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1.
Angiol Sosud Khir ; 26(3): 45-52, 2020.
Artigo em Russo | MEDLINE | ID: mdl-33063751

RESUMO

AIM: This study was undertaken to evaluate the efficacy of three-stage measurement of the transit-time flow through coronary bypass grafts with the help of flowmetry for early verification of technical errors during on-pump coronary artery bypass graft surgery. PATIENTS AND METHODS: We performed an intraoperative analysis of 214 bypass grafts with the help of three-stage flowmetry. The first stage of measuring was performed on-pump with and without the proximal loop test, the second stage of measurement was performed after weaning the patient off the heart-lung machine, and the third stage of measurement was carried out after heparin inactivation prior to chest wound closure. RESULTS: Amongst the 214 transplants regarded as functioning, intraoperative flowmetry revealed insufficient blood flow in 9 (4.2%) cases. Technical surgical errors were confirmed in these shunts during revision thereof. In 6 (2.8%) of the 9 such grafts we detected non-optimal parameters of flowmetry during the first measurement (while the heart was stopped); of these, in 5 (2.3%) cases non-optimal blood flow was verified with the use of the proximal loop test on the target coronary artery and in 1 (0.47%) case without it. In another one (0.47%) of the nine such transplants, inadequate blood flow was revealed during the second measurement, which confirmed technical errors in proximal anastomoses. In a further 2 (0.93%) of the 9 such transplants we observed low parameters of blood flow during the third measurement, which was related to kinking of the shunts due to their excessive length. All surgical errors were corrected immediately at the stage of verification thereof. CONCLUSION: The strategy of three-stage assessment of flowmetry makes it possible to ensure and confirm adequate functionality of coronary artery bypass grafts at all stages of the operation, thus allowing timely verification and immediate correction of any technical problems with coronary artery bypass grafts.


Assuntos
Ponte de Artéria Coronária , Vasos Coronários , Anastomose Cirúrgica , Humanos , Reologia
2.
Annu Int Conf IEEE Eng Med Biol Soc ; 2020: 2342-2345, 2020 07.
Artigo em Inglês | MEDLINE | ID: mdl-33018477

RESUMO

Resistant hypertension (RH) is a major healthcare issue, causing cardiovascular and cerebrovascular diseases. In recent years, radiofrequency (RF) ablation to renal sympathetic denervation (RSD) is a new effective method for the treatment of RH. However, the effect of RSD on renal artery blood flow still need further research. In this study, Particle Image Velocimetry (PIV) experiment and RF ablation experiment were used to observe the blood flow states in three conditions: no ablation with flow, ablation with no flow, and ablation with flow. The results showed that when the blood flow was 1L/min in renal artery without ablation, it was uniform laminar flow. When the blood was static in renal artery with ablation, there was eddy around the ablation catheter. When the blood flow was 1L/min in renal artery with ablation, the eddy disappeared and the blood flow was uniform laminar flow. Therefore, when the renal artery blood flow is 1L/min, there will be no thrombus and hemolysis in the renal artery due to eddy current and large velocity gradient, which preliminarily verified the safety of the RSD. Keyword: Resistant hypertension; Radiofrequency ablation; Flow field; PIVClinical relevance-When the blood flow of renal artery is 1L/min, there will be no thrombus and hemolysis in renal artery due to eddy current and large velocity gradient during the operation of RF ablation to renal sympathetic denervation.


Assuntos
Ablação por Cateter , Rim , Rim/cirurgia , Artéria Renal/cirurgia , Reologia , Simpatectomia
3.
Annu Int Conf IEEE Eng Med Biol Soc ; 2020: 2496-2499, 2020 07.
Artigo em Inglês | MEDLINE | ID: mdl-33018513

RESUMO

The small intestine is the primary site of enzymatic digestion and nutrient absorption in humans. Intestinal contractions facilitate digesta mixing, transport and contact with the absorptive surfaces. These motility patterns are regulated by an underlying electrical activity, termed slow waves. In this study, we use computational fluid dynamics simulation of flow and mixing of intestinal contents in the human duodenum with anatomically realistic geometry and contraction patterns. Parameters including the amplitude of contraction (10-50% reduction of radius) and the rheology of the digesta (Newtonian vs Non-Newtonian power law fluid) were altered in-order to study their effects on mixing. Interesting flow features such as stagnation points and reversed flow were observed with digesta. Increases in the amplitude of contraction lead to increased propulsion of digesta along the intestine and increased mixing.


Assuntos
Duodeno , Intestino Delgado , Conteúdo Gastrointestinal , Humanos , Intestinos , Reologia
4.
Water Res ; 182: 116031, 2020 Sep 01.
Artigo em Inglês | MEDLINE | ID: mdl-32810736

RESUMO

Recent reports and experimental data closely indicate that bed-sediment entrainment by debris flows strongly impacts the evolution of the topographic signature of a valley. However, it is difficult to constrain the physics of the entrainment process in numerical models. The challenge is deeply embedded in the shape of the velocity profile, whose knowledge is fundamental for estimating debris-flow basal shear stress exerting on bed sediment. Most two-dimensional models are restricted because the depth-integrated shallow water assumption is problematic in this aspect. One alternative is to combine a three-dimensional, particle-based numerical model with a progressive entrainment law. In this paper, we propose a three-dimensional, surface cell (SC)-based smooth particle hydrodynamics (SPH) model for simulating bed-sediment entrainment by viscous debris flows. The dynamic behavior of a debris flow is simulated by the open-source DualSPHysics scheme, into which the Herschel-Bulkley-Papanastasiou (HBP) rheology model is incorporated. Subsequently, the bed surface is meshed, over which the particles belonging to a certain cell at each time step are identified to represent the basal velocity and flow depth using a novel SC-based algorithm. With the extracted velocities of these basal particles, the sediment entrainment rate of each cell can be estimated using the optimized progressive entrainment law. The proposed SC-HBP-SPH method is tested by means of a full-scale flume experiment carried out in a previous study. The results show that the proposed model can adequately describe and reproduce the complex dynamic process of bed-sediment entrainment by overriding debris flows.


Assuntos
Hidrodinâmica , Movimentos da Água , Sedimentos Geológicos , Reologia , Viscosidade
5.
Medicine (Baltimore) ; 99(34): e21914, 2020 Aug 21.
Artigo em Inglês | MEDLINE | ID: mdl-32846858

RESUMO

We aimed to evaluate the accuracy and interchangeability of stroke volume and cardiac output measured by electrical velocimetry and transthoracic echocardiography during cesarean delivery.We enrolled 20 parturients in this prospective observational study. We recorded the stroke volume and cardiac output using both methods and compared the values at seven specific time points. We analyzed the data using linear regression analysis for Pearson's correlation coefficients and Bland-Altman analysis to determine percentage errors. We conducted a trending ability analysis based on the four-quadrant plot with the concordance rate and correlation coefficient.We recorded 124 paired datasets during cesarean delivery. The correlation coefficients of the measured cardiac output and stroke volume between the two methods were 0.397 (P < .001) and 0.357 (P < .001). The 95% limits of agreement were -1.0 to 8.1 L min for cardiac output and -10.4 to 90.4 ml for stroke volume. Moreover, the corresponding percentage errors were 62% and 60%. The concordance correlation coefficients were 0.447 (95% CI: 0.313-0.564) for stroke volume and 0.562 (95% CI: 0.442-0.662) for cardiac output. Both methods showed a moderate trending ability for stroke volume (concordance rate: 82% (95% CI: 72-90%)) and cardiac output (concordance rate: 85% (95% CI: 78-93%)).Our findings indicated that electrical velocimetry monitoring has limited accuracy, precision, and interchangeability with transthoracic echocardiography; however, it had a moderate trending ability for stroke volume and cardiac output measurements during cesarean delivery.


Assuntos
Débito Cardíaco , Cesárea/métodos , Ecocardiografia/métodos , Reologia/métodos , Adulto , Algoritmos , China/epidemiologia , Confiabilidade dos Dados , Ecocardiografia/estatística & dados numéricos , Feminino , Hemodinâmica , Humanos , Monitorização Intraoperatória/instrumentação , Gravidez , Estudos Prospectivos , Reologia/estatística & dados numéricos , Volume Sistólico
6.
Phys Rev Lett ; 125(6): 068101, 2020 Aug 07.
Artigo em Inglês | MEDLINE | ID: mdl-32845697

RESUMO

Shape, dynamics, and viscoelastic properties of eukaryotic cells are primarily governed by a thin, reversibly cross-linked actomyosin cortex located directly beneath the plasma membrane. We obtain time-dependent rheological responses of fibroblasts and MDCK II cells from deformation-relaxation curves using an atomic force microscope to access the dependence of cortex fluidity on prestress. We introduce a viscoelastic model that treats the cell as a composite shell and assumes that relaxation of the cortex follows a power law giving access to cortical prestress, area-compressibility modulus, and the power law exponent (fluidity). Cortex fluidity is modulated by interfering with myosin activity. We find that the power law exponent of the cell cortex decreases with increasing intrinsic prestress and area-compressibility modulus, in accordance with previous finding for isolated actin networks subject to external stress. Extrapolation to zero tension returns the theoretically predicted power law exponent for transiently cross-linked polymer networks. In contrast to the widely used Hertzian mechanics, our model provides viscoelastic parameters independent of indenter geometry and compression velocity.


Assuntos
Actinas/química , Fibroblastos/química , Fibroblastos/citologia , Modelos Biológicos , Actinas/fisiologia , Animais , Fenômenos Biomecânicos , Linhagem Celular , Membrana Celular/química , Membrana Celular/fisiologia , Força Compressiva , Cães , Elasticidade , Microscopia de Força Atômica , Miosinas/química , Miosinas/fisiologia , Reologia/métodos , Viscosidade
7.
Wiad Lek ; 73(4): 696-699, 2020.
Artigo em Inglês | MEDLINE | ID: mdl-32731699

RESUMO

OBJECTIVE: The aim of the present research was to investigate the rheological properties of the medicinal syrup for oral administration with glucosamine hydrochloride and levocarnitine. PATIENTS AND METHODS: Matherials and methods: Coefficient of the dynamic flow (at shear rates of 3,49 and 10,3 s -1, as well as at shear rates of 27.2 and 149.0 s-1), mechanical stability, the index of destruction and restoration were studied. The rheological (structural-mechanical) properties of the samples were determined using a Rheolab QC rotary viscometer (AntonPaar, Austria) with coaxial cylinders CC27 / S-SN29766. The rheological parameters were studied at the temperature 20±0,5 °Ð¡. RESULTS: Results: It is established that the syrup has weakly expressed plastic viscous and thixotropic properties (the hysteresis area for the syrupis 1710.19 Pas/s). Such results characterize the system as a reopex. CONCLUSION: Conclusions: The results of the study enables classification of the research object as system with a low degree of fluidity. Such dependence is typical for systems of the Newtonian type of flow and characterizes the syrup under investigation as a weakly structured disperse system.


Assuntos
Reologia , Administração Oral , Viscosidade
8.
Nat Commun ; 11(1): 4193, 2020 08 21.
Artigo em Inglês | MEDLINE | ID: mdl-32826921

RESUMO

Photochemical reactions are a powerful tool in (bio)materials design due to the spatial and temporal control light can provide. To extend their applications in biological setting, the use of low-energy, long wavelength light with high penetration propertiesis required. Further regulation of the photochemical process by additional stimuli, such as pH, will open the door for construction of highly regulated systems in nanotechnology- and biology-driven applications. Here we report the green light induced [2+2] cycloaddition of a halochromic system based on a styrylquinoxaline moiety, which allows for its photo-reactivity to be switched on and off by adjusting the pH of the system. Critically, the [2+2] photocycloaddition can be activated by green light (λ up to 550 nm), which is the longest wavelength employed to date in catalyst-free photocycloadditions in solution. Importantly, the pH-dependence of the photo-reactivity was mapped by constant photon action plots. The action plots further indicate that the choice of solvent strongly impacts the system's photo-reactivity. Indeed, higher conversion and longer activation wavelengths were observed in water compared to acetonitrile under identical reaction conditions. The wider applicability of the system was demonstrated in the crosslinking of an 8-arm PEG to form hydrogels (ca. 1 cm in thickness) with a range of mechanical properties and pH responsiveness, highlighting the potential of the system in materials science.


Assuntos
Reação de Cicloadição/métodos , Hidrogéis/química , Luz , Processos Fotoquímicos , Animais , Catálise , Sobrevivência Celular , Fibroblastos , Concentração de Íons de Hidrogênio , Camundongos , Fótons , Polímeros/química , Reologia
9.
Virus Res ; 288: 198129, 2020 10 15.
Artigo em Inglês | MEDLINE | ID: mdl-32822689

RESUMO

The COVID-19 pandemic caused by SARS-CoV-2 affects all aspects of human life. Detection platforms that are efficient, rapid, accurate, specific, sensitive, and user friendly are urgently needed to manage and control the spread of SARS-CoV-2. RT-qPCR based methods are the gold standard for SARS-CoV-2 detection. However, these methods require trained personnel, sophisticated infrastructure, and a long turnaround time, thereby limiting their usefulness. Reverse transcription-loop-mediated isothermal amplification (RT-LAMP), a one-step nucleic acid amplification method conducted at a single temperature, has been used for colorimetric virus detection. CRISPR-Cas12 and CRISPR-Cas13 systems, which possess collateral activity against ssDNA and RNA, respectively, have also been harnessed for virus detection. Here, we built an efficient, rapid, specific, sensitive, user-friendly SARS-CoV-2 detection module that combines the robust virus amplification of RT-LAMP with the specific detection ability of SARS-CoV-2 by CRISPR-Cas12. Furthermore, we combined the RT-LAMP-CRISPR-Cas12 module with lateral flow cells to enable highly efficient point-of-care SARS-CoV-2 detection. Our iSCAN SARS-CoV-2 detection module, which exhibits the critical features of a robust molecular diagnostic device, should facilitate the effective management and control of COVID-19.


Assuntos
Betacoronavirus/genética , Sistemas CRISPR-Cas , Técnicas de Laboratório Clínico/métodos , Colorimetria/métodos , Infecções por Coronavirus/diagnóstico , Técnicas de Diagnóstico Molecular/métodos , Técnicas de Amplificação de Ácido Nucleico/métodos , Pneumonia Viral/diagnóstico , Técnicas de Laboratório Clínico/instrumentação , Colorimetria/instrumentação , Infecções por Coronavirus/virologia , Endodesoxirribonucleases/química , Humanos , Técnicas de Diagnóstico Molecular/instrumentação , Técnicas de Amplificação de Ácido Nucleico/instrumentação , Pandemias , Pneumonia Viral/virologia , Sistemas Automatizados de Assistência Junto ao Leito , Reologia , Sensibilidade e Especificidade
10.
J Chromatogr A ; 1627: 461391, 2020 Sep 13.
Artigo em Inglês | MEDLINE | ID: mdl-32823097

RESUMO

In this study, a three-phase laminar flow microfluidic chip (TPL chip) combined with HPLC was developed for monitoring free and total concentrations of paclitaxel (PTX) in blood simultaneously. A diluted whole blood sample (aqueous phase) was introduced into the chip, ethyl acetate (organic phase) was introduced into the chip for extraction, and an interphase was used to prevent the blood sample from coming into direct contact with the organic phase. Because only free drug can quantitatively diffuse into the organic extraction phase and the free drug fraction has a linear relationship with the dilution factor of blood, both the free and total drug concentrations can be obtained by detecting the concentration of paclitaxel in the organic extraction phase. The governing factor such as flow rate for extraction was optimized. Docetaxel was used as an internal standard. The reliability of the quantitative diffusion of molecules in the TPL chip was proved by the methodological investigation of PTX in PBS sample, which showed a good linearity in the concentration range of 0.5 - 100 µg/mL and a detection limit of 7 ng/mL. Good repeatibilities for retention time (RSD of PTX is 1.23%, docetaxel is 1.14%, n = 5) and peak area ratio of PTX to docetaxel (RSD is 4.38%) were obtained. For blood sample analysis, only 100 µL of sample was needed and whole pretreatment was finished in 35 min, and a recovery of 94~117% were obtained. The provided method showed advantages in fast analysis speed, minimum sample handing, and potential ability of automation, and integration.


Assuntos
Microfluídica/métodos , Paclitaxel/sangue , Reologia , Animais , Cromatografia Líquida de Alta Pressão , Humanos , Ratos , Reprodutibilidade dos Testes , Albumina Sérica Humana/análise
11.
Nat Commun ; 11(1): 4000, 2020 08 10.
Artigo em Inglês | MEDLINE | ID: mdl-32778657

RESUMO

Additive manufacturing permits innovative soft device architectures with micron resolution. The processing requirements, however, restrict the available materials, and joining chemically dissimilar components remains a challenge. Here we report silicone double networks (SilDNs) that participate in orthogonal crosslinking mechanisms-photocurable thiol-ene reactions and condensation reactions-to exercise independent control over both the shape forming process (3D printing) and final mechanical properties. SilDNs simultaneously possess low elastic modulus (E100% < 700kPa) as well as large ultimate strains (dL/L0 up to ~ 400 %), toughnesses (U ~ 1.4 MJ·m-3), and strengths (σ ~ 1 MPa). Importantly, the latent condensation reaction permits cohesive bonding of printed objects to dissimilar substrates with modulus gradients that span more than seven orders of magnitude. We demonstrate soft devices relevant to a broad range of disciplines: models that simulate the geometries and mechanical properties of soft tissue systems and multimaterial assemblies for next generation wearable devices and robotics.


Assuntos
Teste de Materiais , Impressão Tridimensional , Silicones/química , Tecnologia Biomédica , Módulo de Elasticidade , Fenômenos Mecânicos , Polímeros , Reologia , Robótica , Resistência à Tração , Fatores de Tempo , Dispositivos Eletrônicos Vestíveis
12.
Nat Commun ; 11(1): 3859, 2020 07 31.
Artigo em Inglês | MEDLINE | ID: mdl-32737298

RESUMO

Non-enzymatic proteins including antibodies function as biomarkers and are used as biopharmaceuticals in several diseases. Protein-responsive soft materials capable of the controlled release of drugs and proteins have potential for use in next-generation diagnosis and therapies. Here, we describe a supramolecular/agarose hydrogel composite that can release a protein in response to a non-enzymatic protein. A non-enzymatic protein-responsive system is developed by hybridization of an enzyme-sensitive supramolecular hydrogel with a protein-triggered enzyme activation set. In situ imaging shows that the supramolecular/agarose hydrogel composite consists of orthogonal domains of supramolecular fibers and agarose, which play distinct roles in protein entrapment and mechanical stiffness, respectively. Integrating the enzyme activation set with the composite allows for controlled release of the embedded RNase in response to an antibody. Such composite hydrogels would be promising as a matrix embedded in a body, which can autonomously release biopharmaceuticals by sensing biomarker proteins.


Assuntos
Anidrase Carbônica II/química , Preparações de Ação Retardada/síntese química , Hidrogéis/química , Ribonucleases/química , Sefarose/química , Animais , Anticorpos/química , Avidina/química , Biotina/química , Anidrase Carbônica II/antagonistas & inibidores , Inibidores da Anidrase Carbônica/química , Bovinos , Ativação Enzimática , Transição de Fase , Reologia , Ribonucleases/antagonistas & inibidores , Sulfonamidas/química
13.
Virus Res ; 288: 198129, 2020 10 15.
Artigo em Inglês | MEDLINE | ID: covidwho-719033

RESUMO

The COVID-19 pandemic caused by SARS-CoV-2 affects all aspects of human life. Detection platforms that are efficient, rapid, accurate, specific, sensitive, and user friendly are urgently needed to manage and control the spread of SARS-CoV-2. RT-qPCR based methods are the gold standard for SARS-CoV-2 detection. However, these methods require trained personnel, sophisticated infrastructure, and a long turnaround time, thereby limiting their usefulness. Reverse transcription-loop-mediated isothermal amplification (RT-LAMP), a one-step nucleic acid amplification method conducted at a single temperature, has been used for colorimetric virus detection. CRISPR-Cas12 and CRISPR-Cas13 systems, which possess collateral activity against ssDNA and RNA, respectively, have also been harnessed for virus detection. Here, we built an efficient, rapid, specific, sensitive, user-friendly SARS-CoV-2 detection module that combines the robust virus amplification of RT-LAMP with the specific detection ability of SARS-CoV-2 by CRISPR-Cas12. Furthermore, we combined the RT-LAMP-CRISPR-Cas12 module with lateral flow cells to enable highly efficient point-of-care SARS-CoV-2 detection. Our iSCAN SARS-CoV-2 detection module, which exhibits the critical features of a robust molecular diagnostic device, should facilitate the effective management and control of COVID-19.


Assuntos
Betacoronavirus/genética , Sistemas CRISPR-Cas , Técnicas de Laboratório Clínico/métodos , Colorimetria/métodos , Infecções por Coronavirus/diagnóstico , Técnicas de Diagnóstico Molecular/métodos , Técnicas de Amplificação de Ácido Nucleico/métodos , Pneumonia Viral/diagnóstico , Técnicas de Laboratório Clínico/instrumentação , Colorimetria/instrumentação , Infecções por Coronavirus/virologia , Endodesoxirribonucleases/química , Humanos , Técnicas de Diagnóstico Molecular/instrumentação , Técnicas de Amplificação de Ácido Nucleico/instrumentação , Pandemias , Pneumonia Viral/virologia , Sistemas Automatizados de Assistência Junto ao Leito , Reologia , Sensibilidade e Especificidade
14.
Int J Nanomedicine ; 15: 4717-4737, 2020.
Artigo em Inglês | MEDLINE | ID: mdl-32636627

RESUMO

Purpose: The present study was designed to study the gentamycin (GTM)-loaded stimulus-responsive chitosan nanoparticles to treat bacterial conjunctivitis. Methods: GTM-loaded chitosan nanoparticles (GTM-CHNPs) were prepared by ionotropic gelation method and further optimized by 3-factor and 3-level Box-Behnken design. Chitosan (A), sodium tripolyphosphate (B), and stirring speed (C) were selected as independent variables. Their effects were observed on particle size (PS as Y1), entrapment efficiency (EE as Y2), and loading capacity (LC as Y3). Results: The optimized formulation showed the particle size, entrapment efficiency, and loading capacity of 135.2±3.24 nm, 60.18±1.65%, and 34.19±1.17%, respectively. The optimized gentamycin-loaded chitosan nanoparticle (GTM-CHNPopt) was further converted to the stimulus-responsive sol-gel system (using pH-sensitive carbopol 974P). GTM-CHNPopt sol-gel (NSG5) exhibited good gelling strength and sustained release (58.99±1.28% in 12h). The corneal hydration and histopathology of excised goat cornea revealed safe to the cornea. It also exhibited significant (p<0.05) higher ZOI than the marketed eye drop. Conclusion: The finding suggests that GTM-CHNP-based sol-gel is suitable for ocular delivery to enhance the corneal contact time and improved patient compliance.


Assuntos
Antibacterianos/administração & dosagem , Gentamicinas/administração & dosagem , Gentamicinas/farmacologia , Hidrogéis/administração & dosagem , Nanopartículas/química , Administração Oftálmica , Animais , Antibacterianos/farmacologia , Quitosana/química , Córnea/efeitos dos fármacos , Portadores de Fármacos , Liberação Controlada de Fármacos , Hidrogéis/química , Concentração de Íons de Hidrogênio , Testes de Sensibilidade Microbiana , Tamanho da Partícula , Polifosfatos/química , Reologia
15.
J Chromatogr A ; 1625: 461270, 2020 Aug 16.
Artigo em Inglês | MEDLINE | ID: mdl-32709322

RESUMO

In sample pre-treatment, millifluidic electromembrane platforms have been developed to extract and pre-concentrate target molecules with good clean-up that minimize matrix effects. Optimal operation conditions are normally determined experimentally, repeating the extractions at different conditions and determining the efficiencies by an analytical technique. To shorten and simplify the optimization protocol, millifluidic platforms have been electrically characterized by impedance spectroscopy. The magnitude of the resistance of the electromembrane has been found very predictive of the migration capacity and extraction efficiency of three different parabens on real time. The optimal conditions (4 V of applied potential) (Electromembrane extraction low voltage) have been successfully applied in the extraction of parabens from urine samples, that not only improves the extraction efficiency (100% for all compounds) but also provides a very low current intensity (7 µA), which is very important in electromembrane to minimize electrolysis phenomena. The possibility to optimize one of the most critical and important parameters such as the voltage with a simple electrical model may accelerate the production of application-specific millifluidic electromembrane platforms in a short development time. The results showed that millifluidic electromembrane extraction based low voltage has a future potential as a simple, selective, and time-efficient sample preparation technique allowing a simple battery as power supply.


Assuntos
Impedância Elétrica , Membranas Artificiais , Microfluídica/instrumentação , Modelos Teóricos , Parabenos/isolamento & purificação , Adulto , Eletrólise , Feminino , Humanos , Limite de Detecção , Reprodutibilidade dos Testes , Reologia , Soluções
16.
J Chromatogr A ; 1625: 461272, 2020 Aug 16.
Artigo em Inglês | MEDLINE | ID: mdl-32709324

RESUMO

Trapping multiple dual mode (trapping MDM) is a preparative liquid-liquid chromatography (LLC) technique well-suited to difficult separations of intermediately-eluting components from similarly structured impurities. In this demonstrative study, a design approach for high process throughput is applied for the trapping MDM separation of a target component, nootkatone (NK), initially comprising 16.7% of an industrial side stream mixture with over 90 impurities. This design approach, previously developed and validated using ternary mixtures of model solutes, is applied to a complex real mixture for the first time. The approach consists of five steps: (1) determination of the maximum starting mixture concentration for feed preparation; (2) determination of the maximum flow rate for maintenance of the pre-set stationary phase fraction; (3) determination of the partition coefficients of the target and main impurities; (4) selection of step durations and number of cycles using an established short-cut method; (5) execution of the trapping MDM separation. The target, NK, was obtained along with a co-eluting component at 78.7% purity and 84.6% yield, demonstrating the effectiveness of trapping MDM for the separation of intermediately-eluting natural product target components from complex starting mixtures.


Assuntos
Produtos Biológicos/química , Cromatografia Líquida/métodos , Extratos Vegetais/química , Sesquiterpenos Policíclicos/isolamento & purificação , Distribuição Contracorrente , Cromatografia Gasosa-Espectrometria de Massas , Sesquiterpenos Policíclicos/química , Reologia , Soluções , Solventes/química
17.
J Chromatogr A ; 1625: 461326, 2020 Aug 16.
Artigo em Inglês | MEDLINE | ID: mdl-32709355

RESUMO

Eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA) are essential fatty acids for human body, which are widely used in the field of healthy food and medicine. Meanwhile, there are some differences in their physiological functions, such as "scavenger for blood vessel" of EPA and "brain protector" of DHA. In order to make full use of EPA and DHA, it is necessary to prepare their high-purity component. In this paper, EPA and DHA were separated and purified by three-zone simulated moving bed (SMB) chromatography with C18 used as stationary phase and ethanol-water as mobile phase. For the single column experiment, a separation unit of SMB, the effects of the ratio of ethanol to water, pH value and temperature on the separation were investigated. The equilibrium dispersion (ED) model was used to obtain the adsorption parameters of EPA and DHA by inverse method and genetic algorithm, and the accuracy of the adsorption parameters was verified by fitting the overloaded elution curves under different conditions. Based on the acquired nonlinear adsorption isotherms the complete separation region was found according to triangle theory. The effects of sample concentration, flow ratios of adsorption zone and rectification zone, and column distribution mode of SMB on the separation were investigated. Under the optimized SMB conditions, the experimental result was that without regard to the other components, the chromatographic purity and recovery values of EPA and DHA exceeded 99% with the productivity of 4.15 g/L/h, and the solvent consumption of 1.11 L/g.


Assuntos
Cromatografia/métodos , Ácidos Docosa-Hexaenoicos/isolamento & purificação , Ácido Eicosapentaenoico/isolamento & purificação , Adsorção , Cromatografia Líquida de Alta Pressão , Ácidos Docosa-Hexaenoicos/química , Ácido Eicosapentaenoico/química , Dinâmica não Linear , Reologia , Solventes/química , Temperatura
18.
J Chromatogr A ; 1625: 461286, 2020 Aug 16.
Artigo em Inglês | MEDLINE | ID: mdl-32709336

RESUMO

In the past two decades, supercritical fluid chromatography has evolved from a niche application to a comprehensive technology and a fully-fledged alternative to conventional high-performance liquid chromatography. In this study, we have focused on chiral separation of synthetic cathinones in gradient supercritical fluid chromatography coupled to mass spectrometry using an inverse gradient of a make-up solvent. Synthetic cathinones possess an amphetamine-like effect and, therefore, are frequently being offered on the Internet as a replacement for illicit drugs. Cathinones are chiral compounds, however, they are usually marketed and used as racemic mixtures. Since the effect of individual enantiomers can significantly vary, there is a need for the development of enantioseparation methods enabling to study the biological effects of individual enantiomers. Since cathinones are basic molecules, they are easily protonated (positively charged) under weakly acidic mobile phase conditions, which is a typical feature of supercritical mobile phases with an alcohol as an organic modifier. The positively charged species represent ideal analytes for ion exchangers, such as chiral zwitterion ion exchangers Chiralpak ZWIX (+) and Chiralpak ZWIX (-), which possess a positively and negatively charged unit in the molecular structure of the selectors. The presence of the positive charge in the selector's structure, functioning as a counter-ion for the positively charged analytes, significantly reduces the required amount of a buffer, which is plausible for hyphenation of such a separation system with mass spectrometry. For mass spectrometry hyphenated to supercritical fluid chromatography, the use of a make-up solvent is required to avoid analyte precipitation when using a low concentration of an organic co-solvent (modifier) in the super-/subcritical mobile phase. Hereby, we introduce a unique approach, which is based on the gradient introduction of the make-up to the post-column effluent. Using this approach, it is possible to keep constant the overall amount of the organic solvent (modifier and make-up) introduced into the mass spectrometer when using a gradient of the organic modifier. We show that the developed gradient elution method facilitates the chiral separation of all employed analytes, while the mobile-phase gradient compensation by the inverse make-up gradient enables their detection with high signal intensities.


Assuntos
Alcaloides/química , Alcaloides/isolamento & purificação , Cromatografia com Fluido Supercrítico/métodos , Espectrometria de Massas/métodos , Reologia , Solventes/química , Alcaloides/síntese química , Cromatografia Líquida de Alta Pressão , Pressão , Estereoisomerismo , Temperatura
19.
Water Sci Technol ; 81(7): 1406-1419, 2020 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-32616693

RESUMO

The anaerobic digestion (AD) process is influenced by a variety of operation parameters, such as sludge rheology, mixing, temperature, solid retention time (SRT), hydraulic retention time (HRT) and solids concentration. The optimum in the mixing lies somewhere between no-mixing and continuous mixing, as the lack or excessive mixing can lead to poor AD performance instead. A three-dimensional computational fluid dynamics steady/unsteady model, incorporating the rheological properties of the sludge, was developed and applied to quantify mixing in a full-scale anaerobic digester. Mechanical and gas mixing solutions were taken into account, keeping constant the daily energy consumption. Results, consisting of velocity magnitude and patterns, dead zone formation and turbulence levels were discussed. Compared to the mechanical mixing, gas mixing had lower percentage of dead zones (about 5% against 50%), larger maximum velocity (about 3 m/s against 1 m/s) as well as larger turbulent kinetic energy levels (0.24 m2/s2 against 0.001 m2/s2).


Assuntos
Reatores Biológicos , Esgotos , Anaerobiose , Hidrodinâmica , Reologia
20.
Water Sci Technol ; 81(8): 1636-1645, 2020 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-32644957

RESUMO

A literature screening on computational fluid dynamics (CFD) modelling in water treatment applications showed a vast range of validation ranging from no validation at all, over residence time distribution (RTD) and tracer testing, to velocity field, species concentration and, finally, turbulence properties measurements. The validation level also differs depending on process scale (laboratory, pilot, full) and type of system (rheology, single phase vs. multiphase). Given the fact that CFD is in more widespread use, a discussion on the extent and need of validation needs to be initiated. This paper serves as a discussion starter on the topic.


Assuntos
Águas Residuárias , Purificação da Água , Simulação por Computador , Hidrodinâmica , Reologia , Água
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