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1.
J Sep Sci ; 46(16): e2300129, 2023 Aug.
Artículo en Inglés | MEDLINE | ID: mdl-37339788

RESUMEN

As a main source for the recognition and identification of lead compounds, traditional Chinese medicine plays a pivotal role in preventing diseases for years. However, screening bioactive compounds from traditional Chinese medicine remains challenging because of the complexity of the systems and the occurrence of the synergic effect of the compounds. The infructescence of Platycarya strobilacea Sieb. et Zucc is prescribed for allergic rhinitis treatment with unknown bioactive compounds and unclear mechanisms. Herein, we immobilized the ß2 -adrenoceptor and muscarine-3 acetylcholine receptor onto the silica gel surface to prepare the stationary phase in a covalent bond through one step. The feasibility of the columns was investigated by the chromatographic method. Ellagic acid and catechin were identified as the bioactive compounds targeting the receptors. The binding constants of ellagic acid were calculated to be (1.56 ± 0.23)×107  M-1 for muscarine-3 acetylcholine receptor and (2.93 ± 0.15)×107  M-1 for ß2 -adrenoceptor by frontal analysis. While catechin can bind with muscarine-3 acetylcholine receptor with an affinity of (3.21 ± 0.05)×105  M-1 . Hydrogen bonds and van der Waals' force were the main driving forces for the two compounds with the receptors. The established method provides an alternative for multi-target bioactive compound screening in complex matrices.


Asunto(s)
Catequina , Medicamentos Herbarios Chinos , Medicamentos Herbarios Chinos/análisis , Ácido Elágico/química , Catequina/análisis , Muscarina , Cromatografía Líquida de Alta Presión/métodos , Cromatografía de Afinidad/métodos , Receptores Colinérgicos , Colinérgicos
2.
Mikrochim Acta ; 190(5): 191, 2023 04 26.
Artículo en Inglés | MEDLINE | ID: mdl-37099040

RESUMEN

An immobilized metal affinity (IMAC) adsorbent was prepared for selective enrichment of adenine type CKs, via grafting polymer chain pendant with iminodiacetic acid (IDA) from polydopamine (PDA)/polyethyleneimine (PEI)-coated magnetic graphene oxide (magGO) via surface-initiated-atom transfer radical polymerization (SI-ATRP). The prepared IMAC sorbent exhibited remarkable adsorption performances and good selectivity for adenine-type CKs and was utilized as a sorbent of magnetic solid-phase extraction (MSPE) for effective enrichment of four adenine-type CKs in bean sprouts. Under the optimized extraction conditions, an analytical method for four adenine type CKs in bean sprouts was established by combining the MSPE combined with ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The recoveries of the analytes were between 80.4 ± 1.9% and 114.6 ± 1.5% (n = 3). The limits of detection (LODs) range from 0.63 to 2.30 pg⋅mL-1. The relative standard deviations of intra-day and inter-day were less than 12.6%. The established method was successfully applied to the selective extraction and sensitive detection of trace adenine-type CKs in plant samples.


Asunto(s)
Citocininas , Polietileneimina , Citocininas/análisis , Citocininas/química , Polietileneimina/química , Espectrometría de Masas en Tándem/métodos , Plantas , Polímeros/química , Fenómenos Magnéticos
3.
Mikrochim Acta ; 190(1): 21, 2022 12 13.
Artículo en Inglés | MEDLINE | ID: mdl-36512123

RESUMEN

N-doped carbon quantum dots (N-CDs) with polyaminobenzene hydrazine as precursor were prepared by solvothermal method for the monitoring of pH fluctuation in HeLa cells via fluorescence imaging. The N-CDs show two emission wavelengths at 582 and 640 nm under different pH with two excitation wavelengths. The fluorescence intensity at 640 nm (λex = 520 nm) and the ratio of F582/F640 (λex = 470 nm) linearly increase with pH in the range of 2.4 ~ 3.6 (R2 = 992) and 5.6 ~ 7.6 (R2 = 0.987), respectively. The sensor exhibits high sensitivity and reversibility and anti-interference capability, thus enabling sensing pH change in intracellular environment in real time, as demonstrated by successful monitoring of intracellular pH fluctuation during H2O2 stimulation in HeLa cells.


Asunto(s)
Citrus sinensis , Puntos Cuánticos , Humanos , Puntos Cuánticos/toxicidad , Carbono/toxicidad , Células HeLa , Peróxido de Hidrógeno , Concentración de Iones de Hidrógeno , Imagen Óptica
4.
J Sep Sci ; 43(14): 2766-2772, 2020 Jul.
Artículo en Inglés | MEDLINE | ID: mdl-32419326

RESUMEN

Poly(ionic liquid)-modified stationary phases can have multiple interactions with solutes. However, in most stationary phases, separation selectivity is adjusted by changing the poly(ionic liquid) anions. In this work, two poly(ionic liquid)-modified silica stationary phases were prepared by introducing the cyano or tetrazolyl group on the pendant imidazolium cation on the polymer chains. Various analytes were selected to investigate their mechanism of retention in the stationary phases using different mobile phases. Two poly(ionic liquid)-modified stationary phases can provide various interactions toward solutes. Compared to the cyano-functionalized poly(ionic liquid) stationary phase, the tetrazolyl-functionalized poly(ionic liquid) stationary phase provides additional cation-exchange and π-π interactions, resulting in different separation selectivity toward analytes. Finally, applicability of the developed stationary phases was demonstrated by the efficient separation of nonsteroidal anti-inflammatory drugs.


Asunto(s)
Antiinflamatorios no Esteroideos/análisis , Imidazoles/química , Líquidos Iónicos/química , Polímeros/química , Cationes/química , Cromatografía Líquida de Alta Presión , Líquidos Iónicos/síntesis química , Estructura Molecular , Polímeros/síntesis química
5.
J Sep Sci ; 43(15): 3110-3119, 2020 Aug.
Artículo en Inglés | MEDLINE | ID: mdl-32468707

RESUMEN

Graphene oxide has received extensive attention because of its unique properties and potential applications. In this study, magnetic nitrogen-doped graphene was prepared by one-step hydrothermal reaction using urea as the dopant and reductant, and ferroferric oxide nanoparticles were in situ deposited on the surface of the nanohybrids. The magnetic nitrogen-doped graphene was characterized using various physical and chemical methods. It was used as a new adsorbent for the magnetic solid-phase extraction of four nonsteroidal anti-inflammatory drugs from the river water. The parameters influencing the extraction efficiency were optimized in detail. Under optimal conditions, this method provided a wide linear range (5-200 ng/mL). The limits of detection were in the range of 1.07-5.10 ng/mL. The recoveries varied from 81.2 to 121.5% with relative standard deviations of less than 10.8%. Overall, we can conclude that the proposed method offers an efficient pretreatment and enrichment and can be successfully applied for the extraction and determination of nonsteroidal anti-inflammatory drugs in complex matrices.


Asunto(s)
Antiinflamatorios no Esteroideos/análisis , Grafito/química , Nitrógeno/química , Extracción en Fase Sólida , Temperatura , Contaminantes Químicos del Agua/análisis , Fenómenos Magnéticos , Estructura Molecular , Tamaño de la Partícula , Propiedades de Superficie
6.
Mikrochim Acta ; 187(8): 472, 2020 07 29.
Artículo en Inglés | MEDLINE | ID: mdl-32725323

RESUMEN

An immobilized metal affinity (IMA) adsorbent was prepared by grafting bottlebrush polymer pendant with iminodiacetic acid (IDA) from the surface of polydopamine (PDA)-coated magnetic graphene oxide (magGO), via surface-initiated atom transfer radical polymerization (SI-ATRP). Poly(hydroxyethyl methacrylate) (PHEMA) was grafted firstly from the PDA-coated magGO as the backbone, and then poly(glycidyl methacrylate) was grafted from the PHEMA chains via the second SI-ATRP to afford the bottlebrush polymer-grafted magGO Thereafter, IDA was anchored on the nanocomposites to produce the IMA adsorbent after chelating copper ions. The adsorbent was characterized by various physical and physicochemical methods. Its adsorption properties were evaluated by using histidine-rich proteins (bovine hemoglobin, BHb) and other proteins (lysozyme and cytochrome-C). The results show that its maximum adsorption capacity to BHb was 378.6 mg g-1, and the adsorption equilibrium can be quickly reached within 1 h. The adsorbent has excellent reproducibility and reusability. It has been applied to selectively purify hemoglobin from human whole blood, indicating its potential in practical applications. Graphical abstract.


Asunto(s)
Grafito/química , Hemoglobinas/aislamiento & purificación , Adsorción , Animales , Bovinos , Cobre/química , Humanos , Iminoácidos/química , Indoles/química , Extracción Líquido-Líquido/métodos , Fenómenos Magnéticos , Polihidroxietil Metacrilato/química , Polímeros/química , Ácidos Polimetacrílicos/química , Reproducibilidad de los Resultados
7.
J Sep Sci ; 42(10): 1896-1904, 2019 May.
Artículo en Inglés | MEDLINE | ID: mdl-30828963

RESUMEN

Considering that the determination of pyrethroid residues is of value for the safety of food, a new poly(ionic liquid)-functionalized magnetic mesoporous nanoparticle was designed and used as an adsorbent in magnetic solid-phase extraction for the enrichment of eight pyrethroids. The porous structure and large surface area of the mesoporous silica shell endow the adsorbent with abundant binding sites. In contrast to the reported poly(ionic liquids) with only one kind of functional group in the cationic part, the new poly(ionic liquids) with mixed cyano and phenyl groups in cationic part matched the chemical structure of the analytes to improve extraction efficiency. Under the optimum conditions, an effective method was established for the determination of eight pyrethroids in apples. Adsorption equilibrium can be quickly reached in 1 min, greatly decreasing the extraction time. The linearity range was found to be 10-200 ng/g, and the detection limits ranged from 0.24 to 1.99 ng/g. Recoveries of analytes in apple samples ranged from 87.3 to 119.0%, with relative standard deviations varying in the range of 3-21.2% (intraday) and 0.3-15.2% (interday). The results indicate that the proposed method is a good candidate for pyrethroid residues in apple samples.


Asunto(s)
Contaminación de Alimentos/análisis , Insecticidas/análisis , Líquidos Iónicos/química , Nanopartículas de Magnetita/química , Malus , Piretrinas/análisis , Adsorción , Sitios de Unión , Cationes , Inocuidad de los Alimentos , Iones , Límite de Detección , Magnetismo , Microscopía Electrónica de Rastreo , Microscopía Electrónica de Transmisión , Microesferas , Reproducibilidad de los Resultados , Dióxido de Silicio/química , Extracción en Fase Sólida , Solventes , Agua/análisis
8.
J Sep Sci ; 42(23): 3512-3520, 2019 Dec.
Artículo en Inglés | MEDLINE | ID: mdl-31556204

RESUMEN

In this work, core-shell structured magnetic mesoporous carbon nanospheres were fabricated from the carbonization of metal-polyphenol coordination polymer-coated Fe3 O4 nanoparticles. The preparation method is simple, fast, versatile, and easy to scale up. Magnetic mesoporous carbon nanospheres exhibit a high specific surface area, high superparamagnetism, and high adsorption efficiencies for phthalates. Four phthalates were extracted from aqueous solutions by using magnetic mesoporous carbon nanospheres via magnetic solid phase extraction. Subsequent analysis was performed by using high-performance liquid chromatography with ultraviolet detection. The analytical method has good linearity in the concentration range of 1-200 ng/mL for diethyl phthalate, diisobutyl phthalate, and dicyclohexyl phthalate, and 3-200 ng/mL for dipropyl phthalate. The limits of detection were in the range of 0.10-0.62 ng/mL. Compared with previous methods, this method has a lower detection limit, wider linearity range, and faster adsorption and desorption rates. The results indicate that magnetic mesoporous carbon nanospheres are suitable for the enrichment of hydrophobic substances from aqueous solutions.

9.
Small ; 14(45): e1802290, 2018 11.
Artículo en Inglés | MEDLINE | ID: mdl-30307703

RESUMEN

The rising dangers of bacterial infections have created an urgent need for the development of a new generation of antibacterial nanoagents and therapeutics. A new near-infrared 808 nm laser-mediated nitric oxide (NO)-releasing nanovehicle (MoS2 -BNN6) is reported through the simple assembly of α-cyclodextrin-modified MoS2 nanosheets with a heat-sensitive NO donor N,N'-di-sec-butyl-N,N'-dinitroso-1,4-phenylenediamine (BNN6) for the rapid and effective treatment of three typical Gram-negative and Gram-positive bacteria (ampicillin-resistant Escherichia coli, heat-resistant Escherichia faecalis, and pathogen Staphylococcus aureus). This MoS2 -BNN6 nanovehicle has good biocompatibility and can be captured by bacteria to increase opportunities of NO diffusion to the bacterial surface. Once stimulated by 808 nm laser irradiation, the MoS2 -BNN6 nanovehicle not only exhibits photothermal therapy (PTT) efficacy but also can precisely control NO release, generating oxidative/nitrosative stress. The temperature-enhanced catalytic function of MoS2 induced by 808 nm laser irradiation simultaneously accelerates the oxidation of glutathione. This acceleration disrupts the balance of antioxidants, ultimately resulting in significant DNA damage to the bacteria. Within 10 min, the MoS2 -BNN6 with enhanced PTT/NO synergetic antibacterial function achieves >97.2% inactivation of bacteria. The safe synergetic therapy strategy can also effectively repair wounds through the formation of collagen fibers and elimination of inflammation during tissue reconstruction.


Asunto(s)
Antibacterianos/química , Disulfuros/química , Molibdeno/química , Óxido Nítrico/química , Antibacterianos/farmacología , Daño del ADN/efectos de los fármacos , Escherichia coli/efectos de los fármacos , Luz , Pruebas de Sensibilidad Microbiana , Donantes de Óxido Nítrico/química , Staphylococcus aureus/efectos de los fármacos
10.
Anal Bioanal Chem ; 410(6): 1709-1724, 2018 Feb.
Artículo en Inglés | MEDLINE | ID: mdl-29285646

RESUMEN

In this study, the strategy of unique adsorbent combined with isotope labeled internal standards was used to significantly reduce the matrix effect for the enrichment and analysis of nine fluoroquinolones in a complex sample by liquid chromatography coupled to quadrupole linear ion trap mass spectrometry (LC-QqQLIT-MS/MS). The adsorbent was prepared conveniently by functionalizing Fe3O4@SiO2 microspheres with phenyl and tetrazolyl groups, which could adsorb fluoroquinolones selectively via hydrophobic, electrostatic, and π-π interactions. The established magnetic solid-phase extraction (MSPE) method as well as using stable isotope labeled internal standards in the next MS/MS detection was able to reduce the matrix effect significantly. In the process of LC-QqQLIT-MS/MS analysis, the precursor and product ions of the analytes were monitored quantitatively and qualitatively on a QTrap system equipped simultaneously with the multiple reaction monitoring (MRM) and enhanced product ion (EPI) scan. Subsequently, the enrichment method combined with LC-QqQLIT-MS/MS demonstrated good analytical features in terms of linearity (7.5-100.0 ng mL-1, r > 0.9960), satisfactory recoveries (88.6%-118.3%) with RSDs < 12.0%, LODs = 0.5 µg kg-1 and LOQs = 1.5 µg kg-1 for all tested analytes. Finally, the developed MSPE-LC-QqQLIT-MS/MS method had been successfully applied to real pork samples for food-safety risk monitoring in Ningxia Province, China. Graphical abstract Mechanism of reducing matrix effect through the as-prepared adsorbent.


Asunto(s)
Antibacterianos/análisis , Fluoroquinolonas/análisis , Análisis de los Alimentos/métodos , Extracción en Fase Sólida/métodos , Espectrometría de Masas en Tándem/métodos , Adsorción , Límite de Detección , Imanes/química , Carne Roja/análisis
11.
Mikrochim Acta ; 185(2): 113, 2018 01 12.
Artículo en Inglés | MEDLINE | ID: mdl-29594664

RESUMEN

The authors describe the preparation of copper-doped magnetic microspheres (Cu-Fe3O4) by a solvothermal method. Due to their good magnetic property and high affinity for compounds containing an imidazole moiety (containing N-H), they are excellent adsorbents for such compounds as tested by eighteen compounds. Specifically, a method has been developed for magnetic solid-phase extraction (MSPE) of theophylline (TP) from plasma. The method enables selective enrichment of TP over many potential interferents that can occur in plasma. Following elution with alkaline methanol, TP was quantified by HPLC-UV at a detection wavelength of 272 nm. Under the optimized conditions, a linear response is found for the 0.02 to 20 µg·mL-1 concentration range, and the limit of detection is as low as 3 ng·mL-1. Recoveries from spiked samples range from 91.2 to 100.4%, and the repeatabilities are between 2.9 and 12% (for n = 6). The method was successfully applied to the determination of TP in rabbit and rat plasma. Graphical abstract Copper-doped magnetic microspheres are described that show good magnetic property and high affinity for compounds containing an imidazole moiety (containing an N-H group). They were successfully applied to the selective extraction of theophylline in plasma.

12.
Mikrochim Acta ; 185(3): 189, 2018 02 20.
Artículo en Inglés | MEDLINE | ID: mdl-29594797

RESUMEN

Poly(3-acrylamidophenylboronic acid) (PAAPBA) was grafted onto polydopamine-coated magnetic graphene oxide via surface-initiated atom transfer radical polymerization to obtain a new kind of boronate affinity material (BAM). The BAM possesses good water dispersity and adsorption capacities as high as 154, 357, 588 and 1111 µmol·g-1 for adenosine, salbutamol, dopamine and catechol, respectively. For the molecules without nitrogen atoms, the BAM can selectively capture the cis-diols under the interference of non-cis-diols. For molecules containing nitrogen, the non-cis-diols are also retained, but much less than the cis-diols. The selectivity can be improved by adding salts to facilitate complexation and to suppress the electrostatic interaction between cis-diols and the boronic acid ligand. The BAM was successfully employed to the enrichment of catecholamines from real urine samples. Results indicate that it is a promising material for the pretreatment of real samples. Graphical abstract Schematic of the preparation of an ultrahigh capacity boronate affinity material by grafting polymer brush from polydopamine coated magnetic graphene oxide. The material has good selectivity to cis-diol-containing molecules and can be applied to enrich catecholamines in urine samples.

13.
Mikrochim Acta ; 185(8): 370, 2018 07 09.
Artículo en Inglés | MEDLINE | ID: mdl-29987393

RESUMEN

Poly(2-naphthyl acrylate) was first grafted onto silica-coated magnetic nanoparticles by surface-initiated atom transfer radical polymerization to prepare a reversed-phase magnetic adsorbent. The resulting polymer brush displays enhanced extraction efficiency by offering active sites on the surfaces of adsorbent. It was applied to the preconcentration of the non-steroidal antiinflammatory drugs (NSAIDs) indomethacin (InDo) and diclofenac (DIC). These drugs interact with the sorbent through hydrophobic and π-interactions, and via electrostatic attraction. By coupling the magnetic solid-phase extraction with HPLC, a method for analysis of InDo and DIC in the environmental water samples was established. The limits of detection range from 0.62 to 0.64 ng·mL-1, and the relative standard deviations for intra-and inter-day analyses of spiked water samples are <11.9%, and relative recoveries are between 62.1 and 96.7%. Graphical abstract A reversed-phase magnetic adsorbent was prepared by grafting poly(2-naphthyl acrylate) brush on the surface of silica coated magnetic nanoparticles. Due to the two conjugated aromatic rings of the monomer, the polymer brush can effectively extract non-steroidal anti-inflammatory drugs through strong π- and hydrophobic interactions.


Asunto(s)
Métodos Analíticos de la Preparación de la Muestra/métodos , Antiinflamatorios no Esteroideos/análisis , Diclofenaco/análisis , Indometacina/análisis , Nanopartículas de Magnetita/química , Naftalenos/química , Polímeros/química , Adsorción , Antiinflamatorios no Esteroideos/aislamiento & purificación , Cromatografía Líquida de Alta Presión , Diclofenaco/aislamiento & purificación , Indometacina/aislamiento & purificación , Dióxido de Silicio/química , Extracción en Fase Sólida
14.
Mikrochim Acta ; 185(8): 361, 2018 07 05.
Artículo en Inglés | MEDLINE | ID: mdl-29978437

RESUMEN

The authors report on the preparation of composites made from graphene oxide (GO) and zeolitic imidazolate framework-8 (ZIF-GO), with various fractions of GO. GO acts as the template and as a modulator for the surface properties of the composites. It also improves the selective adsorption of specific proteins, i.e. hemoglobin (Hb) in this case. The adsorption capacity for Hb is as high as 436 mg g-1 when using a composite containing 20% of GO as sorbent, and 95% of specific activity is maintained for the Hb recovered. The sorbent is applied to selectively isolate Hb from human whole blood. Graphical abstract Graphene oxide-zeolitic imidazolate framework-8 composites (ZIF-GO) with varying mass ratios of GO were prepared in order to tune surface properties and to improve the adsorption selectivity toward hemoglobin.


Asunto(s)
Fraccionamiento Químico/métodos , Grafito/química , Hemoglobinas/aislamiento & purificación , Imidazoles/química , Óxidos/química , Zeolitas/química , Adsorción , Hemoglobinas/análisis , Humanos , Modelos Moleculares , Conformación Molecular
15.
J Sep Sci ; 40(9): 1861-1868, 2017 May.
Artículo en Inglés | MEDLINE | ID: mdl-28247469

RESUMEN

Mixed-mode chromatographic stationary phases require functionalization with at least two functional groups to yield multiple interactions with analytes. Departing from reported methods, a mixture of two different monomers, glycidyl methacrylate and 2-dimethylaminoethylmethacrylate, was grafted onto the surface of silica by a one-step surface-initiated atom transfer radical polymerization to prepare a novel hydrophilic interaction/anion-exchange mixed-mode chromatographic stationary phase. The grafted amounts of functional groups were controlled via varying the ratio of monomers in the polymerization system. The influences of water content, salt concentration and pH in the mobile phase were investigated to illustrate the mixed interaction between the stationary phase and analytes. The retention of various solutes on three columns, especially acidic and basic solutes, showed an obvious dependence on the ratio of the two monomers in the polymerization system. The results indicated that the strategy proposed in this work was beneficial to develop various types of mixed-mode chromatographic stationary phases with adjustable selectivity to meet the needs of complex samples. Finally, the column was successfully employed in the isolation of melamine in liquid milk.


Asunto(s)
Cromatografía por Intercambio Iónico , Leche/química , Triazinas/análisis , Animales , Interacciones Hidrofóbicas e Hidrofílicas , Polimerizacion , Dióxido de Silicio
16.
J Sep Sci ; 40(24): 4700-4708, 2017 Dec.
Artículo en Inglés | MEDLINE | ID: mdl-29044953

RESUMEN

A novel approach that involved the grafting of diblock copolymer with two types of monomer onto substrate by sequential surface initiated-atom transfer radical polymerization was proposed to prepare a mixed-mode chromatographic stationary phase. The distinguishing feature of this method is that it can be applied in the preparation of various mixed-mode stationary phases. In this study, a new reverse-phase/ion-exchange stationary phase was prepared by grafting hydrophobic styrene and cationic sodium 4-styrenesulfonate by the proposed approach onto silica surface. The chromatographic properties of the prepared stationary phase were evaluated by the separation of benzene derivatives, anilines, and ß-agonists, and by the effect of pH values and acetonitrile content on the retention. Compared with typical RP columns, the prepared stationary phase achieved the better resolution and higher selectivity at a shorter separation time and lower organic content. Moreover, the application of the prepared column was proved by separating widely distributed polar and charged compounds simultaneously.

17.
Anal Bioanal Chem ; 408(27): 7595-7605, 2016 Nov.
Artículo en Inglés | MEDLINE | ID: mdl-27580602

RESUMEN

Immobilized metal affinity chromatography (IMAC) has been widely used for the specific separation of biopolymers. However, leakage of metal ions from IMAC adsorbents is of concern in IMAC. In this study, we designed a novel tridenate bis(5-methyltetrazolium)amine (BMTA) to reduce the leakage of metal ions by improving the affinity to immobilized metal ions. The ligand was bonded onto silica via three-step reaction to prepare a high-performance IMAC stationary phase. The chromatographic behaviors of ribonuclease A, cytochrome c, and lysozyme on the Cu(II)-, Ni(II)-, and Zn(II)-chelated stationary phase were investigated with respect to pH effect and elution with an imidazole gradient. The retention times of these three proteins increased by increasing the pH of the mobile phase but decreased by increasing the concentration of the competitive displacer. The retaining strength of the three proteins on the chelated stationary phase were in the order Cu(II) > Ni(II) > Zn(II). The behavior of these three proteins was consistent with the properties of a typical IMAC. The BMTA ligand exhibited a much stronger affinity for Cu(II) and Ni(II) than iminodiacetic acid (IDA), which is often regarded as a standard tridentate IMAC ligand. Quantum mechanical calculations at the B3LYP/6-31G level were used to image the coordination mode of the protein-metal ions-BMTA complex. In addition, a fused histidine-tagged cecropin b-human epidermal growth factor (CB-EGF) from Escherichia coli crude extract was purified by the Ni(II)-chelated stationary phase, and the purity of the CB-EGF was determined to be at least 90 %. These results suggest that the BMTA ligand may have potential applications in the preparation of therapeutics. Graphical Abstract A novel ligand of tridenate bis(5-methyltetrazolium)amine (BMTA) was designed to reduce the leakage of metal ions from the column in immobolized metal affinity chromatography (IMAC).


Asunto(s)
Cromatografía de Afinidad/métodos , Citocromos c/aislamiento & purificación , Muramidasa/aislamiento & purificación , Ribonucleasa Pancreática/aislamiento & purificación , Sales de Tetrazolio/química , Adsorción , Cobre/química , Factor de Crecimiento Epidérmico/aislamiento & purificación , Humanos , Concentración de Iones de Hidrógeno , Imidazoles/química , Iminoácidos/química , Níquel/química , Teoría Cuántica , Dióxido de Silicio/química , Zinc/química
18.
Biomed Chromatogr ; 29(8): 1133-6, 2015 Aug.
Artículo en Inglés | MEDLINE | ID: mdl-25624166

RESUMEN

Boronate affinity has attracted much attention in recent years. It has been broadly used for selective isolation and enrichment of cis-diol-containing molecules. Conventionally, the cis-diols are adsorbed in mild alkaline aqueous solutions. In this work, for the first time, we found that boronate affinity adsorption could also be performed in nonaqueous solvent at nonbasic pH. Cis-diol-containing compounds present in herbal medicines were used for the adsorption test. The results indicated that all compounds obtained higher recoveries in the organic solvents (methanol, acetonitrile, ethyl acetate) compared with alkaline buffer. The adsorption of vicinal cis-diol-containing molecules in organic solvents could be accomplished rapidly, with high selectivity and high recoveries (>80%). These results shed light on the possibility of boronate affinity adsorption in nonaqueous solvents. The results are very important for the isolation and enrichment of cis-diols, which have poor solubility in water, especially for those in herbal medicines.


Asunto(s)
Ácidos Borónicos/química , Ácidos Cafeicos/aislamiento & purificación , Luteolina/aislamiento & purificación , Quercetina/aislamiento & purificación , Rutina/aislamiento & purificación , Adsorción , Cromatografía de Afinidad/métodos , Solventes/química
19.
Biomed Chromatogr ; 29(12): 1834-41, 2015 Dec.
Artículo en Inglés | MEDLINE | ID: mdl-26061980

RESUMEN

Salbutamol (SAL) is the most widely used ß2 -agonist drug for asthma and chronic obstructive pulmonary patients, but it is also often abused as feed additive. In recent years, the abuse of SAL has led to a large number of food safety incidents. Therefore, the monitoring of SAL residues in animal products is very important. A highly selective boronate affinity magnetic adsorbent was synthesized and developed for detection of trace levels of SAL residues in pig tissue samples. The obtained Fe3O4@SiO2@FPBA(4-formylphenylboronic acid) magnetic adsorbent showed good adsorption ability to catechol and SAL, and then it was successfully applied as special magnetic solid-phase phase extraction adsorbent coupled with high-performance liquid chromatography (HPLC) for simultaneous isolation and determination of cis-diol compounds. The binding capacity of catechol and SAL reached 96 and 50 µmol/g, respectively. The method was successfully established for the detection of trace levels of SAL in pig tissue samples. The linear range extended from 0.32 to 800 µg/kg (R(2) = 0.9994). The limit of detection of SAL was 0.19 µg/kg. The recoveries were satisfactory (89.5-108.0%) at three spiked levels with RSD between 2.1 and 11.3%. These results indicated that the method has potential for enrichment and detection of trace levels of SAL residual in animal food products.


Asunto(s)
Albuterol/análisis , Ácidos Borónicos/química , Cromatografía Líquida de Alta Presión/métodos , Residuos de Medicamentos/análisis , Carne/análisis , Extracción en Fase Sólida/métodos , Albuterol/aislamiento & purificación , Animales , Residuos de Medicamentos/aislamiento & purificación , Límite de Detección , Modelos Lineales , Imanes , Reproducibilidad de los Resultados , Porcinos
20.
J Chromatogr A ; 1735: 465308, 2024 Oct 25.
Artículo en Inglés | MEDLINE | ID: mdl-39244912

RESUMEN

The high speed enrichment of benzoylurea insecticides (BUs) in complex matrices is an essential and challenging step. The present study focuses on the synthesis of a hierarchical pore nitrogen-doped carbon material for magnetic solid phase extraction (MSPE) of BUs. This material was prepared through the carbonization of a composite material ZIF-67@MCA which assembly with hydrogen-bonded organic frameworks (melamine-cyanurate, MCA) and zeolitic imidazolate framework (ZIF-67) at room temperature. The optimal adsorption effect is achieved when the mass ratio of ZIF-67 to MCA is 1/3, and the carbonization was performed at 600 °C, the such obtained carbon material was denoted as 1/3ZIF-67@MCA-DCs-600. The material was characterized with various physical methods including X-ray diffractometry (XRD), Fourier transform infrared spectrometry (FTIR), X-ray photoelectron spectroscopy (XPS), scanning electron microscope (SEM), Brunauer-Emmett-Teller (BET), vibrating sample magnetometer (VSM), water contact angle measurement, Raman spectrometry. 1/3ZIF-67@MCA-DCs-600 exhibits a macro-mesoporous 3D structure with a high degree of nitrogen doping and relatively large specific surface area, making it suitable for magnetic solid phase extraction (MSPE). The adsorption of BUs with concentration of 100 ng mL-1 can reach equilibrium within 5 s. The interaction between BUs and the adsorbent, facilitated by π-π stacking, hydrophobic interactions, hydrogen bonding forces, as well as the material's porosity, enables efficient extraction recoveries ranging from 45 % to 92 %. The enrichment of BUs was achieved through the establishment of an MSPE method under optimized conditions, which was further coupled with high performance liquid chromatography (HPLC) for the determination of the four BUs. The linear range spans from 5 ng ml-1 to 1000 ng ml-1 with the correlation coefficient (R2) of ≥ 0.99, Meanwhile, the detection limit for these four BUs falls within the range of 0.01 to 0.10 ng ml-1. The material exhibits good reusability and can be reused for at least 5 cycles. Inter day and intra-day precision ranges from 2.1-7.9 % and 1.0-5.4 %, respectively. The method demonstrates a high level of reliability in practical applications for the determination of BUs.


Asunto(s)
Carbono , Enlace de Hidrógeno , Insecticidas , Nitrógeno , Extracción en Fase Sólida , Insecticidas/análisis , Insecticidas/química , Insecticidas/aislamiento & purificación , Extracción en Fase Sólida/métodos , Adsorción , Carbono/química , Nitrógeno/química , Estructuras Metalorgánicas/química , Porosidad , Triazinas/química , Triazinas/aislamiento & purificación , Límite de Detección , Urea/química , Zeolitas/química
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