tentatively identified by liquid chromatography - mass spectrometry analysis. Furthermore, the inhibitory activity of four identified compounds on TYR was tested in vitro, and three of them, namely, puerarin, puerarin-6â³-O-xyloside and puerarin apioside were verified to have good TYR inhibitory activity with IC50 value of 478.5, 513.8, and 877.3 µM, respectively. In addition, the molecular docking results indicated that these compounds could bind to the amino acid residues in TYR catalytic pocket. These results proved that the proposed method is a feasible approach for screening of TYR inhibitors from plant extract.
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Isoflavonas , Pueraria , Inibidores Enzimáticos/farmacologia , Simulação de Acoplamento Molecular , Monofenol Mono-Oxigenase , Extratos Vegetais/farmacologia , Reprodutibilidade dos TestesRESUMO
BACKGROUND: Salvia miltiorrhiza (Danshen, DS) and Panax notoginseng (Sanqi, SQ) are famous traditional Chinese herbs, and their herbal pair (DS-SQ) has been popular used as anti-thrombotic medicines. However, there is still a lack of sufficient scientific evidence to illustrate the optimum combination ratio of these two herbs as well as its action mechanisms. The purpose of this study is to investigate the anti-thrombotic effects of DS-SQ on zebrafish and explore its possible action mechanism. METHODS: Firstly, the chemical components in DS-SQ extract were analyzed by LC-ESI-MS/MS. Then, a phenylhydrazine (PHZ)-induced zebrafish thrombosis model was developed for evaluating the anti-thrombotic effects of DS-SQ extracts with different combination ratios and their nine pure compounds. Followed, Real-time quantitative PCR (RT-qPCR) assays were performed to investigate the potential antithrombotic mechanisms of DS-SQ. RESULTS: Thirty-three components were tentatively identified by LC-MS analysis. DS-SQ at the ratio of 10:1 presented the best anti-thrombotic effect, and rosmarinic acid, lithospermic acid and salvianolic acid B of DS showed good anti-thrombotic activity on zebrafish thrombosis model. The RT-qPCR assays indicated that DS-SQ (10:1) could cure the PHZ-induced thrombosis by downregulating the expression of PKCα, PKCß, fga, fgb, fgg and vWF in zebrafish. CONCLUSIONS: DS-SQ with the combination ratio of 10:1 showed optimum anti-thrombotic effect on PHZ-induced zebrafish thrombosis model, which provided a reference for reasonable clinical applications of DS-SQ herbal pair.