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1.
Adv Mater ; 36(18): e2310663, 2024 May.
Artigo em Inglês | MEDLINE | ID: mdl-38267010

RESUMO

Organic phosphorescent scintillating materials have shown great potential for applications in radiography and radiation detection due to their efficient utilization of excitons. However, revealing the relationship between molecule stacking and the phosphorescent radioluminescence of scintillators is still challenging. This study reports on two phenothiazine derivatives with polymorphism-dependent phosphorescence radioluminescence. The experiments reveal that molecule stacking significantly affects the non-radiation decay of the triplet excitons of scintillators, which further determines the phosphorescence scintillation performance under X-ray irradiation. These phosphorescent scintillators exhibit high radio stability and have a low detection limit of 278 nGys-1. Additionally, the potential application of these scintillators in X-ray radiography, based on their X-ray excited radioluminescence properties, is demonstrated. These findings provide a guideline for obtaining high-performance phosphorescent scintillating materials by shedding light on the effect of crystal packing on the radioluminescence of organic molecules.

2.
Chemphyschem ; 24(22): e202300211, 2023 11 16.
Artigo em Inglês | MEDLINE | ID: mdl-37610324

RESUMO

As an exceptional Fenton-like reagent, cerium oxide (CeO2 ) finds applications in biomedical science and organic pollutants treatment. The Fenton-like reaction catalyzed by CeO2 typically encompasses two distinct processes: one resembling the classical Fenton reaction, wherein cerium (Ce3+ ) triggers the decomposition of hydrogen peroxide (H2 O2 ) to yield reactive oxygen species (ROS), and the other involves the complexation of H2 O2 on the Ce3+ surface, leading to the formation of peroxides. However, the influence of diverse CeO2 morphologies on these two reaction pathways has not been comprehensively explored. In this study, CeO2 exhibiting three typical morphologies, rods, cubes, and spheres, were prepared. The generation of ROS and peroxides was evaluated using the 3,3,5,5-tetramethylbenzidine (TMB) oxidation reaction and the reduction current of H2 O2 , respectively. Moreover, the impacts of pH variations and CeO2 /H2 O2 concentrations on the production and conversion of these two reaction products were investigated. To corroborate the distinctions between the resultant products and their applicability, apoptosis assays and acid orange 7 (AO7) degradation analyses were performed. Notably, CeO2 rods exhibited the highest proportion of Ce3+ , predominantly engaging in complexation with H2 O2 to foster peroxide formation, thereby facilitating the robust degradation of AO7. However, the generated peroxides appeared to occupy Ce3+ sites, thereby impeding the H2 O2 decomposition process. Conversely, Ce3+ species on the surface of CeO2 cubes were primarily involved in H2 O2 decomposition, leading to heightened ROS production, and thus showcasing substantial potential for damaging A549 tumor cells. It is worth noting that the ability of these Ce3+ species to form peroxides through complexation with H2 O2 was comparatively reduced. In summation, this study sheds light on the intricate interplay between distinct CeO2 morphologies and their divergent impacts on Fenton-like reactions. These findings expand our comprehension of the influences on its reactivity of CeO2 morphologies and open new insights for applications in diverse domains, from organic dye degradation to tumor therapy.


Assuntos
Cério , Peróxidos , Espécies Reativas de Oxigênio , Catálise , Cério/química
3.
Chem Commun (Camb) ; 58(95): 13266-13269, 2022 Nov 29.
Artigo em Inglês | MEDLINE | ID: mdl-36373264

RESUMO

We present a novel series of neutral photo-acid generators (PAGs) based on carbazole derivatives. A photo-induced 6π-electrocyclization reaction of carbazole derivatives triggers the subsequent release of halogen acids. With UV irradiation, PAGs spontaneously release acid molecules quantitatively forming polyaromatic compounds. To our knowledge, it is considered the highest quantum yield (over 85%) among Brønsted PAGs.

4.
Pathogens ; 11(6)2022 Jun 20.
Artigo em Inglês | MEDLINE | ID: mdl-35745562

RESUMO

The increasing prevalence of crop-threatening root-knot nematodes (RKNs) has stimulated extensive research to discover effective nematicides. A highly focused strategy for accomplishing this is the development of biocontrol agents by a variety of soilborne microorganisms, as different bacterial metabolites have demonstrated promising nematicidal activities. In this study, we characterized the nematicidal and suppressive activity of a bacterial isolate against the agriculturally important RKN Meloidogyne incognita and the model nematode Caenorhabditis elegans, and the main M. incognita-toxic metabolite of the strain. After a preliminary screening of 22 bacterial isolates with a corrected mortality (CM) of whole-cell culture greater than 50% against C. elegans from different RKN-incident soils in China, a total of 14 isolates with CM of the supernatant of culture suspension (SCS) higher than 50% against both M. incognita and C. elegans were rescreened. An isolate with the highest CM of 86.1% and 95.0% for M. incognita and C. elegans, respectively, was further identified as the species Brevundimonas bullata via morphological examination, physiological and biochemical assays and alignment analysis of 16S rRNA gene sequences. The SCS of this strain, namely, B. bullata MB756, exhibited synchronous M. incognita killing activity along with significant detrimental effects on the growth, brood size, and locomotion of C. elegans. The effects of heat treatment, pH, inoculations, and protease K proteolysis on the CM of MB756 SCS were evaluated. A major M. incognita-toxic substance in the MB756 SCS was assayed and identified using thin-layer chromatography, column chromatography and high-performance liquid chromatography with a mass spectrometer, and it was preliminarily identified as 2-ethylhexan-1-ol, with a molecular formula of C8H18O and a molecular weight of 130.3 Da.

5.
Front Pharmacol ; 12: 792360, 2021.
Artigo em Inglês | MEDLINE | ID: mdl-34938196

RESUMO

Sonodynamic therapy (SDT) is a developing modality for cancer treatment based on the synergistic effect of ultrasound and chemical compounds which are known as sonosensitizers. The development of more efficient sonosensitizers has become an urgent issue in this field. In this study, a novel porphyrin derivative (BBTPP) mediated SDT was evaluated on PC-9 cells. Pulsed low-intensity ultrasound (PLIU) was used for its little thermal and mechanical damage. The accumulation of drugs in cells was evaluated through porphyrin fluorescence, and the cytotoxicity of BBTPP was evaluated using a cell counting kit-8 assay. The sonodynamic effect was investigated by Hoechst 33342/PI and Annexin V-FITC/PI double staining, which showed an apoptotic rate of 18.87% in the BBTPP-SDT group, as compared with 1.71%, 1.4%, 1.57%, 3.61%, 11.18% in the control, BBTPP, hematoporphyrin monomethyl ether (HMME), ultrasound, and HMME-SDT groups, respectively. The sono-toxic effect of BBTPP was significantly superior to HMME. Our results showed that BBTPP-SDT resulted in much higher intracellular reactive oxygen species (ROS) and lipid peroxidation levels which were evaluated by 2',7'-dichlorodihydrofluorescein diacetate (H2DCFDA) and Liperfluo assay, respectively. The expressions of Bax, Bcl-2, caspase-9, caspase-8, and cleaved caspase-3 proteins were evaluated to investigate the apoptotic mechanism of BBTPP-SDT. The results of this study showed that the combination of BBTPP and PLIU induced the generation of ROS, resulting in lipid peroxidation, and activated both the extrinsic and intrinsic apoptotic pathways of PC-9 cells. Our results also suggested that the ether group introduced in the side chain of porphyrin could enhance the sono-toxicity of porphyrin-based sensitizers under the sonication of PLIU. These results supported the possibility of BBTPP as a promising sonosensitizer, and an appropriate side chain could enhance the sono-sensitivity of porphyrins.

6.
Front Oncol ; 11: 715541, 2021.
Artigo em Inglês | MEDLINE | ID: mdl-34540685

RESUMO

BACKGROUND: Hepatocellular carcinoma (HCC) is known for its poor prognosis. Long noncoding RNAs (lncRNAs) are critical in the pathogenesis of various types of cancers. We tried to explore the role of lncRNA in the development of HCC. METHODS: We identified the role of lncRNA AC007639.1 in the pathogenesis of HCC through bioinformatics and biological experiments in HepG2, Hep3B, and SMMC-7721 cells as well as the nude mice xenograft model. RESULTS: We found that lncRNA AC007639.1 was overexpressed in hepatocellular carcinoma. Knocking down of lncRNA AC007639.1 by specific siRNAs or shRNAs promoted cancer cell death. The growth of mouse xenograft tumor created using lncRNA AC007639.1 deficient HepG2 cells was significantly slowed down. Furthermore, the knockdown of lncRNA AC007639.1 in HCC cells led to the increased expression of p53 and decreased expression of angiopoietin-like 4. CONCLUSION: LncRNA AC007639.1 was involved in the pathogenesis and progression of hepatocellular carcinoma by inhibition of apoptosis and increasing HCC resistance to chemotherapy.

7.
Pest Manag Sci ; 77(10): 4365-4374, 2021 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-33963810

RESUMO

BACKGROUND: Root-knot nematodes (RKNs) are harmful plant-parasitic nematodes that cause serious damage to plant hosts. In the long-term practice of RKN management, bacterial nematicides have attracted increasing attention as an effective biocontrol means. Here we determined the active substances against Meloidogyne incognita from a nematicidal bacterium, developed a biocontrol agent (BCA) based on optimized culture processes. The effects of the BCA on RKN control and plant growth-promotion were evaluated in tomato pot trials. RESULTS: Pseudomonas simiae strain MB751 exhibiting significant nematicidal activity against M. incognita second-stage juveniles (J2) with approximately 80% mortality (with culture supernatant, 96% volume percentage) was isolated from a vineyard. A set of purification and identification experiments was performed to determine the main nematicidal component in MB751. A cyclic dipeptide Cyclo(L-Pro-L-Leu) was identified with a lethal concentration necessary to kill 50% of the population (LC50 ) of 65.3 µg mL-1 against M. incognita J2. Following optimization trials on culture medium/fermentation conditions, such as the single factor test, Plackett-Burman test, steepest ascent, and response surface methodology experiments, the MB751 fermentation broth was then prepared as a BCA via a cold-air drying process. The BCA and was evaluated in tomato pot experiments for effectiveness in suppressing M. incognita. Significant effects on M. incognita suppression and plant-growth promotion as well as induced systemic resistance to M. incognita of tomato, were observed. CONCLUSION: The cyclic dipeptide-producing bacterium P. simiae MB751 exhibited high nematicidal activity and performance. Further development of this BCA should be pursued for the management of M. incognita in agriculture. © 2021 Society of Chemical Industry.


Assuntos
Agentes de Controle Biológico , Pseudomonas , Tylenchoidea , Animais , Antinematódeos/farmacologia , Dipeptídeos
8.
Poult Sci ; 99(11): 5366-5377, 2020 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-33142453

RESUMO

Mycoplasma synoviae (MS) is an important avian pathogen causing considerable economic hardship in the poultry industry. A major inflammation caused by MS is synovitis that occurs in the synovial tendon sheath and joint synovium. However, the overall appearance of pathological changes in the tendon sheath and surrounding tissues caused by MS infection at the level of pathological tissue sections was poor. Studies on the role of MS and synovial sheath cells (SSCs) interaction in the development of synovitis have not been carried out. Through histopathological observation, our study found that a major MS-induced pathological change of the tendon sheath synovium was extensive scattered and focal inflammatory cell infiltration of the tendon sheath synovial layer. In vitro research experiments revealed that the CFU numbers of MS adherent and invading SSC, the levels of expression of various pattern recognition receptors, inflammatory cytokines, and chemokines coding genes, such as IL-1ß, IL-6, IL-8, CCL-20, RANTES, MIP-1ß, TLR7, and TLR15 in SSCs, and chemotaxis of macrophages were significantly increased when the multiplicity of infection (MOI) of MS to SSC were increased tenfold. The expression level of IL-12p40 in SSC was significantly higher when the MOIs of MS to SSC were increased by a factor of 100. The interaction between MS and SSC can activate macrophages, which was manifested by a significant increase in the expression of IL-1ß, IL-6, IL-8, CCL-20, RANTES, MIP-1ß, and CXCL-13. This study systematically demonstrated that the interaction of MS with chicken SSC contributes to the inflammatory response caused by the robust expression of related cytokines and macrophage chemotaxis. These findings are helpful in elucidating the molecular mechanism of MS-induced synovitis in chickens.


Assuntos
Galinhas , Interações Hospedeiro-Patógeno , Cápsula Articular , Infecções por Mycoplasma , Mycoplasma synoviae , Animais , Citocinas/genética , Regulação da Expressão Gênica/imunologia , Interações Hospedeiro-Patógeno/imunologia , Inflamação/veterinária , Cápsula Articular/citologia , Cápsula Articular/microbiologia , Macrófagos/citologia , Macrófagos/microbiologia , Infecções por Mycoplasma/fisiopatologia , Infecções por Mycoplasma/veterinária
9.
Dalton Trans ; 49(42): 14985-14994, 2020 Nov 03.
Artigo em Inglês | MEDLINE | ID: mdl-33084690

RESUMO

Two rare earth metal-organic frameworks (MOFs), [Y2(PTC)2(H2O)2]·3H2O (Y-PTC) and [Eu2(PTC)2(H2O)5]·H2O (Eu-PTC) together with the solid solutions [Eu2xY2(1-x)(PTC)2(H2O)5]·H2O (EuxY1-x-PTC, x = 0.013-0.82), were synthesized hydrothermally, and characterized by microanalysis, IR spectroscopy, TG, powder, and single crystal X-ray diffraction techniques. Eu-PTC and Y-PTC showed different crystal structures; however, all solid solutions were isomorphic to Eu-PTC even at x = 0.013, leading to the IR spectra and TG plots of the solid solutions to be similar to those of Eu-PTC but distinct from those of Y-PTC. DFT calculations for the crystal lattice energy demonstrated that the procedure for the crystallizing nucleation of Eu-PTC occurred prior to that of Y-PTC in the reaction solution, leading to the all solid solutions being isomorphic to Eu-PTC. The solid emission spectra at ambient condition showed that Y-PTC emitted ligand-based phosphorescence at 433 nm with a quantum yield (QY) of 27.02%, while Eu-PTC and EuxY1-x-PTC (x = 0.013-0.82) emitted the characteristic luminescence of Eu3+ ions, and most solid solutions showed higher QYs than Eu-PTC; in particular, the QY of Eu0.195Y0.805-PTC was up to 29.48%, i.e., increased by 10% regarding Eu-PTC (19.86%). Interestingly, solid solutions with x = 0.013-0.395 showed excitation-wavelength-dependent luminescence, and such type of luminescence MOFs have promising applications including the areas of precise temperature, gas sensing and information encryption or anti-counterfeiting materials.

10.
Medicine (Baltimore) ; 99(37): e21944, 2020 Sep 11.
Artigo em Inglês | MEDLINE | ID: mdl-32925727

RESUMO

RATIONALE: Multiple acyl-CoA dehydrogenase deficiency (MADD) is a rare inborn error of metabolism affecting fatty acid, amino acid, and choline metabolism. The clinical manifestation of MADD is heterogeneous, from severe neonatal forms to mild late-onset forms. PATIENT CONCERNS: Here, we report a patient who presented with severe hypoglycemia and exercise intolerance suggestive of MADD. Serum tandem mass spectrometry analysis indicated elevated levels of various acyl carnitines at 25 days of age. Exome sequencing of the proband revealed compound heterozygous mutations, c. 413T>G (p.Leu138Arg) and c.1667C > G (p.Pro556Arg), in the ETFDH gene as the probable causative mutations. DIAGNOSES: Based on the patient's clinical presentation and test results, the patient was diagnosed with MADD. INTERVENTIONS: A high-calorie and reduced-fat diet was given together with oral supplements of L-carnitine (150 mg/day). OUTCOMES: He passed away at the age of 4 months because of severe respiratory distress accompanied by muscle weakness. LESSONS: He passed away at the age of 4 months because of severe respiratory distress accompanied by muscle weakness. Clinicians should consider MADD in the differential diagnosis when patients present with muscle weakness and biochemical abnormalities. Gene testing plays a critical role in confirming the diagnosis of MADD and may not only prevent the need for invasive testing but also allow for timely initiation of treatment.


Assuntos
Flavoproteínas Transferidoras de Elétrons/genética , Proteínas Ferro-Enxofre/genética , Deficiência Múltipla de Acil Coenzima A Desidrogenase/genética , Oxirredutases atuantes sobre Doadores de Grupo CH-NH/genética , Humanos , Recém-Nascido , Masculino , Mutação
11.
Microbiol Resour Announc ; 9(6)2020 Feb 06.
Artigo em Inglês | MEDLINE | ID: mdl-32029555

RESUMO

Here, we report the complete genome sequence of Mycoplasma synoviae HN01, a virulent epidemic strain isolated from a sick chicken with synovitis in Henan Province, China. HN01 is the Asian source of an M. synoviae strain that is completely sequenced, genome annotated, and published with relevant data.

12.
ACS Omega ; 4(7): 12230-12237, 2019 Jul 31.
Artigo em Inglês | MEDLINE | ID: mdl-31460338

RESUMO

Cocrystallization may alter material physicochemical properties; thus, the strategy of forming a cocrystal is generally used to improve the material performance for practical applications. In this study, two transition-metal complex cocrystals [Zn(bpy)3]H0.5BDC·H1.5BDC·0.5bpy·3H2O (1) and [Cu2(BDC)(bpy)4]BDC·bpy·2H2O (2) have been achieved using a hydrothermal reaction, where bpy and H2BDC represent 2,2'-bipyridine and benzene-1,3-dicarboxylic acid, respectively. Cocrystals were characterized by microanalysis, infrared spectroscopy, and UV-visible spectroscopy. Cocrystal 1 contains five components and crystallizes in a monoclinic space group P21/n. The H0.5BDC1.5-, H1.5BDC0.5-, and H2O molecules construct three-dimensional H-bonding organic framework; the [Zn(bpy)3]2+ coordination cations and uncoordinated bpy molecules reside in channels, where two coordinated bpy ligands in [Zn(bpy)3]2+ and one uncoordinated bpy adopt sandwich-type alignment via π···π stacking interactions. Cocrystal 2 with four components crystallizes in a triclinic space group P-1 to form alternating layers; the binuclear [Cu2(bpy)4(BDC)]2+ cations and uncoordinated bpy molecules build the cationic layers, and the BDC2- species with disordered lattice water molecules form the anionic layers. Cocrystal 1 shows intense photoluminescence at an ambient condition with a quantum yield of 14.96% and decay time of 0.48 ns, attributed to the π* → π electron transition within phenyl/pyridyl rings, and 2 exhibits magnetic behavior of an almost isolated spin system with rather weak antiferromagnetic coupling in the [Cu2(bpy)4(BDC)]2+ cation.

13.
Inorg Chem ; 58(10): 6772-6780, 2019 May 20.
Artigo em Inglês | MEDLINE | ID: mdl-31070904

RESUMO

Two new Pb2+-based coordination polymers (CPs), [Pb2(HBTC)2(DMF)] (1) and [Pb(HPTC)] (2), have been synthesized under solvothermal condition; herein, H3BTC and H3PTC represent 1,3,5-benzenetricarboxylic acid and 2,4,6-pyridine tricarboxylic acid, respectively. Both 1 and 2 were characterized by microanalysis, infrared spectra (IR), thermal gravimetric analyses (TGA), and powder X-ray diffraction (PXRD) techniques. Single-crystal structural analysis indicates that 1 and 2 show different coordination sphere around Pb2+ ions and distinct coordination frameworks. The I1O2 type three-dimensional (3D) nonporous metal-organic framework forms in 1, where the Pb2+ ion shows holo-directed coordination geometry, while the I0O2 type two-dimensional (2D) coordination polymeric layered structure forms in 2, where Pb2+ ion shows a hemidirected coordination sphere and the 6s2 lone electron pair in Pb2+ ion is stereochemically active. The two CPs emit intense and long-lasting greenish phosphorescence in air at room temperature, with absolute quantum yields of 1.2% for 1 and 4.7% for 2 and decay lifetimes of 0.73 ms for 1 and 1.52 ms for 2.

15.
ACS Appl Mater Interfaces ; 3(9): 3308-15, 2011 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-21870870

RESUMO

In this paper, highly selective core-shell molecularly imprinted polymers (MIPs) of tadalafil on the surface of magnetic nanoparticles (MNPs) were prepared. Three widely used functional monomers 2-(trifluoromethyl) acrylic acid (TFMAA), acrylic acid (AA), and methacrylic acid (MAA) were compared theoretically as the candidates for MIP preparation. MIP-coated magnetic nanoparticles (MIP-coated MNPs) showed large adsorption capacity, high recognition ability, and fast binding kinetics for tadalafil. Furthermore, because of the good magnetic properties, MIP-coated MNPs can achieve rapid and efficient separation with an external magnetic field simply. The resulting MIP-coated MNPs were used as dispersive solid-phase extraction (DSPE) materials coupled with HPLC-UV for the selective extraction and detection of tadalafil from medicines (herbal sexual health products). Encouraging results were obtained. The amounts of tadalafil that were detected from the herbal sexual health product was 43.46 nmol g(-1), and the recoveries were in the range of 87.36-90.93% with the RSD < 6.55%.


Assuntos
Carbolinas/química , Medicamentos de Ervas Chinesas/química , Nanopartículas de Magnetita/química , Impressão Molecular/métodos , Polímeros/química , Acrilatos/química , Adsorção , Carbolinas/isolamento & purificação , Cromatografia Líquida de Alta Pressão/métodos , Metacrilatos/química , Extração em Fase Sólida/métodos , Tadalafila
16.
J Chromatogr B Analyt Technol Biomed Life Sci ; 879(25): 2595-600, 2011 Sep 01.
Artigo em Inglês | MEDLINE | ID: mdl-21820977

RESUMO

This paper reports a surface molecular self-assembly strategy for molecular imprinting on magnetic nanoparticles for selective separation and detection of estrogens in feeds. First, γ-methacryloxypropyltrimethoxysilane (MEMO) was successfully assembled at the surface magnetic nanoparticles through simple free radical polymerization, and subsequently, the copolymerization was further assembled between methacrylic acid (MAA) and ethylene glycol dimethacrylate (EGDMA) in the presence of templates 17ß-estradiol (E2). The synthesized magnetic molecularly imprinted polymers for E2 (E2-MMIPs) showed quick separation, large adsorption capacity, high selectivity and fast binding kinetics for E2. Meanwhile, a dispersive solid-phase extraction (DSPE) based on E2-MMIPs has been established for efficient separation and fast enrichment of estrogens from the feeds. The assay exhibited a linear range of 0.1-4 µM for E2 and estriol (E3) with the correlation coefficient above 0.9996 and 0.9994, respectively. Recoveries of E2 from three kinds of feeds spiked at different concentration levels ranged from 92.7% to 97.0% with RSD<4.7%, and recoveries of E3 ranged from 71.9% to 83.1% with RSD<4.9%, respectively. The method is simple and sensitive, and can be used as an alternative tool to effectively separate and enrich the trace of estrogens in agricultural products by HPLC-UV.


Assuntos
Ração Animal/análise , Estradiol/química , Nanopartículas de Magnetita/química , Impressão Molecular/métodos , Estriol/análise , Estriol/isolamento & purificação , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Extração em Fase Sólida/métodos , Termodinâmica
17.
J Hazard Mater ; 191(1-3): 177-83, 2011 Jul 15.
Artigo em Inglês | MEDLINE | ID: mdl-21555181

RESUMO

An analytical procedure for selective extraction of sildenafil and vardenafil in herbal dietary supplements (HDSs) has been set up by using the magnetic molecularly imprinted polymers (MMIPs) as the extraction and clean-up materials, followed by high performance liquid chromatography-ultraviolet (HPLC-UV). The MMIPs were prepared by a surface molecular imprinting technique, using Fe(3)O(4) magnetite as a magnetically susceptible component, sildenafil as template molecule, 2-(trifluoromethyl) acrylic acid (TFMAA) as functional monomer, ethylene glycol dimethacrylate (EGDMA) as polymeric matrix components. The MMIPs were characterized by transmission electron microscope (TEM), Fourier transform infrared spectrometer (FT-IR), X-ray diffraction (XRD) and vibrating sample magnetometer (VSM), respectively. The heterogeneity of the MMIPs was modeled with the Freundlich isotherm equation. The resulting MMIPs had high recognition ability and fast binding kinetics for sildenafil. The MMIPs were used as dispersive solid-phase extraction (DSPE) materials to selectively extract sildenafil and vardenafil from HDSs, the contents of sildenafil and vardenafil were found to be 8.05 and 3.86 µg g(-1), respectively, and the average recoveries in spiked HDSs were 70.91-91.75% with a relative standard deviation (R.S.D.) below 7%. The MMIPs were successfully used to selectively enrich and determine sildenafil and vardenafil from HDSs.


Assuntos
Suplementos Nutricionais , Medicina Herbária , Imidazóis/análise , Magnetismo , Inibidores de Fosfodiesterase/análise , Piperazinas/análise , Polímeros/química , Sulfonas/análise , Adsorção , Cromatografia Líquida de Alta Pressão , Cinética , Purinas/análise , Citrato de Sildenafila , Espectrofotometria Ultravioleta , Triazinas/análise , Dicloridrato de Vardenafila , Difração de Raios X
18.
Eur J Drug Metab Pharmacokinet ; 35(3-4): 137-46, 2011 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-21302041

RESUMO

In this study, an attempt was made to describe and validate liquid chromatography-electrospray ionization tandem mass spectrometry as a fast, sensitive and reproducible method for determining finasteride in human plasma. Finasteride and internal standard (pantoprazole) were extracted by liquid-liquid extraction using methyl tert-butyl ether. Separation was performed by using a flow rate gradient on a reverse phase C18 column at 25°C. The mobile phase consisted of methanol-water (70:30, v/v) containing 0.5% anhydrous formic acid. The protonated analytes were quantitated in positive ionization by multiple reaction monitoring in mass spectrometry. The mass transitions are m/z 373.4→305.3 and 384.1→200.0 for finasteride and pantoprazole, respectively. The method had a run time of 3.6 min and a linear calibration curve at a range of 0.2-100 ng mL(-1) (r2=0.9958). The lower limit of quantification was 0.2 ng mL(-1). The extraction recoveries of finasteride from the biological matrix were more than 82.7%, and the intra- and inter-day precision of the assay at four concentrations were 2.4-8.0% with an accuracy of 94.3-105.8%. The developed method requires less plasma (0.1 mL), but has high sensitivity. The validated method has been successfully used to analyze human plasma samples in pharmacokinetic or bioequivalence studies.


Assuntos
Inibidores de 5-alfa Redutase/sangue , Cromatografia Líquida/métodos , Finasterida/sangue , Espectrometria de Massas por Ionização por Electrospray/métodos , Inibidores de 5-alfa Redutase/farmacocinética , Administração Oral , Adulto , Finasterida/farmacocinética , Humanos , Masculino , Reprodutibilidade dos Testes , Espectrometria de Massas em Tandem/métodos , Equivalência Terapêutica , Adulto Jovem
19.
Eur J Drug Metab Pharmacokinet ; 35(3-4): 147-55, 2011 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-21302042

RESUMO

A highly sensitive and rapid method for the analysis of pantoprazole in human plasma using liquid chromatography coupled to tandem electrospray ionization mass spectrometry was developed. The procedure involves a simple protein precipitation method with methyl alcohol and separation by RP-HPLC. Detection was performed by positive ion electrospray ionization in multiple reaction monitoring mode, monitoring the transitions m/z 384.1→200.0 and m/z 346.1→198.0, for quantification of pantoprazole and IS, respectively. The standard calibration curves showed good linearity within the range of 5-5,000 ng mL(-1). The lower limit of quantitation (LLOQ) was about 5 ng mL(-1). The extractive recovery of pantoprazole from the biological matrix was more than 77.58% and the matrix effect was complied with relevant provision. The intra-day accuracy of the drug containing serum samples was more than 92.19% with a precision of 0.79-5.36%. The inter-day accuracy was 85.49% or more, with a precision of 0.91-12.67%. Intra and inter-day accuracy of the assay at four concentrations were 97.9-98.2% with a precision of 4.2-13.9%. This method offered good precision and accuracy and was successfully applied to the pharmacokinetic and bioequivalence studies of 40 mg of enteric-coated pantoprazole in 20 healthy Chinese volunteers.


Assuntos
2-Piridinilmetilsulfinilbenzimidazóis/sangue , Cromatografia Líquida de Alta Pressão/métodos , Inibidores da Bomba de Prótons/sangue , Espectrometria de Massas por Ionização por Electrospray/métodos , 2-Piridinilmetilsulfinilbenzimidazóis/administração & dosagem , 2-Piridinilmetilsulfinilbenzimidazóis/farmacocinética , Administração Oral , Adolescente , Adulto , Calibragem , Cápsulas , China , Estudos Cross-Over , Preparações de Ação Retardada , Humanos , Masculino , Pantoprazol , Inibidores da Bomba de Prótons/administração & dosagem , Inibidores da Bomba de Prótons/farmacocinética , Reprodutibilidade dos Testes , Espectrometria de Massas em Tandem/métodos , Equivalência Terapêutica , Adulto Jovem
20.
J Hazard Mater ; 186(2-3): 1513-9, 2011 Feb 28.
Artigo em Inglês | MEDLINE | ID: mdl-21195544

RESUMO

To assess the potential risks associated with the environmental exposure of steroid estrogens, a novel highly efficient and selective estrogen enrichment procedure based on the use of molecularly imprinted polymer has been developed and evaluated. Herein, analogue of estrogens, namely 17-ethyl estradiol (EE(2)) was used as the pseudo template, to avoid the leakage of a trace amount of the target analytes. The resulting pseudo molecularly imprinted polymers (PMIPs) showed large sorption capacity, high recognition ability and fast binding kinetics for estrogens. Moreover, using these imprinted particles as dispersive solid-phase extraction (DSPE) materials, the amounts of three estrogens (E(1), E(2) and E(3)) which were detected by HPLC-UV from the chicken tissue samples were 0.28, 0.31 and 0.17 µg g(-1), and the recoveries were 72.5-78.7%, 90.3-95.2% and 80.5-83.6% in spiked chicken tissue samples with RSD <7%, respectively. All these results reveal that EE(2)-PMIPs as DSPE materials coupled with HPLC-UV could be applied to the highly selective separation and sensitive determination of trace estrogens in chicken tissue samples.


Assuntos
Galinhas/metabolismo , Estrogênios/análise , Carne/análise , Polímeros/síntese química , Animais , Calibragem , Cromatografia Líquida de Alta Pressão , Estradiol/química , Estrogênios/metabolismo , Géis , Microscopia Eletrônica de Transmissão , Peso Molecular , Nanopartículas , Polímeros/química , Dióxido de Silício , Extração em Fase Sólida , Espectrofotometria Ultravioleta , Espectroscopia de Infravermelho com Transformada de Fourier
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