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1.
Chemosphere ; 362: 142706, 2024 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-38936490

RESUMO

This research investigated the comparative efficacy of sulfamic acid (SA) and phytic acid (PA), both individually and in combination, for treating potential foodborne pathogens and pre-formed foulants. Pathogens studied included Listeria monocytogenes, E. coli DH5α, Salmonella typhimurium, Staphylococcus aureus, and vegetative Bacillus cereus, in suspended aqueous solutions, as well as Pseudomonas aeruginosa biofilm on quartz glass surfaces. Inactivation kinetics for Listeria monocytogenes revealed concentration-dependent rate constants (k) of 6.6(±0.2) × 10-6 M and 2.8(±0.1) × 10-8 M for single treatments of SA and PA, respectively, and ranged from 6.9(±0.3) to 50.7(±2.3) × 10-6 M for combined treatments with PA pre-treatment concentrations of 75-758 µM. Observable cellular abnormalities in Listeria monocytogenes, such as membrane vesiculation, chelation, cellular disruption, biomolecule leakage, and lipid peroxidation, were identified after exposure to PA or SA, either individually or in combination. The optimized combined treatment of PA and SA achieved significant removal (i.e., >3-log; 99.9%) of potential foodborne pathogens under simulated food-washing process conditions. Additionally, over 90% descaling efficacy was observed for pre-formed foulants such as CaCO3 precipitates and Pseudomonas aeruginosa biofilm on quartz glass surfaces with the combined treatment. These findings provide novel insights into the versatile utility of PA and SA for optimizing combinational water disinfection systems and addressing (in)organic foulant scaling on surfaces in the food processing industry.


Assuntos
Listeria monocytogenes , Ácido Fítico , Listeria monocytogenes/efeitos dos fármacos , Listeria monocytogenes/fisiologia , Ácido Fítico/química , Staphylococcus aureus/efeitos dos fármacos , Biofilmes/efeitos dos fármacos , Ácidos Sulfônicos/química , Microbiologia de Alimentos , Pseudomonas aeruginosa/efeitos dos fármacos , Pseudomonas aeruginosa/fisiologia , Escherichia coli/efeitos dos fármacos , Salmonella typhimurium/efeitos dos fármacos , Bacillus cereus/efeitos dos fármacos
2.
Drug Metab Pers Ther ; 38(2): 179-190, 2023 06 01.
Artigo em Inglês | MEDLINE | ID: mdl-36577508

RESUMO

OBJECTIVES: Antioxidant property like radical scavenging is a primary target to elucidate the efficacy mechanism of a drug against diseases linked to oxidative stress such as cancer, metabolic disorders, rheumatoid arthritis, etc. In alternative therapies, homeopathy is one of the preferred choices by patients and clinicians due to its potential to cure chronic and complex illnesses. However, the efficacy of homeopathic preparations at high diluted potencies attracts rational criticism due to insufficient scientific knowledge supporting the mechanism of action. Therefore, an attempt was made to estimate the total phenolic content (TPC) and radical scavenging activity of clinically prescribed homeopathic drugs. METHODS: With gallic acid as a reference control, mother tinctures (MTs) and different potencies of Eucalyptus globulus (EG), Syzygium jambolanum (SJ), Ruta graveolens (RG), and Thuja occidentalis (TO) were used to perform Folin-Ciocalteu test, 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid) (ABTS), and 2,2-diphenyl-1-picrylhydrazyl (DPPH) assays. RESULTS: The results showed TPC of MTs equivalent to µg/mL of gallic acid viz; EG (4,872.5 ± 133.2), SJ (8,840.5 ± 14.8), RG (985.6 ± 39.1), and TO (341.5 ± 19.5) with significant ABTS and DPPH radical scavenging potential. Whereas 30C and 200C potencies of each homeopathic drug showed undetectable phenolic content and insignificant radical scavenging potential compared to vehicle control, i.e., alcohol 90% (2.0 ± 1.5). CONCLUSIONS: The reported efficacy of 30C and 200C potencies of homeopathic medicines against oxidative stress-related illnesses might be due to mechanisms other than radical scavenging. Furthermore, the assays studied can be helpful in drug standardization and quality control of MTs that are used as starting material in homeopathic preparations.


Assuntos
Antioxidantes , Homeopatia , Humanos , Antioxidantes/farmacologia , Antioxidantes/química , Homeopatia/métodos , Ácidos Sulfônicos/química , Ácido Gálico , Fenóis/farmacologia
3.
Future Med Chem ; 14(23): 1741-1753, 2022 12.
Artigo em Inglês | MEDLINE | ID: mdl-36538284

RESUMO

Aim: Cholinesterase inhibitors and radical scavengers have been recognized as powerful symptomatic anti-Alzheimer's disease agents. Hence, the present study aimed to develop new triazineamides as potent anticholinesterase and antioxidant agents. Methods: Triazineamide (7a-i) derivatives were synthesized using cyanuric chloride via nucleophilic substitution followed by condensation. Ellman assay, 2,2-azinobis(3-ethylbenzthiazoline-6-sulfonic acid) radical scavenging assay and molecular docking studies with Autodock 4.2.3 program were conducted. Results: Triazineamide 7c was assessed as a potent, selective and mixed-type dual inhibitor of acetylcholinesterase, with and IC50 of 5.306 ± 0.002 µM, by binding simultaneously with the catalytic active and peripheral anionic sites of acetylcholinesterase, and it had strong 2,2-azinobis(3-ethylbenzthiazoline-6-sulfonic acid) radical scavenging abilities. Conclusion: These results suggest that triazineamides may be of interest to establish a structural basis for new anti-Alzheimer's disease agents.


Assuntos
Doença de Alzheimer , Antioxidantes , Humanos , Antioxidantes/farmacologia , Antioxidantes/química , Inibidores da Colinesterase/farmacologia , Inibidores da Colinesterase/química , Acetilcolinesterase/metabolismo , Simulação de Acoplamento Molecular , Doença de Alzheimer/tratamento farmacológico , Ácidos Sulfônicos/química , Relação Estrutura-Atividade
4.
Nat Prod Res ; 35(4): 702-706, 2021 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-30942104

RESUMO

The antioxidant effect of 95% ethanol extract and its three subfractions, PE (petroleum ether), EtOAc (ethyl acetate), and water extracts, from Gannanzao navel orange peel, were evaluated by ABTS (2,2'-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid)), DPPH (1,1-diphenyl-2-picryl-hydrazyl) and FRAP (ferric reducing/antioxidant potential) methods for the first time. Furthermore, the TPC (total polyphenol content), TFC (total flavonoid content), and primary individual flavonoids of the four extracts were analyzed and compared. The results indicated that: (1) the EtOAc extract exhibited the best antioxidant potential among these four extracts in all three antioxidant bioassay platforms; (2) Corresponding to the antioxidant potential, the EtOAc extract contained the highest contents of both TPC and TFC; (3) Compared with other extracts, the EtOAc extract was significantly (p < 0.01) rich in the contents of narirutin, sinensetin, nobiletin, 4',5,6,7-tetramethoxyflavone, and 3,3',4',5,6,7-hexamethoxyflavone, which might be the main bioactive compounds responsible for the excellent antioxidant potential of EtOAc extract.


Assuntos
Antioxidantes/farmacologia , Citrus sinensis/química , Flavonoides/análise , Extratos Vegetais/farmacologia , Benzotiazóis/química , Compostos de Bifenilo/química , Cromatografia Líquida de Alta Pressão , Flavonoides/química , Ferro/metabolismo , Oxirredução , Picratos/química , Extratos Vegetais/química , Polifenóis/análise , Ácidos Sulfônicos/química
5.
Int J Biol Macromol ; 168: 775-783, 2021 Jan 31.
Artigo em Inglês | MEDLINE | ID: mdl-33227330

RESUMO

The interaction between biomacromolecules and ligands has attracted great interest because of their biological properties. Calf thymus DNA (ctDNA) can interact with bioactive compounds to form complexes. Here, ctDNA-ligand complexes were studied using fluorescence, absorption, and infrared spectroscopy, circular dichroism, ABTS assay and competitive displacement. The binding constants of bioactive compounds at the intercalative site of ctDNA ranked in order kaempferol > apigenin > quercetin > curcumin > riboflavin, while the binding constants at minor groove sites ranked quercetin > kaempferol > naringenin ~ apigenin > hesperetin > curcumin ~ resveratrol ~ riboflavin > caffeic acid. CtDNA maintained stable B-form with an enhancement of base stacking and a decrease of right-handed helicity in the presence of these bioactive compounds, except for hesperetin and caffeic acid. Bioactive compounds preferentially bound to guanine bases and tended to transfer into a more hydrophobic environment upon complexation with ctDNA. The DNA complexation did not affect the ABTS·+ scavenging capacity of quercetin, kaempferol, resveratrol and apigenin but increased the ones of naringenin, caffeic acid, curcumin, hesperetin and riboflavin. The data gathered here should be useful to understand the binding modes of DNA with ligands for their potential application in pharmaceutical and food industries.


Assuntos
Antioxidantes/farmacologia , DNA/metabolismo , Compostos Fitoquímicos/farmacologia , Animais , Antioxidantes/química , Sítios de Ligação , DNA/química , Indústria Farmacêutica , Indústria Alimentícia , Interações Hidrofóbicas e Hidrofílicas , Compostos Fitoquímicos/química , Ácidos Sulfônicos/química , Tiazóis/química
6.
Molecules ; 25(22)2020 Nov 13.
Artigo em Inglês | MEDLINE | ID: mdl-33202876

RESUMO

Seeking to enrich the yet less explored field of scorpionate complexes bearing antioxidant properties, we, here, report on the synthesis, characterization and assessment of the antioxidant activity of new complexes derived from three scorpionate ligands. The interaction between the scorpionate ligands thallium(I) hydrotris(5-methyl-indazolyl)borate (TlTp4Bo,5Me), thallium(I) hydrotris(4,5-dihydro-2H-benzo[g]indazolyl)borate (TlTpa) and potassium hydrotris(3-tert-butyl- pyrazolyl)borate (KTptBu), and metal(II) chlorides, in dichloromethane at room temperature, produced a new family of complexes having the stoichiometric formula [M(Tp4Bo,5Me)2] (M = Cu, 1; Zn, 4; Cd, 7), [M(Tpa)2] (M = Cu, 2; Zn, 5; Cd, 8), [Cu(HpztBu)3Cl2] (3), [Zn(TptBu)Cl] (6) and [Cd(BptBu)(HpztBu)Cl] (9). The obtained metal complexes were characterized by Fourier transform infrared spectroscopy, proton nuclear magnetic resonance and elemental analysis, highlighting the total and partial hydrolysis of the scorpionate ligand TptBu during the synthesis of the Cu(II) complex 3 and the Cd(II) complex 9, respectively. An assessment of the antioxidant activity of the obtained metal complexes was performed through both enzymatic and non-enzymatic assays against 1,1-diphenyl-2-picryl- hydrazyl (DPPH·), 2,2'-Azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS+·), hydroxyl (HO·), nitric oxide (NO·), superoxide (O2-) and peroxide (OOH·) radicals. In particular, the complex [Cu(Tpa)2]⋅0.5H2O (2) exhibited significant antioxidant activity, as good and specific activity against superoxide (O2-·), (IC50 values equal to 5.6 ± 0.2 µM) and might be identified as auspicious SOD-mimics (SOD = superoxide dismutase).


Assuntos
Antioxidantes/análise , Cádmio/análise , Cobre/análise , Zinco/análise , Benzotiazóis/química , Compostos de Bifenilo/química , Radical Hidroxila/química , Concentração Inibidora 50 , Ligantes , Espectroscopia de Ressonância Magnética , Óxido Nítrico/química , Peróxidos/química , Picratos/química , Espectroscopia de Infravermelho com Transformada de Fourier , Ácidos Sulfônicos/química , Superóxidos/química , Temperatura , Tálio/química
7.
Clin Cancer Res ; 26(15): 3990-3998, 2020 08 01.
Artigo em Inglês | MEDLINE | ID: mdl-32345649

RESUMO

PURPOSE: Incomplete oncologic resections and damage to vital structures during colorectal cancer surgery increases morbidity and mortality. Moreover, neoadjuvant chemoradiotherapy has become the standard treatment modality for locally advanced rectal cancer, where subsequent downstaging can make identification of the primary tumor more challenging during surgery. Near-infrared (NIR) fluorescence imaging can aid surgeons by providing real-time visualization of tumors and vital structures during surgery. EXPERIMENTAL DESIGN: We present the first-in-human clinical experience of a novel NIR fluorescent peptide, cRGD-ZW800-1, for the detection of colon cancer. cRGD-ZW800-1 was engineered to have an overall zwitterionic chemical structure and neutral charge to lower nonspecific uptake and thus background fluorescent signal. We performed a phase I study in 11 healthy volunteer as well as a phase II feasibility study in 12 patients undergoing an elective colon resection, assessing 0.005, 0.015, and 0.05 mg/kg cRGD-ZW800-1 for the intraoperative visualization of colon cancer. RESULTS: cRGD-ZW800-1 appears safe, and exhibited rapid elimination into urine after a single low intravenous dose. Minimal invasive intraoperative visualization of colon cancer through full-thickness bowel wall was possible after an intravenous bolus injection of 0.05 mg/kg at least 2 hours prior to surgery. Longer intervals between injection and imaging improved the tumor-to-background ratio. CONCLUSIONS: cRGD-ZW800-1 enabled fluorescence imaging of colon cancer in both open and minimal invasive surgeries. Further development of cRGD-ZW800-1 for widespread use in cancer surgery may be warranted given the ubiquitous overexpression of various integrins on different types of tumors and their vasculature.


Assuntos
Carcinoma/diagnóstico , Colo/diagnóstico por imagem , Neoplasias do Colo/diagnóstico , Corantes Fluorescentes/administração & dosagem , Imagem Óptica/métodos , Idoso , Idoso de 80 Anos ou mais , Animais , Carcinoma/patologia , Carcinoma/terapia , Quimiorradioterapia Adjuvante , Colectomia/métodos , Colo/patologia , Colo/cirurgia , Neoplasias do Colo/patologia , Neoplasias do Colo/terapia , Estudos de Viabilidade , Feminino , Corantes Fluorescentes/efeitos adversos , Corantes Fluorescentes/química , Corantes Fluorescentes/farmacocinética , Voluntários Saudáveis , Humanos , Integrinas/metabolismo , Masculino , Camundongos , Pessoa de Meia-Idade , Terapia Neoadjuvante , Imagem Óptica/efeitos adversos , Peptídeos Cíclicos/administração & dosagem , Peptídeos Cíclicos/efeitos adversos , Peptídeos Cíclicos/química , Peptídeos Cíclicos/farmacocinética , Compostos de Amônio Quaternário/administração & dosagem , Compostos de Amônio Quaternário/efeitos adversos , Compostos de Amônio Quaternário/química , Compostos de Amônio Quaternário/farmacocinética , Ratos , Espectroscopia de Luz Próxima ao Infravermelho/métodos , Ácidos Sulfônicos/administração & dosagem , Ácidos Sulfônicos/efeitos adversos , Ácidos Sulfônicos/química , Ácidos Sulfônicos/farmacocinética , Testes de Toxicidade Aguda
8.
Biomolecules ; 9(5)2019 05 08.
Artigo em Inglês | MEDLINE | ID: mdl-31072044

RESUMO

The anticancer activity of acridone derivatives has attracted increasing interest, therefore, a variety of substituted analogs belonging to this family have been developed and evaluated for their anti-cancer properties. A series of N-alkyl-acridones 1-6 and N,N'-dialkyl-9,9'-biacridylidenes 7-12 with variable alkyl chains were examined for their topoisomerase I activity at neutral and acidic conditions as well as for their binding capacity to calf thymus and possible radical trapping antioxidant activity. It was found that at a neutral pH, topoisomerase I activity of both classes of compounds was similar, while under acidic conditions, enhanced intercalation was observed. N-alkyl-acridone derivatives 1-6 exhibited stronger, dose-dependent, cytotoxic activity against MCF-7 human breast epithelial cancer cells than N,N'-dialkyl-9,9'-biacridylidenes 7-12, revealing that conjugation of the heteroaromatic system plays a significant role on the effective distribution of the compound in the intracellular environment. Cellular investigation of long alkyl derivatives against cell migration exhibited 40-50% wound healing effects and cytoplasm diffusion, while compounds with shorter alkyl chains were accumulated both in the nucleus and cytoplasm. All N,N'-dialkyl-9,9'-biacridylidenes showed unexpected high scavenging activity towards DPPH or ABTS radicals which may be explained by higher stabilization of radical cations by the extended conjugation of heteroaromatic ring system.


Assuntos
Acridinas/farmacologia , Acridonas/farmacologia , Neoplasias da Mama/patologia , DNA Topoisomerases Tipo I/metabolismo , Sequestradores de Radicais Livres/farmacologia , Acridinas/química , Acridonas/química , Benzotiazóis/química , Compostos de Bifenilo/química , Sobrevivência Celular/efeitos dos fármacos , DNA/metabolismo , Feminino , Humanos , Células MCF-7 , Picratos/química , Ácidos Sulfônicos/química , Cicatrização/efeitos dos fármacos
9.
Bioengineered ; 9(1): 90-97, 2018 Jan 01.
Artigo em Inglês | MEDLINE | ID: mdl-28662363

RESUMO

The effectiveness and economics of polyvinyl sulfonic acid (PVSA) as a ribonuclease inhibitor for in vitro systems is reported. PVSA was shown to inhibit RNA cleavage in the presence of RNase A as well as in the presence of Escherichia coli lysate, suggesting that PVSA can act as a broader ribonuclease inhibitor. In addition, PVSA was shown to improve the integrity of mRNA transcripts by up to 5-fold in vitro as measured by their translational viability. Improved preservation of mRNA transcripts in the presence of PVSA under common RNA storage conditions is also reported. A cost comparison with commercially available RNAse inhibitors indicates the economic practicality of PVSA which is approximately 1,700 times less expensive than commonly used ribonuclease inhibitors. PVSA can also be separated from RNA by alcohol precipitation for applications that may be sensitive to the presence of PVSA.


Assuntos
Proteínas de Bactérias/antagonistas & inibidores , Inibidores Enzimáticos/farmacologia , Polivinil/farmacologia , Biossíntese de Proteínas , RNA Mensageiro/metabolismo , Ribonucleases/antagonistas & inibidores , Ácidos Sulfônicos/farmacologia , Proteínas de Bactérias/genética , Proteínas de Bactérias/metabolismo , Ensaios Enzimáticos , Inibidores Enzimáticos/química , Inibidores Enzimáticos/economia , Escherichia coli/enzimologia , Escherichia coli/genética , Cinética , Polivinil/química , Polivinil/economia , Estabilidade de RNA , RNA Mensageiro/química , RNA Mensageiro/genética , Ribonucleases/genética , Ribonucleases/metabolismo , Frações Subcelulares/metabolismo , Ácidos Sulfônicos/química , Ácidos Sulfônicos/economia , Transcrição Gênica
10.
Nanoscale ; 8(10): 5488-96, 2016 Mar 14.
Artigo em Inglês | MEDLINE | ID: mdl-26902537

RESUMO

Rapid detection of sarcosine is a key requirement for both diagnosis and treatment of disease. We report here a simple yet sensitive colorimetric nanocomposite platform for rapid detection of sarcosine in alkaline media. The approach exploited the benefits of a rapid color-producing reaction between an organic indicator, 1,2-naphthoquinone-4-sulphonic acid sodium salt (NQS), and the analyte of sarcosine species as well as the good catalytic ability of graphene oxide (GO) to the formation of highly colored products due to its good water dispersibility, extremely large surface area and facile surface modification. As a result, a NQS functionalized GO nanocomposite through π-π stacking has been demonstrated to be useful as a highly efficient catalyst system for the selective and sensitive colorimetric determination of sarcosine by providing a nanocomposite-amplified colorimetric response. Meanwhile, the strategy offered excellent selectivity toward sarcosine species against other amino acids as well as a satisfying detection limit of 0.73 µM. More importantly, by using an electrochemical method, a credible sensing mechanism of GO nanocomposite-based colorimetric platform for a special analyte determination can be easily verified and elucidated, which also provides an attractive alternative to conventional characterization strategies.


Assuntos
Colorimetria/métodos , Grafite/química , Nanopartículas Metálicas/química , Nanocompostos/química , Óxidos/química , Sarcosina/análise , Catálise , Análise Custo-Benefício , Eletroquímica , Concentração de Íons de Hidrogênio , Nanotecnologia , Naftoquinonas/química , Solubilidade , Ácidos Sulfônicos/química
11.
Mol Imaging ; 142015.
Artigo em Inglês | MEDLINE | ID: mdl-25812603

RESUMO

Hematoxylin-eosin (H&E) staining of tissue has been the mainstay of pathology for more than a century. However, the learning curve for H&E tissue interpretation is long, whereas intra- and interobserver variability remain high. Computer-assisted image analysis of H&E sections holds promise for increased throughput and decreased variability but has yet to demonstrate significant improvement in diagnostic accuracy. Addition of biomarkers to H&E staining can improve diagnostic accuracy; however, coregistration of immunohistochemical staining with H&E is problematic as immunostaining is completed on slides that are at best 4 µm apart. Simultaneous H&E and immunostaining would alleviate coregistration problems; however, current opaque pigments used for immunostaining obscure H&E. In this study, we demonstrate that diagnostic information provided by two or more independent wavelengths of near-infrared (NIR) fluorescence leave the H&E stain unchanged while enabling computer-assisted diagnosis and assessment of human disease. Using prostate cancer as a model system, we introduce NIR digital pathology and demonstrate its utility along the spectrum from prostate biopsy to whole mount analysis of H&E-stained tissue.


Assuntos
Diagnóstico por Computador , Espectroscopia de Luz Próxima ao Infravermelho , Biomarcadores/metabolismo , Biópsia , Humanos , Imuno-Histoquímica , Masculino , Neoplasias da Próstata/diagnóstico , Neoplasias da Próstata/patologia , Compostos de Amônio Quaternário/química , Espectrometria de Fluorescência , Espectrofotometria Ultravioleta , Ácidos Sulfônicos/química
12.
Water Sci Technol ; 70(6): 1056-64, 2014.
Artigo em Inglês | MEDLINE | ID: mdl-25259495

RESUMO

Photo-Fenton-like treatment of the commercially important naphthalene sulphonate K-acid (2-naphthylamine-3,6,8-trisulphonic acid) was investigated using UV-C, UV-A and visible light irradiation. Changes in toxicity patterns were followed by the Vibrio fischeri bioassay. Rapid and complete degradation of K-acid accompanied with nearly complete oxidation and mineralization rates (>90%) were achieved for all studied irradiation types. On the other hand, detoxification was rather limited and did not change significantly during photo-Fenton-like treatment. Several oxidation products could be identified via liquid chromatograph-mass spectrometer analyses, such as desulphonated and hydroxylated naphthalene derivatives, quinones, and ring-opening as well as dimerization products. Photo-Fenton-like treatment of K-acid with UV-C, UV-A and visible light irradiation occurred through a series of hydroxylation and desulphonation reactions, followed by ring cleavage. A common degradation pathway for photo-Fenton-like treatment of K-acid using different irradiation types was proposed.


Assuntos
2-Naftilamina/análogos & derivados , Ácidos Sulfônicos/química , Eliminação de Resíduos Líquidos/métodos , Poluentes Químicos da Água/química , 2-Naftilamina/química , Aliivibrio fischeri , Peróxido de Hidrogênio , Estrutura Molecular , Oxirredução , Raios Ultravioleta
13.
J Chromatogr A ; 1355: 73-9, 2014 Aug 15.
Artigo em Inglês | MEDLINE | ID: mdl-24997109

RESUMO

Two ionization techniques for liquid chromatography-mass spectrometry (LC-MS) determination of sulfonate ester potentially genotoxic impurities (PGIs) were evaluated. Twelve PGIs including methyl, ethyl, propyl and isopropyl esters of methanesulfonate, benzenesulfonate and p-toluenesulfonate were studied in this research. Electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI) sources were compared in terms of performance and quality parameters for detection of the twelve PGIs. Their mass spectra obtained by APCI and ESI were very different in both fragment ions and relative abundances. In APCI negative ion mode the twelve sulfonate esters showed their stable precursor ions of [M-alkyl](-), which readily yielded product ions of [M-alkyl-CH3](-) (for aliphatic sulfonate esters) or [M-alkyl-SO2](-) (for aromatic sulfonate esters) with collision-induced dissociation (CID) applied; and working in selected reaction monitoring (SRM) mode has allowed limits of detection to be decreased. In the case of ESI ionization, these compounds showed their precursor ions [M+H](+), but their abundance was easily competed by formation of ions [M+NH4](+) and/or [M+Na](+), which led to poor analytical sensitivity and reproducibility. Although mobile phase additives could enhance the responses of adduct ions like [M+NH4](+) and [M+Na](+), no improvement was obtained when using SRM mode. Twelve sulfonate esters were systematically compared and APCI was shown to be a better ionization technique for rapid and sensitive determination of these PGIs. Performance of the developed approach for rapid determination of 12 PGIs was also evaluated. Quality parameters were established and good precision (relative standard deviations <8%) and very low limits (2-4ng/mL) of detection were obtained, mainly when using APCI in SRM mode.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Ésteres/química , Mutagênicos/isolamento & purificação , Ácidos Sulfônicos/isolamento & purificação , Espectrometria de Massas em Tandem/métodos , Cátions/química , Cromatografia Líquida de Alta Pressão/instrumentação , Mutagênicos/química , Reprodutibilidade dos Testes , Ácidos Sulfônicos/química , Espectrometria de Massas em Tandem/instrumentação , Fatores de Tempo
14.
Anal Chim Acta ; 818: 1-6, 2014 Mar 25.
Artigo em Inglês | MEDLINE | ID: mdl-24626396

RESUMO

Drug purity and affinity are essential attributes during development and production of therapeutic proteins. In this work, capillary electrophoresis (CE) was used to determine both the affinity and composition of the biotechnologically produced "nanobody" EGa1, the binding fragment of a heavy-chain-only antibody. EGa1 is an antagonist of the epidermal growth factor receptor (EGFR), which is overexpressed on the surface of tumor cells. Using a background electrolyte (BGE) of 50mM sodium phosphate (pH 8.0) in combination with a polybrene-poly(vinylsulfonic acid) capillary coating, CE analysis of EGa1 showed the presence of at least three components. Affinity of the EGa1 components towards the extracellular domain of EGFR was assessed by adding different concentrations (0-12 nM) of the receptor to the BGE while measuring the effective electrophoretic mobility of the respective EGa1 components. Binding curves obtained by plotting electrophoretic mobility shifts as a function of receptor concentration, yielded dissociation constants (Kd) of 1.65, 1.67, and 1.75 nM for the three components, respectively; these values were comparable to the Kd of 2.1 nM obtained for the bulk EGa1 product using a cellular assay. CE with mass spectrometry (MS) detection using a BGE of 25 mM ammonium acetate (pH 8.0) revealed that the EGa1 sample comprised of significant amounts of deamidated, bisdeamidated and N-terminal pyroglutamic acid products. CE-MS using a BGE of 100mM acetic acid (pH 2.8) in combination with a polybrene-dextran sulfate-polybrene capillary coating demonstrated the additional presence of minor products related to incomplete removal of the signal peptide from the produced nanobody. Combining the results obtained from affinity CE and CE-MS, it is concluded that the EGa1 nanobody product is heterogeneous, comprising highly-related proteins that exhibit very similar affinity towards EGFR.


Assuntos
Técnicas de Química Analítica/métodos , Eletroforese Capilar , Anticorpos de Domínio Único/análise , Acetatos/química , Ácido Acético/química , Sequência de Aminoácidos , Sulfato de Dextrana/química , Receptores ErbB/antagonistas & inibidores , Receptores ErbB/imunologia , Brometo de Hexadimetrina/química , Cinética , Espectrometria de Massas , Dados de Sequência Molecular , Fosfatos/química , Polivinil/química , Anticorpos de Domínio Único/imunologia , Anticorpos de Domínio Único/metabolismo , Ácidos Sulfônicos/química
15.
Colloids Surf B Biointerfaces ; 107: 1-10, 2013 Jul 01.
Artigo em Inglês | MEDLINE | ID: mdl-23466536

RESUMO

A unique silane based adsorbent material, [stearyl alcohol (SA)-grafted-epichlorohydrin (E)]-grafted-aminoproypyl silanetriol (APST) was synthesized and functionalized with sulphonyl groups via sulphonation process [(SA-g-E)-g-APST/SO3H]. The adsorbent material characterization was done by FTIR, XRD, and TGA analysis. Immobilization of protein Lysozyme (LYZ) using batch adsorption process was carried out for studying the protein-particle interaction. The most suitable pH for maximum adsorption was found to be 7.0. Pseudo-second-order kinetic model was found to be the best fit and the adsorption equilibrium was attained within 3h. Studies on diffusion parameters explained that the adsorption mechanism was controlled by film diffusion mode. The adsorption process was then evaluated using the various isotherm models and the Sips isotherm model proved to be the best fit with a maximum adsorption capacity of 37.68 mg/g. The isotherm favorability of the adsorption process was calculated by calculating the separation factor (R(L)) and the values confirmed the favorability of the adsorption process. Studies on adsorption percentage with respect to temperature and thermodynamic studies revealed that adsorption process is exothermic, spontaneous with maximum entropy. Batch adsorption/desorption studies in acidic medium, for over six cycles showed the repeatability and regeneration capability of the adsorbent material (SA-g-E)-g-APST/SO3H.


Assuntos
Enzimas Imobilizadas/metabolismo , Muramidase/metabolismo , Polímeros/química , Silanos/química , Ácidos Sulfônicos/química , Adsorção , Custos e Análise de Custo , Difusão , Epicloroidrina/química , Concentração de Íons de Hidrogênio , Cinética , Reprodutibilidade dos Testes , Espectroscopia de Infravermelho com Transformada de Fourier , Temperatura , Termogravimetria , Difração de Raios X
16.
Artigo em Inglês | MEDLINE | ID: mdl-23041925

RESUMO

New, simple and rapid spectrophotometric method has been developed and validated for the assay of two macrolide drugs, azithromycin (AZT) and erythromycin (ERY) in pure and pharmaceutical formulations. The proposed method was based on the reaction of AZT and ERY with sodium 1,2-naphthoquinone-4-sulphonate (NQS) in alkaline medium at 25 °C to form an orange-colored product of maximum absorption peak at 452 nm. All variables were studied to optimize the reaction conditions and the reaction mechanism was postulated. Beer's law was obeyed in the concentration range 1.5-33.0 and 0.92-8.0 µg mL(-1) with limit of detection values of 0.026 and 0.063 µg mL(-1) for AZT and ERY, respectively. The calculated molar absorptivity values are 4.3 × 10(4) and 12.3 × 10(4) L mol(-1) cm(-1) for AZT and ERY, respectively. The proposed methods were successfully applied to the determination of AZT and ERY in formulations and the results tallied well with the label claim. The results were statistically compared with those of an official method by applying the Student's t-test and F-test. No interference was observed from the concomitant substances normally added to preparations.


Assuntos
Antibacterianos/análise , Azitromicina/análise , Eritromicina/análise , Naftoquinonas/química , Preparações Farmacêuticas/química , Espectrofotometria/métodos , Corantes/química , Limite de Detecção , Espectrofotometria/economia , Ácidos Sulfônicos/química
17.
J Agric Food Chem ; 60(38): 9573-80, 2012 Sep 26.
Artigo em Inglês | MEDLINE | ID: mdl-22950743

RESUMO

Hydrogen peroxide scavenging (HPS) activity of unfermented (green, yellow, and white), partially fermented (oolong), and completely fermented (black) tea ( Camellia sinensis ), maté ( Ilex paraguariensis ), and various herbal infusions, as well as individual compounds (flavan-3-ols, flavonols, cinnamic and benzoic acids, and methylxanthines), was assessed by recently developed direct current (DC) polarographic assay. Correlations of tea and herbal infusion HPS activity with total phenolic content determined using the Folin-Ciocalteu assay (FC-GAE) (0.81 and 0.93), ferric reducing/antioxidant power (FRAP) (0.97 and 0.92), 1,1-diphenyl-2-picrylhydrazyl (DPPH) (0.77 and 0.80), and 2,2'-azinobis(3-ethylbenzthiazoline-6-sulfonic acid) (ABTS) scavenging (0.86 and 0.86) were statistically significant. Correlations between relative antioxidant capacity index (RACI), calculated by assigning all applied assays equal weight, and HPS (0.98), FRAP (0.97), ABTS (0.89), and DPPH (0.89) confirmed DC polarographic assay reliability when applied individually. Correlation analysis, ANOVA, and Levene and Tukey's HSD tests unequivocally confirmed this reliable, rapid, and low-cost assay validity, clearly demonstrating its advantages over spectrophotometric assays applied.


Assuntos
Antioxidantes/análise , Bebidas/análise , Polarografia/métodos , Chá/química , Ácido Benzoico/análise , Benzotiazóis/química , Compostos de Bifenilo/química , Camellia sinensis/química , Cinamatos/análise , Flavonóis/análise , Sequestradores de Radicais Livres/análise , Sequestradores de Radicais Livres/química , Peróxido de Hidrogênio/análise , Ilex paraguariensis/química , Fenóis/análise , Picratos/química , Reprodutibilidade dos Testes , Ácidos Sulfônicos/química , Xantinas/análise , Xantinas/química
18.
J Environ Manage ; 99: 44-51, 2012 May 30.
Artigo em Inglês | MEDLINE | ID: mdl-22318240

RESUMO

The commercially important naphthalene sulfonate K-acid (C(10)H(9)NO(9)S(3); 2-naphthylamine 3,6,8-tri sulfonic acid) was subjected to electrocoagulation employing stainless steel electrodes. An experimental design tool was used to mathematically describe and optimize the single and combined influences of major process variables on K-acid and its organic carbon (COD and TOC) removal efficiencies as well as electrical energy consumption. Current density, followed by treatment time were found to be the parameters affecting process responses most significantly, whereas initial K-acid concentration had the least influence on the electrocoagulation performance. Process economics including sludge generation, electrode consumption, and electrochemical efficiency, as well as organically bound adsorbable halogen formation and toxicity evolution were primarily considered to question the feasibility of K-acid electrocoagulation. Considering process economics and ecotoxicological parameters, process implementation appeared to be encouraging.


Assuntos
2-Naftilamina/análogos & derivados , Técnicas Eletroquímicas , Poluição Ambiental/prevenção & controle , Ácidos Sulfônicos/química , 2-Naftilamina/química , Modelos Químicos , Análise de Regressão
19.
Rapid Commun Mass Spectrom ; 25(13): 1801-11, 2011 Jul 15.
Artigo em Inglês | MEDLINE | ID: mdl-21638355

RESUMO

The structural elucidation of carbonyl-containing by-products arising from Uniblu-OH ozonation has been investigated by liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) employing a quadrupole time-of-flight mass spectrometer. The by-products were derivatized with 2,4-dinitrophenylhydrazine, allowing the formation of [M-H](-) ions of the derivatives in the electrospray source. Exact mass measurements of both the [M-H](-) ions and their product ions allowed the elemental formulae and related structures of ten by-products to be determined confidently. The main degradation pathway were decarboxylation followed by further oxidation. It is noteworthy that the experimental procedure employed allowed the identification of both nitrogen- and sulphur-containing carbonyl by-products during Uniblu-OH ozonation. This result is of environmental relevance for monitoring the balance of organic nitrogen and sulphur during the ozonation of organic pollutants. These atoms, in fact, do not undergo complete mineralization.


Assuntos
Antraquinonas/química , Corantes/química , Espectrometria de Massas por Ionização por Electrospray/métodos , Ácidos Sulfônicos/química , Hidrazinas , Íons , Peso Molecular , Oxirredução , Indústria Têxtil , Poluentes Químicos da Água
20.
Talanta ; 84(5): 1350-4, 2011 Jun 15.
Artigo em Inglês | MEDLINE | ID: mdl-21641450

RESUMO

This work presents a new flow-based coupled electrochemical technique for evaluation of "total antioxidant capacity (TAC)". A sequential injection (SI) with amperometric detection was applied to the TAC analysis of commercial instant ginger infusion beverages using 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) assay. Besides having chromogenic properties, the ABTS reagent behaves as an electroactive species at the glassy carbon electrode in phosphate buffer pH 7.0, the decrease of the cathodic current signal of the ABTS(+) radical after reaction with antioxidants can be monitored. The SI system, furnished with an in-house electrochemical detection cell (ECD), was optimized with respect to the applied potential, sample and reagent volume, and flow rate to the detector. Gallic acid was used as the standard antioxidant and the capacity was reported as gallic acid equivalent (GAE) unit. TAC measurements of ginger infusions at the optimum condition were performed using the proposed technique and also with the classical batch spectrophotometric ABTS assay. TAC values obtained from our method and the standard method are in good agreement (r(2)=0.956). The SI-amperometric technique provided satisfactory precision (4.11% RSD) with rapid sample throughput (40 samples h(-1)). Also using this method, the consumption of the expensive ABTS reagent was greatly reduced.


Assuntos
Eletroquímica/economia , Eletroquímica/métodos , Análise de Injeção de Fluxo/economia , Análise de Injeção de Fluxo/métodos , Sequestradores de Radicais Livres/análise , Sequestradores de Radicais Livres/química , Benzotiazóis/análise , Benzotiazóis/química , Bebidas/análise , Ácido Gálico/análise , Ácido Gálico/química , Zingiber officinale/química , Indicadores e Reagentes/química , Ácidos Sulfônicos/análise , Ácidos Sulfônicos/química , Fatores de Tempo
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