Rapid and highly efficient synthesis of some 1-aroyl-3,5-dimethylpyrazoles is achieved by the cyclocondensation of corresponding aroyl hydrazides with 2,4-pentanedione in the absence of solvent and catalyst, under mic...Rapid and highly efficient synthesis of some 1-aroyl-3,5-dimethylpyrazoles is achieved by the cyclocondensation of corresponding aroyl hydrazides with 2,4-pentanedione in the absence of solvent and catalyst, under microwave irradiation. The reaction proceeds rapidly and is completed within 40-70 s giving a series of 1-aroyl-3,5-dimethylpyrazoles derivatives in high yields. All of the compounds have been characterized by FTIR, ^1H NMR, and mass spectroscopy.展开更多
In this paper,we present the design of four different circular bioassay platforms,which are suitable for homogeneous microwave heating,using theoretical calculations(i.e.,COMSOLTM multiphysics software).Circular bioas...In this paper,we present the design of four different circular bioassay platforms,which are suitable for homogeneous microwave heating,using theoretical calculations(i.e.,COMSOLTM multiphysics software).Circular bioassay platforms are constructed from poly(methyl methacrylate)(PMMA)for optical transparency between 400-800 nm,has multiple sample capacity(12,16,19 and 21 wells)and modified with silver nanoparticle films(SNFs)to be used in microwave-accelerated bioassays(MABs).In addition,a small monomode microwave cavity,which can be operated with an external microwave generator(100 W),for use with the bioassay platforms in MABs is also developed.Our design parameters for the circular bioassay platforms and monomode microwave cavity during microwave heating were:(i)temperature profiles,(ii)electric field distributions,(iii)location of the circular bioassay platforms inside the microwave cavity,and(iv)design and number of wells on the circular bioassay platforms.We have also carried out additional simulations to assess the use of circular bioassay platforms in a conventional kitchen microwave oven(e.g.,900 W).Our results show that the location of the circular bioassay platforms in the microwave cavity was predicted to have a significant effect on the homogeneous heating of these platforms.The 21-well circular bioassay platform design in our monomode microwave cavity was predicted to offer a homogeneous heating pattern,where inter-well temperature was observed to be in between 23.72-24.13°C and intra-well temperature difference was less than 0.21°C for 60 seconds of microwave heating,which was also verified experimentally.展开更多
In this paper,we demonstrate the application of Metal-Assisted and Microwave-Accelerated Evaporative Crystallization(MA-MAEC)technique to rapid and selective crystallization of a small drug compound.i.e.acetaminophen....In this paper,we demonstrate the application of Metal-Assisted and Microwave-Accelerated Evaporative Crystallization(MA-MAEC)technique to rapid and selective crystallization of a small drug compound.i.e.acetaminophen.Subsequent characterization of the crystals by optical microscopy,powder X-ray diffraction(PXRD)and Raman spectroscopy showed quantitatively selective growth of different crystal forms at various experimental conditions.Acetaminophen crystals were grown predominantly as Form I(99%)on blank glass slides at room temperature.Form II crystals with 39%purity grown on SIFs using microwave energy.展开更多
Metal-Assisted and Microwave-Accelerated Evaporative Crystallization(MA-MAEC),is a new approach to crystallization of drug compounds,amino acids,DNA and proteins.In this work,we report our additional findings on the e...Metal-Assisted and Microwave-Accelerated Evaporative Crystallization(MA-MAEC),is a new approach to crystallization of drug compounds,amino acids,DNA and proteins.In this work,we report our additional findings on the effect of engineered surfaces and sample volume on the rapid crystallization of glycine.With the use of hydrophilic functionalized surfaces and the MA-MAEC technique,glycine crystals~1 mm in size were grown in 35 seconds with 100%selectivity for theα-form.The use of moderately hydrophobic surfaces resulted in the growth of glycine crystals only at room temperature.An increase in volume of initial glycine solution(5-100μL)resulted in an increase in crystal size without a significant increase in total crystallization time.Raman spectroscopy and powder X-ray diffraction results demonstrated that the glycine crystals grown on engineered surfaces were structurally identical to those grown using conventional evaporative crystallization.展开更多
We demonstrate the design and the proof-of-concept use of a new,circular poly(methyl methacrylate)-based bioassay platform(PMMA platform),which affords for the rapid processing of 16 samples at once.The circular PMMA ...We demonstrate the design and the proof-of-concept use of a new,circular poly(methyl methacrylate)-based bioassay platform(PMMA platform),which affords for the rapid processing of 16 samples at once.The circular PMMA platform(5 cm in diameter)was coated with a silver nanoparticle film to accelerate the bioassay steps by microwave heating.A model colorimetric bioassay for biotinylated albumin(using streptavidin-labeled horse radish peroxidase)was performed on the PMMA platform coated with and without silver nanoparticles(a control experiment),and at room temperature and using microwave heating.It was shown that the simulated temperature profile of the PMMA platform during microwave heating were comparable to the real-time temperature profile during actual microwave heating of the constructed PMMA platform in a commercial microwave oven.The model colorimetric bioassay for biotinylated albumin was successfully completed in~2 min(total assay time)using microwave heating,as compared to 90 min at room temperature(total assay time),which indicates a~45-fold decrease in assay time.Our PMMA platform design afforded for significant reduction in non-specific interactions and low background signal as compared to non-silvered PMMA surfaces when employed in a microwave-accelerated bioassay carried out in a conventional microwave cavity.展开更多
We report a method for rapid detection and analysis of biological and environmental analytes by microwave-accelerated bioassays(MABs)and a novel MATLAB-based image processing of colorimetric signals.In this regard,col...We report a method for rapid detection and analysis of biological and environmental analytes by microwave-accelerated bioassays(MABs)and a novel MATLAB-based image processing of colorimetric signals.In this regard,colorimetric bioassays for histidine-rich protein 2(HRP-2)and microcystin-leucine arginine(MC-LR)toxin were carried out using MABs and without microwave heating(i.e,gold standard bioassays).Our MATLAB-based detection method is based on the direct correlation of color intensity of a solution calculated from images captured with a smartphone with the concentration of the biomolecule of interest using a MATLAB code developed in-house.We demonstrated that our MATLAB-based detection method can yield bioassay sensitivity comparable to the colorimetric gold standard tool,i.e.,UV-Visible spectroscopy.In addition,colorimetric bioassay time for the HRP-2 assay(used in malaria diagnosis)and colorimetric MC-LR bioassay(used in MC-LR toxin diagnosis)was reduced from up to 2 hours at room temperature without microwave heating to 15 minutes using the MABs technique.展开更多
N-(4-Methyl-3-tolylthiazol-2(3H)-ylidene) substituted benzamides (2a-o) were synthesized in good to excellent yields by the base-catalyzed direct cyclization of corresponding 1-tolyl-3-aryl thioureas (la-o) wi...N-(4-Methyl-3-tolylthiazol-2(3H)-ylidene) substituted benzamides (2a-o) were synthesized in good to excellent yields by the base-catalyzed direct cyclization of corresponding 1-tolyl-3-aryl thioureas (la-o) with 2-bromoacetone through microwave irradiation in a solvent-free medium. Compared to traditional thermal heating, microwave irradiation provides a much more cleaner, efficient and faster method for synthesis of the title compounds. 2009 Aamer Saeed. Published by Elsevier B.V. on behalf of Chinese Chemical Society. All rights reserved.展开更多
The effect of metal surfaces on the crystallization of lysozyme using the Metal-Assisted and Microwave-Accelerated Evaporative Crystallization(MA-MAEC)technique and a monomode microwave system is described.Our microwa...The effect of metal surfaces on the crystallization of lysozyme using the Metal-Assisted and Microwave-Accelerated Evaporative Crystallization(MA-MAEC)technique and a monomode microwave system is described.Our microwave system(is called the iCrystal system hereafter for brevity)is comprised of a 100 W variable power monomode microwave source,a monomode cavity,fiber optic temperature probes and digital cameras.Crystallization of lysozyme(a model protein)was conducted using the iCrystal system on four different types of circular crystallization plates with 21-well sample capacity(i.e.,crystallization plates):(i)blank:a continuous surface without a metal,(ii)silver nanoparticle films(SNFs):a discontinuous metal film,(iii)iron nano-columns:a semi-continuous metal film,and(iv)indium tin oxide(ITO):a continuous metal film.Lysozyme crystals grown on all crystallization plates were characterized by X-ray crystallography and found to be X-ray diffraction quality.The use of iron nano-columns afforded for the growth of largest number of lysozyme crystals with a narrow size distribution.ITO-modified crystallization plates were deemed to be best of all the crystallization plates based on the observations that lysozyme crystals were grown at the shortest time(370±36 minutes)with a narrow size distribution up to 460 m in size.展开更多
Tumor detection can be carried out via the detection of proteins,such as p53,which is known to play vital role in more than 50%of all cancers affecting humans.Early diagnosis of tumor detection can be achieved by decr...Tumor detection can be carried out via the detection of proteins,such as p53,which is known to play vital role in more than 50%of all cancers affecting humans.Early diagnosis of tumor detection can be achieved by decreasing the lower detection limit of p53 bioassays.Microwave-accelerated bioassay(MAB)technique,which is based on the use of circular bioassay platforms in combination with microwave heating,is employed for the rapid and sensitive detection of p53 protein.Direct sandwich ELISA was constructed on our circular bioassay platforms based on DNA-protein binding interactions.Colorimetric and fluorescence based detection methods were used for room temperature bioassay(control bioassay;total bioassay time is 27 hours)and bioassay using microwave heating(i.e.,the MAB technique;total bioassay time is 10 minutes).In the colorimetric based detection,a very high background signal due to the non-specific binding of proteins for the bioassay carried out at room temperature and a LLOD of 0.01 ng/mL for p53 was observed using the MAB technique.The LLOD for the fluorescence-based detection using the MAB technique was found to be 0.01 ng/mL.The use of circular bioassay platforms in the MAB technique results in microwave-induced temperature gradient,where the specific protein binding interactions are significantly accelerated;thereby reducing the background signal and the lower limit of detection of p53 protein.展开更多
文摘Rapid and highly efficient synthesis of some 1-aroyl-3,5-dimethylpyrazoles is achieved by the cyclocondensation of corresponding aroyl hydrazides with 2,4-pentanedione in the absence of solvent and catalyst, under microwave irradiation. The reaction proceeds rapidly and is completed within 40-70 s giving a series of 1-aroyl-3,5-dimethylpyrazoles derivatives in high yields. All of the compounds have been characterized by FTIR, ^1H NMR, and mass spectroscopy.
基金supported by Maryland Innovation Initiative(Phase 1)Award from Technology Development Corporation.Additional partial support was supported by Award Number 5-K25EB007565-05 from the National Institute of Biomedical Imaging and BioengineeringThe content is solely the responsibility of the authors and does not necessarily represent the official views of the National Institute of Biomedical Imaging and Bioengineering or the National Institutes of Health.Additional financial support was provided by the MARC U*STAR program(Grant No.5-T34GM007977-27).
文摘In this paper,we present the design of four different circular bioassay platforms,which are suitable for homogeneous microwave heating,using theoretical calculations(i.e.,COMSOLTM multiphysics software).Circular bioassay platforms are constructed from poly(methyl methacrylate)(PMMA)for optical transparency between 400-800 nm,has multiple sample capacity(12,16,19 and 21 wells)and modified with silver nanoparticle films(SNFs)to be used in microwave-accelerated bioassays(MABs).In addition,a small monomode microwave cavity,which can be operated with an external microwave generator(100 W),for use with the bioassay platforms in MABs is also developed.Our design parameters for the circular bioassay platforms and monomode microwave cavity during microwave heating were:(i)temperature profiles,(ii)electric field distributions,(iii)location of the circular bioassay platforms inside the microwave cavity,and(iv)design and number of wells on the circular bioassay platforms.We have also carried out additional simulations to assess the use of circular bioassay platforms in a conventional kitchen microwave oven(e.g.,900 W).Our results show that the location of the circular bioassay platforms in the microwave cavity was predicted to have a significant effect on the homogeneous heating of these platforms.The 21-well circular bioassay platform design in our monomode microwave cavity was predicted to offer a homogeneous heating pattern,where inter-well temperature was observed to be in between 23.72-24.13°C and intra-well temperature difference was less than 0.21°C for 60 seconds of microwave heating,which was also verified experimentally.
基金supported by Award Number 5-K25EB007565-05 from the National Institute of Biomedical Imaging and Bioengineering.
文摘In this paper,we demonstrate the application of Metal-Assisted and Microwave-Accelerated Evaporative Crystallization(MA-MAEC)technique to rapid and selective crystallization of a small drug compound.i.e.acetaminophen.Subsequent characterization of the crystals by optical microscopy,powder X-ray diffraction(PXRD)and Raman spectroscopy showed quantitatively selective growth of different crystal forms at various experimental conditions.Acetaminophen crystals were grown predominantly as Form I(99%)on blank glass slides at room temperature.Form II crystals with 39%purity grown on SIFs using microwave energy.
基金supported by Award Number 5-K25EB007565-05 from the National Institute of Biomedical Imaging and Bioengineering.
文摘Metal-Assisted and Microwave-Accelerated Evaporative Crystallization(MA-MAEC),is a new approach to crystallization of drug compounds,amino acids,DNA and proteins.In this work,we report our additional findings on the effect of engineered surfaces and sample volume on the rapid crystallization of glycine.With the use of hydrophilic functionalized surfaces and the MA-MAEC technique,glycine crystals~1 mm in size were grown in 35 seconds with 100%selectivity for theα-form.The use of moderately hydrophobic surfaces resulted in the growth of glycine crystals only at room temperature.An increase in volume of initial glycine solution(5-100μL)resulted in an increase in crystal size without a significant increase in total crystallization time.Raman spectroscopy and powder X-ray diffraction results demonstrated that the glycine crystals grown on engineered surfaces were structurally identical to those grown using conventional evaporative crystallization.
基金supported by Award Number 5-K25EB007565-05 from the National Institute of Biomedical Imaging and Bioengineering.
文摘We demonstrate the design and the proof-of-concept use of a new,circular poly(methyl methacrylate)-based bioassay platform(PMMA platform),which affords for the rapid processing of 16 samples at once.The circular PMMA platform(5 cm in diameter)was coated with a silver nanoparticle film to accelerate the bioassay steps by microwave heating.A model colorimetric bioassay for biotinylated albumin(using streptavidin-labeled horse radish peroxidase)was performed on the PMMA platform coated with and without silver nanoparticles(a control experiment),and at room temperature and using microwave heating.It was shown that the simulated temperature profile of the PMMA platform during microwave heating were comparable to the real-time temperature profile during actual microwave heating of the constructed PMMA platform in a commercial microwave oven.The model colorimetric bioassay for biotinylated albumin was successfully completed in~2 min(total assay time)using microwave heating,as compared to 90 min at room temperature(total assay time),which indicates a~45-fold decrease in assay time.Our PMMA platform design afforded for significant reduction in non-specific interactions and low background signal as compared to non-silvered PMMA surfaces when employed in a microwave-accelerated bioassay carried out in a conventional microwave cavity.
基金supported by the National Institute of General Medical Sciences of the National Institutes of Health under Award Number UL1GM118973Partial support from the sponsorship by the Army Research Laboratory and was accomplished under Cooperative Agreement Number W911NF-12-2-0022.The views and conclusions contained in this document are those of the authors and should not be interpreted as representing the official policies,either expressed or implied,of the Army Research Laboratory,official views of the National Institutes of Health or the U.S.Government.The U.S.Government is authorized to reproduce and distribute reprints for Government purposes notwithstanding any copyright notation herein.
文摘We report a method for rapid detection and analysis of biological and environmental analytes by microwave-accelerated bioassays(MABs)and a novel MATLAB-based image processing of colorimetric signals.In this regard,colorimetric bioassays for histidine-rich protein 2(HRP-2)and microcystin-leucine arginine(MC-LR)toxin were carried out using MABs and without microwave heating(i.e,gold standard bioassays).Our MATLAB-based detection method is based on the direct correlation of color intensity of a solution calculated from images captured with a smartphone with the concentration of the biomolecule of interest using a MATLAB code developed in-house.We demonstrated that our MATLAB-based detection method can yield bioassay sensitivity comparable to the colorimetric gold standard tool,i.e.,UV-Visible spectroscopy.In addition,colorimetric bioassay time for the HRP-2 assay(used in malaria diagnosis)and colorimetric MC-LR bioassay(used in MC-LR toxin diagnosis)was reduced from up to 2 hours at room temperature without microwave heating to 15 minutes using the MABs technique.
文摘N-(4-Methyl-3-tolylthiazol-2(3H)-ylidene) substituted benzamides (2a-o) were synthesized in good to excellent yields by the base-catalyzed direct cyclization of corresponding 1-tolyl-3-aryl thioureas (la-o) with 2-bromoacetone through microwave irradiation in a solvent-free medium. Compared to traditional thermal heating, microwave irradiation provides a much more cleaner, efficient and faster method for synthesis of the title compounds. 2009 Aamer Saeed. Published by Elsevier B.V. on behalf of Chinese Chemical Society. All rights reserved.
基金supported by the National Center for Advancing Translational Sciences of the National Institutes of Health under Award Number R41TR001275support was provided ARL W911NF-12-2-0041(Seifu)and from NSF MRI-DMR-1337339(Seifu).
文摘The effect of metal surfaces on the crystallization of lysozyme using the Metal-Assisted and Microwave-Accelerated Evaporative Crystallization(MA-MAEC)technique and a monomode microwave system is described.Our microwave system(is called the iCrystal system hereafter for brevity)is comprised of a 100 W variable power monomode microwave source,a monomode cavity,fiber optic temperature probes and digital cameras.Crystallization of lysozyme(a model protein)was conducted using the iCrystal system on four different types of circular crystallization plates with 21-well sample capacity(i.e.,crystallization plates):(i)blank:a continuous surface without a metal,(ii)silver nanoparticle films(SNFs):a discontinuous metal film,(iii)iron nano-columns:a semi-continuous metal film,and(iv)indium tin oxide(ITO):a continuous metal film.Lysozyme crystals grown on all crystallization plates were characterized by X-ray crystallography and found to be X-ray diffraction quality.The use of iron nano-columns afforded for the growth of largest number of lysozyme crystals with a narrow size distribution.ITO-modified crystallization plates were deemed to be best of all the crystallization plates based on the observations that lysozyme crystals were grown at the shortest time(370±36 minutes)with a narrow size distribution up to 460 m in size.
基金supported by National Institute of Biomedical Imaging and Bioengineering,award number 5-K25EB007565-05。
文摘Tumor detection can be carried out via the detection of proteins,such as p53,which is known to play vital role in more than 50%of all cancers affecting humans.Early diagnosis of tumor detection can be achieved by decreasing the lower detection limit of p53 bioassays.Microwave-accelerated bioassay(MAB)technique,which is based on the use of circular bioassay platforms in combination with microwave heating,is employed for the rapid and sensitive detection of p53 protein.Direct sandwich ELISA was constructed on our circular bioassay platforms based on DNA-protein binding interactions.Colorimetric and fluorescence based detection methods were used for room temperature bioassay(control bioassay;total bioassay time is 27 hours)and bioassay using microwave heating(i.e.,the MAB technique;total bioassay time is 10 minutes).In the colorimetric based detection,a very high background signal due to the non-specific binding of proteins for the bioassay carried out at room temperature and a LLOD of 0.01 ng/mL for p53 was observed using the MAB technique.The LLOD for the fluorescence-based detection using the MAB technique was found to be 0.01 ng/mL.The use of circular bioassay platforms in the MAB technique results in microwave-induced temperature gradient,where the specific protein binding interactions are significantly accelerated;thereby reducing the background signal and the lower limit of detection of p53 protein.