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1.
Ann Nucl Med ; 34(7): 460-466, 2020 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-32390105

RESUMO

OBJECTIVE: The APTEDB is an aptide specific to the extra domain B (EDB) of fibronectin with high affinity for EDB, which is expressed in malignant tumors including brain cancer (U87MG) and colorectal cancer (HT-29). Aim of this study was to evaluate the [99mTc] Tc-APTEDB potential as an imaging probe for colorectal cancer. METHODS: Radiochemical purity was evaluated by HPLC and radio-isotope TLC scanner. Blocking study for specific binding assay and affinity calculation (Kd) on HT-29 cell lines were also carried out. Planar imaging and bio-distribution studies were performed in HT-29 tumor-bearing mice. RESULTS: The APTEDB was efficiently labeled with technetium-99m in high radiochemical yield (up to 97%). Cellular binding study demonstrated specific binding of the [99mTc] Tc-APTEDB in cultured HT-29 cells. The Kd value was found to be 40.46 ± 13.39 nM. The tumor-to-muscle ratio was ~ 1.5 in ex vivo bio-distribution study at 1 h after injection. Planar imaging study showed higher activity accumulation in EDB expressing HT-29 tumor relative to muscle (used as control) (~ 1.7) at 1 h. CONCLUSIONS: Although more studies are required to find out the full potential of this radio-ligand as an imaging probe, the present results nevertheless provide useful information about [99mTc] Tc-APTEDB, which might be beneficial in design and development of new [99mTc] Tc-APTEDB for efficient targeting of tumor in vivo.


Assuntos
Neoplasias Colorretais/metabolismo , Peptídeos/química , Peptídeos/metabolismo , Tecnécio/química , Animais , Linhagem Celular Tumoral , Transformação Celular Neoplásica , Neoplasias Colorretais/diagnóstico por imagem , Neoplasias Colorretais/patologia , Células HT29 , Humanos , Marcação por Isótopo , Camundongos , Radioquímica , Distribuição Tecidual
2.
Anal Chem ; 89(17): 8808-8815, 2017 09 05.
Artigo em Inglês | MEDLINE | ID: mdl-28770992

RESUMO

A prerequisite for ordered two-dimensional (2D) separations and full utilization of the enhanced 2D peak capacity is selective exploitation of the sample attributes, described as sample dimensionality. In order to take sample dimensionality into account prior to optimization of a 2D separation, a new concept based on construction of 2D separation selectivity maps is proposed and demonstrated for ion chromatography × capillary electrophoresis (IC×CE) separation of low-molecular-mass organic acids as test analytes. For this purpose, 1D separation selectivity maps were constructed based on calculation of pairwise separation factors and identification of critical pairs for four IC stationary phases and 28 levels of background electrolyte pH in CE. The derived IC and CE maps were then superimposed and the effectiveness of the respective 2D separations assessed using an in silico approach, followed by testing examples of one successful and one unsuccessful 2D combination experimentally. The results confirmed the efficacy of the predictions, which require a minimal number of experiments compared to the traditional one-at-a-time approach. Following the same principles, the proposed framework can also be adapted for optimization of separation selectivity in various 2D combinations and for other applications.

3.
Anal Chim Acta ; 950: 7-31, 2017 Jan 15.
Artigo em Inglês | MEDLINE | ID: mdl-27916132

RESUMO

Described as intrinsically powerful building blocks for two-dimensional separations by Giddings [Anal. Chem., 56 (1984) 1258A-1270A], the coupling of chromatography and electrophoresis has been proven to enhance the resolution of a wide array of molecules in complex biological, environmental and food samples. This review provides a comprehensive overview of multidimensional chromato-electrophoretic (LC - E) and electrophero-chromatographic (E - LC) separation systems from inception to the most recent published examples. LC separation modes include reversed phase, ion exchange, and size exclusion. Electromigration separation modes include capillary, microchip or free flow electrophoresis; micellar electrokinetic chromatography; electrochromatography; and isoelectric focusing. The advantages and disadvantages of various non-gel based off-line and on-line hyphenation technologies of LC - E and E - LC are discussed, with conditions and system characteristics also provided.

4.
Anal Chem ; 87(17): 8673-8, 2015 Sep 01.
Artigo em Inglês | MEDLINE | ID: mdl-26171657

RESUMO

A comprehensively coupled online two-dimensional ion chromatography-capillary electrophoresis (IC × CE) system for quantitative analysis of inorganic anions and organic acids in water is introduced. The system employs an in-house built sequential injection-capillary electrophoresis instrument and a nonfocusing modulation interface comprising a tee-piece and a six-port two-position injection valve that allows comprehensive sampling of the IC effluent. High field strength (+2 kV/cm) enables rapid second-dimension separations in which each peak eluted from the first-dimension separation column is analyzed at least three times in the second dimension. The IC × CE approach has been successfully used to resolve a suite of haloacetic acids, dalapon, and common inorganic anions. Two-dimensional peak capacity for IC × CE was 498 with a peak production rate of 9 peaks/min. Linear calibration curves were obtained for all analytes from 5 to 225 ng/mL (except dibromoacetic acid (10-225 ng/mL) and tribromoacetic acid (25-225 ng/mL)). The developed approach was used to analyze a spiked tap water sample, with good measured recoveries (69-119%).

5.
Eur Arch Otorhinolaryngol ; 272(10): 2697-701, 2015 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-25145642

RESUMO

The purpose of the present study was to evaluate effect of depth of general anesthesia on the threshold of electrically evoked compound action potential in cochlear implantation. A prospective clinical study in a single-subject design was conducted in the cochlear implant center of a tertiary care University-based hospital. Sixty-one cochlear-implanted children with bilateral, severe to profound sensory neural hearing loss were enrolled in the study. During the operation electrically evoked compound action potentials (e-ECAP) were measured in two phase of general anesthesia; in deep and in light anesthesia. Thresholds of e-ECAP in these two phases of anesthesia were compared. Thirty-one children received HiRes90k1j prosthesis and 30 children received CI24RE prosthesis. Thresholds difference of electrically evoked compound action potential between light and deep anesthesia in all tested electrodes in either group were statistically significant (P < 0.001). Non-measurable e-ECAP in some electrodes at deep anesthesia was measurable in light phase of anesthesia. Depth of anesthesia can have significant influence on e-ECAP threshold and it is important to reduce the depth of anesthesia to achieve better results.


Assuntos
Anestesia Geral/métodos , Limiar Auditivo/fisiologia , Implante Coclear/métodos , Potenciais Evocados Auditivos/fisiologia , Perda Auditiva Neurossensorial/cirurgia , Criança , Pré-Escolar , Feminino , Perda Auditiva Neurossensorial/fisiopatologia , Humanos , Lactente , Masculino , Estudos Prospectivos
6.
Electrophoresis ; 36(1): 36-61, 2015 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-25330057

RESUMO

One of the most cited limitations of capillary (and microchip) electrophoresis is the poor sensitivity. This review continues to update this series of biannual reviews, first published in Electrophoresis in 2007, on developments in the field of on-line/in-line concentration methods, covering the period July 2012-July 2014. It includes developments in the field of stacking, covering all methods from field-amplified sample stacking and large-volume sample stacking, through to ITP, dynamic pH junction, and sweeping. Attention is also given to on-line or in-line extraction methods that have been used for electrophoresis.


Assuntos
Eletroforese Capilar/instrumentação , Eletroforese Capilar/métodos , Animais , Desenho de Equipamento , Humanos , Concentração de Íons de Hidrogênio , Extração Líquido-Líquido/instrumentação , Extração Líquido-Líquido/métodos , Tamanho da Amostra , Sensibilidade e Especificidade , Extração em Fase Sólida/instrumentação , Extração em Fase Sólida/métodos
7.
Biol Trace Elem Res ; 147(1-3): 378-85, 2012 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-22187326

RESUMO

In the present study, a novel quantitative method, namely magnetic nanoparticle-based solid-phase extraction (MSPE), was applied to extract vitamin B(12) from pharmaceutical formulations. The technique involves the use of Fe(3)O(4) nanoparticles modified by sodium dodecyl sulfate (SDS) as an efficient adsorbent for solid-phase extraction of vitamin B(12). Collection of magnetic nanoparticles (MNPs) from aqueous solution was simply achieved by applying external magnetic field. The analyte was desorbed from MNPs using alkali 1-propanol. The extracted analyte was analyzed by using flow injection inductively coupled plasma-optical emission spectrometry. Factors affecting the extraction efficiency were investigated and optimized. Under the optimum conditions, enhancement factor of 184, linear dynamic range of 2.5-500 µg L(-1) with correlation of determination (R(2) > 0.999), and limit of detection of 1.0 µg L(-1) were obtained for vitamin B(12). The percent relative standard deviation based on five-replicate determination was less than 6.2%. The method was successfully applied for extraction and determination of vitamin B(12) in different types of pharmaceutical samples such as multivitamin tablet, effervescent tablet, and injection sample. The results showed that the proposed method based on SDS-Fe(3)O(4) MSPE was a simple, accurate, and highly efficient approach for analysis of vitamin B(12).


Assuntos
Nanopartículas de Magnetita/química , Preparações Farmacêuticas/química , Extração em Fase Sólida/métodos , Vitamina B 12/análise , Vitamina B 12/isolamento & purificação , Adsorção , Concentração de Íons de Hidrogênio , Nanopartículas de Magnetita/ultraestrutura , Microscopia Eletrônica de Varredura , Reprodutibilidade dos Testes , Dodecilsulfato de Sódio/química , Espectrofotometria Atômica/métodos , Comprimidos , Fatores de Tempo , Vitamina B 12/farmacocinética , Complexo Vitamínico B/química
8.
Mol Divers ; 12(3-4): 191-6, 2008.
Artigo em Inglês | MEDLINE | ID: mdl-18830679

RESUMO

A rapid and efficient one-pot method for the synthesis of 4,6-diarylpyrimidin-2(1H)-ones and related heterocycles is described. The condensation of acetophenone derivatives, aldehydes and urea in the presence of sulfamic acid was employed to synthesize a variety of pyrimidinones in moderate to excellent yields. The scope and limitations of this method are described.


Assuntos
Pirimidinonas/síntese química , Catálise , Conservação dos Recursos Naturais , Espectroscopia de Ressonância Magnética , Métodos , Estrutura Molecular , Pirimidinonas/química , Solventes , Espectrofotometria Infravermelho , Ácidos Sulfônicos
9.
Mol Divers ; 12(3-4): 181-5, 2008.
Artigo em Inglês | MEDLINE | ID: mdl-18780153

RESUMO

A rapid and efficient one-pot method for the synthesis of quinazolinone derivatives and related heterocycles by condensation of 2-amino benzimidazole and 3-amino-1,2,4-triazole, as amine sources, with dimedone and different aldehydes in the presence of H6P2W18O(62).18H2O as a green and reusable catalyst in refluxing acetonitrile has been developed.


Assuntos
Benzimidazóis/química , Benzimidazóis/síntese química , Quinazolinonas/química , Quinazolinonas/síntese química , Ácidos , Catálise , Conservação dos Recursos Naturais , Espectroscopia de Ressonância Magnética , Estrutura Molecular , Compostos de Tungstênio
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