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Microwave synthesis solutions from Personal Chemistry.

By fulfilling the specific design criteria required for safe and reproducible microwave synthesis, Personal Chemistry introduced the first microwave system designed for organic chemistry in 2000. The principle of microwave synthesis offers 3 major benefits to chemistry development: speed, reproducibility, and a scalable approach to compound synthesis. Additionally, significant advantages of our technical solution are ease of use, safety, verified synthesis methods to enable new users, and an efficient workflow that fits the drug discovery process. To gain the greatest advantages offered by microwave synthesis, Personal Chemistry has implemented a system called Coherent Synthesis. Incorporating planning systems, automation, distributed system access, searchable databases and reaction optimisation kits, the technology has already proved itself to dramatically improve the quality of output from medicinal chemistry for lead optimisation in all the major pharmaceutical and biotech companies.

Automation↗

Single vessel procedure for acid-vapour partial digestion in a focused microwave: Fe and Co determination in biological samples by ETAAS.

A single vessel procedure using a focused microwave oven is proposed for biological sample preparation with nitric acid vapour under atmospheric pressure. A laboratory-made PTFE support vessel equipped with four cups that received the samples was adapted to fit on the microwave glass vessel. Biological samples (30 mg) were directly weighed into these PTFE cups followed by the addition of 150 microliters of water or H2O2. The mixture was exposed to acid vapour stemming from 15 ml of concentrated HNO3 placed in the bottom of the glass vessel. The acid vapour was formed at 115 degrees C and brought about the Co and Fe extraction in 10 and 60 min, respectively. The resulting suspension was diluted with 0.14 mol l-1 HNO3 to a final volume of 1.0 ml, shaken and centrifuged. The supernatant was analysed by electrothermal atomic absorption spectrometry (ETAAS) by placing the cups directly in the autosampler of the spectrometer. This system minimised contamination, and reagent and time consumption and was suitable for Co and Fe determination in biological materials. The accuracy of the proposed method was assessed by using certified reference materials and by comparison with the closed vessel microwave as a comparative technique. Cobalt and Fe recovery was around 82-99%. As an additional advantage, up to 6 samples can be simultaneously prepared in each vessel, thereby improving the sample throughput from 6 to 24, when a 6-cavity focused microwave is used.

Animals↗

Microwave plasma treatment of polymer surface for irreversible sealing of microfluidic devices.

Microwave plasma was generated in a glass bottle containing 2-3 Torr of oxygen for plasma treatment of a polymer surface. A "kitchen microwave oven" and a dedicated microwave digestion oven were used as the power source. Poly(dimethylsiloxane)(PDMS) slabs treated by a 30 W plasma for 30-60 s sealed irreversibly to form microfluidic devices that can sustain solution flow of an applied pressure of 42 psi without leaking. Experimental set up and conditions for the production of a homogeneous plasma to activate the PDMS surface for irreversible sealing are described in detail. The surface of a microwave plasma-treated PDMS slab was characterized using atomic force microscopy (AFM) and attenuated total reflection-Fourier Transform infrared spectroscopy (ATR-FTIR). The plasma-treated surface bears silica characteristics.

Dimethylpolysiloxanes↗

Influence of microwave radiation on free Candida antarctica lipase B activity and stability.

The influence of microwave heating on free Candida antarctica lipase B activity and stability was studied over the temperature range from 40 to 110 degrees C. Concerning the lipase activity, identical initial rate and conversion yield were obtained under microwave radiation and classical thermal heating for the alcoholysis between ethyl butyrate and butanol in a solvent-free system. On the other hand, the kinetics of the free lipase inactivation in butanol appears to be influenced by the heating mode. The Arrhenius plot obtained under classical heating was linear over all the temperature range studied whereas a biphasic Arrhenius plot was obtained under microwaves. The non-classical effect of the microwave heating on the initial rate of the enzymatic inactivation was thus dependent on the temperature of incubation.

Butanols↗

Temperature course and distribution during plasma heating with a microwave device.

In spite of the much shorter thawing times, the use of microwave devices for heating units of fresh frozen plasma is still being discussed. Concerns about general and localised overheating are the main arguments against the use of microwave devices. We evaluated the warming of fresh frozen plasma using the recently introduced Transfusio-therm 2000(R) microwave blood warmer. Units of fresh frozen plasma were weighed and the heating times were recorded. The surface temperature of the fresh frozen plasma bags during heating was recorded every 10 s. Temperature variation on the surface was examined by measuring the difference between peripheral and centrally placed temperature sensors. After heating, plasma temperature was determined using a calibrated thermometer. There were no signs of overheating during the heating process. The surface temperature of three units of fresh frozen plasma heated simultaneously (n = 45) was 34.0 degrees C (SD, 1.5 degrees C) after a mean heating time of 23.2 min (SD, 1.1 min). The mean (SD) temperature difference was -0.6 (0.5) degrees C and the mean (SD) plasma temperature was 33.6 (0.8) degrees C. Heating one fresh frozen plasma unit at a time (n = 20), the mean (SD) heating time was 6.3 (0.4) min. The surface temperature after heating was 34.3 (0.2) degrees C, the mean (SD) temperature difference was -0.6 (0.4) degrees C and the mean (SD) plasma temperature after heating 33.1 (0.6) degrees C. We conclude that no general or localised overheating of fresh frozen plasma occurs during or after heating with the microwave blood warmer.

Blood Preservation↗

Early morphologic changes following microwave endocardial ablation for treatment of chronic atrial fibrillation during mitral valve surgery.

INTRODUCTION: The aim of this study was to investigate the early qualitative and quantitative structural changes in the left atrial wall after endocardial microwave ablation in patients with chronic atrial fibrillation (AF) undergoing mitral surgery. METHODS AND RESULTS: Seven patients with chronic AF of for at least 6 months underwent surgical microwave energy ablation. Linear isolation of pulmonary veins was performed in all patients by microwave energy applications to the endocardial surface delivered by catheter at 65-W constant power for 45 seconds. Biopsies were obtained from a selected site (below the right lower pulmonary vein) of the left atrial posterior wall before and after the ablation procedure in all patients. Control tissues from the same sites were obtained at autopsy from patients with noncardiac causes of death. Light and electron microscopy was used to examine qualitative and quantitative changes in tissue morphology. Tissues after endocardial ablation procedure showed significantly increased loss of contractile material. Electron microscopy of atrial tissue demonstrated loss of profile of perinuclear and plasma membranes of myocytes, disruption of the endothelial cells of capillary vessels, and presence of macrophages. CONCLUSION: Lesions created by endocardial microwave energy ablation revealed a transmural effect on the left atrial wall without a significant reduction in thickness but a significant increase in the myolytic areas involving the entire cytosol and occlusion of the small intramyocardial vessels within the ablative lesion.

Aged↗

Combined atrial fibrillation and mitral valve surgery using microwave technology.

Atrial fibrillation is associated with a significant morbidity and mortality and is typically related to patients with mitral valve disease. Microwave ablation is a new option for surgical treatment of chronic atrial fibrillation. We present our experience with surgical treatment of mitral valve disease and microwave ablation in patients with chronic atrial fibrillation. In 105 patients (73 women, 32 men, 68.6 +/- 8 years of age from 45 to 83 years, ejection fraction 28% to 80%, left atrial diameter 56 +/- 9.1 mm from 35 to 97 mm) with mitral valve disease, chronic atrial fibrillation was documented for 8.6 +/- 6.8 years. Microwave ablation was performed using a continuous ablation line starting at the posterior mitral valve annulus and incorporating the interior of all pulmonary veins. In 33 patients, mitral valve reconstruction was performed. Ten patients received biologic valve replacement; 3 of them got a stentless quattro mitral valve prosthesis. Survival rate was 99.1% (n = 104). In the 6-month follow-up, 42 of 69 patients were in sinus rhythm (61%); in the 1-year follow-up, 37 of 64 patients were in sinus rhythm (57.8%). Microwave ablation is a safe and efficient method for surgical treatment of chronic atrial fibrillation in patients with mitral valve disease.

Aged↗

Microwave recanalization: thermal effects with nitinol and stainless-steel stents.

BACKGROUND AND STUDY AIMS: A previous study we conducted evaluated the thermal effects of microwave irradiation when attempting recanalization of a nitinol stent occluded by tumor ingrowth. The present study evaluates the thermal effects of microwave irradiation on different stents in vitro. METHODS: The thermal response to microwave energy was evaluated in a muscle-equivalent phantom containing a nitinol (Accuflex) or stainless-steel stent (Wallstent). The phantom temperature was monitored continuously at different distances from an electrode, with either stent type in place. The tip of the electrode was either in contact with the stent or not in contact with it. RESULTS: The steel stent showed a smaller temperature increase than nitinol at 2 mm from the electrode. Without electrode contact, the stents did not differ significantly during the first 40s of irradiation. The stents did not differ significantly with regard to temperatures further from the electrode. When the electrode was in contact with the stent, the rise in temperature was significantly greater with the stainless-steel stent than with the nitinol one, but the phantom temperature did not exceed 45 degrees C with either of the stents. CONCLUSIONS: In patients with a Wallstent stainless-steel stent, microwave coagulation therapy to recanalize stent occlusions appears to be feasible in the same conditions as with an Accuflex nitinol stent.

Alloys↗

Tensile bond strength of acrylic resin denture teeth to a microwave- or heat-processed denture base.

STATEMENT OF PROBLEM: Fracture of acrylic resin prosthetic teeth from acrylic resin denture bases can be a problem for some patients. The optimal combination of acrylic resin denture tooth, denture base material, and processing method is not known. Purpose. The objective of this study was to compare the tensile bond strengths of heat- and microwave-polymerized acrylic resins among 4 types of acrylic resin denture teeth. MATERIAL AND METHODS: Heat-polymerized (Lucitone 199) and microwave-polymerized (Acron MC) acrylic resins were used. Four types of acrylic resin denture teeth (IPN, SLM, Vitapan, and SR-Orthotyp-PE) were milled to a fixed diameter according to ADA specification no. 15. Ten specimens of each tooth type were processed to each of the denture base materials according to the manufacturers' instructions. Ten additional resin control specimens without teeth also were fabricated. Specimens were thermocycled and tested for strength until fracture with a custom alignment device. Data were analyzed with analysis of variance and Duncan's multiple range test. A scanning electron microscope was used to identify adhesive and cohesive failures within debonded specimens. RESULTS: The mean force required to fracture the specimens ranged from 5.3 +/- 3.01 to 21.6 +/- 5.2 MPa for the microwave-polymerized base and 11.2 +/- 3.0 to 39.1 +/- 5.1 MPa for the heat-polymerized base. The most common failure was cohesive within the denture tooth. With each base material, Orthotyp and IPN teeth exhibited the highest bond strengths; SLM and Orthotyp bond strengths were similar. In general, heat-polymerized groups failed cohesively within the denture base resin or the tooth, and microwave-polymerized groups failed adhesively at either the ridge lap or occlusal surface of the denture tooth. CONCLUSION: Within the limitations of this study, the results suggest that the type of denture base material and denture tooth selected for use may influence the tensile bond strength of the tooth to the base. Selection of more compatible combinations of base and resin teeth may reduce the number of prosthesis fractures and resultant repairs.

Acrylic Resins↗

Dimensional change in complete dentures fabricated by injection molding and microwave processing.

STATEMENT OF PROBLEM: Acrylic resin complete dentures undergo dimensional changes during polymerization. Techniques with injection molding and polymerization and microwave polymerization are reported to reduce these changes and thereby improve clinical fit. These dimensional changes need to be quantified. PURPOSE: The purpose of this study was to compare differences in dimensional changes of simulated maxillary complete dentures during polymerization and storage in water after injection molding and conventional polymerization, or microwave polymerization against a control of conventionally packed and polymerized simulated maxillary complete dentures. MATERIAL AND METHODS: Forty identical maxillary denture bases were prepared in dental wax with anatomic teeth. They were invested and the wax eliminated from the molds. Ten specimens each were randomly assigned to 1 of 4 groups. Group 1 was compression molded and conventionally polymerized; group 2 was injection molded and conventionally polymerized (Success); group 3 was injection molded and microwave polymerized (Acron MC); and group 4 was injection molded and microwave polymerized (Microbase). Intermolar width and changes in vertical dimension of occlusion, were determined after polymerization and after storage in water for 28 days. Measurements in triplicate were made between points scribed on the second molar teeth with a traveling microscope (accurate to 0.005 mm). Vertical dimension of occlusion was measured between points scribed on the upper and lower members of an articulator by use of an internal micrometer (accurate to 0.05 mm). Data were analyzed by use of a 1-way analysis of variance with Tukey post-hoc contrasts (P <.05). RESULTS: Polymerization contractions (intermolar widths) for each group were: group 1, -0.24%; group 2, -0.27%; group 3, -0.35%; and group 4, -0.37%. The Microbase specimens had greater shrinkage than conventionally polymerized specimens, but there were no significant differences between the groups. All injection methods had less postpolymerization increase in vertical dimension of occlusion (0.63 to 0.41 mm) than the conventional Trevalon control (0.74 mm), but only group 4 was significantly different (P<.004). After storage in water for 28 days, all specimens increased in vertical dimension of occlusion (0.10% to 0.16%) from polymerization techniques, but there were no significant differences between groups. CONCLUSION: Within the limitations of this study, injection molding resulted in a slightly less increase of vertical dimension of occlusion than conventional polymerization techniques, the difference being significant for Microbase compared with the conventional Trevalon control.

Acrylic Resins↗

Microwave-assisted protein preparation and enzymatic digestion in proteomics.

The combinations of gel electrophoresis or LC and mass spectrometry are two popular approaches for large scale protein identification. However, the throughput of both approaches is limited by the speed of the protein digestion process. Present research into fast protein enzymatic digestion has been focused mainly on known proteins, and it is unclear whether these results can be extrapolated to complex protein mixtures. In this study microwave technology was used to develop a fast protein preparation and enzymatic digestion method for protein mixtures. The protein mixtures in solution or in gel were prepared and digested by microwave-assisted protein enzymatic digestion, which rapidly produces peptide fragments. The peptide fragments were further analyzed by capillary LC and ESI-ion trap-MS or MALDI-TOF-MS. The technique was optimized using bovine serum albumin and then applied to human urinary proteins and yeast lysate. The method enabled preparation and digestion of protein mixtures in solution (human urinary proteins) or in gel (yeast lysate) in 6 or 25 min, respectively. Equivalent (in-solution) or better (in-gel) digestion efficiency was obtained using microwave-assisted protein enzymatic digestion compared with the standard overnight digestion method. This new application of microwave technology to protein mixture preparation and enzymatic digestion will hasten the application of proteomic techniques to biological and clinical research.

Chromatography, Liquid↗

Rapid polymerisation with microwave irradiation for transmission electron microscopy.

Successful results of microwave polymerisation of different epoxy formulations have been reported in the literature. The present study was intended to shorten the time needed for polymerisation of epoxy resin by the use of a microwave technique. A standard double fixation and tissue processing was applied to samples of rat kidney tissue. Tissue samples from the control group were polymerised in a conventional oven at 60 degrees C for 48 h, while tissue from the experimental group was irradiated in a microwave oven, initially at 900 W for 10 min and then at 360 W for another 100 min. During this irradiation, the sealed BEEM capsules were submerged in a water bath, so that the temperature rise was uniform and constant. This resulted in a homogeneous and rapid polymerisation. The cutting properties of the blocks in both groups were similar and no noticeable difference in the quality of the sections was evident when evaluated with TEM. The results showed that the use of a microwave oven reduced the time needed for the polymerisation of Epon blocks without any loss in quality.

Animals↗

Migration from plasticized films into foods. 1. Migration of di-(2-ethylhexyl)adipate from PVC films during home-use and microwave cooking.

Migration of di-(2-ethylhexyl)adipate (DEHA) into a diverse range of foods arising from the domestic use of plasticized PVC films has been determined using a stable isotope dilution GC/MS procedure. Aspects of home use reported in this study include the wrapping and covering of foods such as cheese, cooked meats, sandwiches, cakes, fresh fruit and vegetables; the use of films during food preparation such as marinading; covering during microwave reheating of previously prepared foods, and covering during microwave cooking. Contact between film and foods was for differing temperatures and times, representative of the range of conditions likely to be experienced in practice in the home. Migration increased with both the length of contact time and temperature of exposure, with the highest levels observed where there was a direct contact between the film and food, and where the latter had a high fat content on the contact surface. Highest levels of migration were observed for cheese, cooked meats, cakes and for microwave-cooked foods, whilst lower levels were observed for wrapping of unfilled sandwiches, fruit and vegetables (except avocado), and for food preparation including microwave reheating where there was covering of the food in a container but little or no direct contact.

Adipates↗

Volatile nitrosamines in microwave-cooked bacon.

Bacon was analysed for volatile nitrosamines after microwave cooking, and the results were compared with those obtained after frying bacon in a pan. Microwave cooking gave statistically significantly lower levels of all three volatile nitrosamines detected in the bacon. NPYR was found in all 20 samples fried in a pan, but in only five microwave-cooked samples. The average volatile nitrosamine levels (micrograms/kg) in microwave-cooked bacon and pan-fried bacon were: NDMA, 0.3 and 1.2; NPIP, 0.04 and 0.2; NPYR, 0.1 and 4.5.

Animals↗

The effect of microwave energy on specific migration from food contact plastics.

Experiments have been carried out with (a) microwave treatment of plastics followed by migration testing using the food simulant, olive oil, and (b) microwave treatment of plastics in direct contact with an organic extractant (iso-octane). In neither of these complementary approaches was there evidence of any difference in migration from plastics that had been microwave-treated compared with plastics that had received an equivalent thermal treatment. Five plastics commonly employed in microwave applications were tested and oligomers, plasticizer, antioxidant and volatile contaminants were monitored as representatives of typical migration species.

Dietary Fats, Unsaturated↗

Microwave pretreatment for enhancement of phosphorus release from dairy manure.

Both the advanced oxidation process (AOP) using a combination of hydrogen peroxide addition and microwave heating (H2O2/microwave), and the microwave heating process were used for solubilization of phosphorus from liquid dairy manure. About 80% of total phosphate was released into the solution at a microwave heating time of 5 min at 170 degrees C. With an addition of H2O2, more than 81% of total phosphate could be released over a reaction period of 49 h at ambient temperature. The AOP process could achieve up to 85% of total phosphate release at 120 degrees C. The results indicated that both the microwave, and the AOP processes could effectively release phosphate from liquid dairy manure. These processes could serve as pretreatments for phosphorus recovery from animal wastes, and could be combined with the struvite crystallization process to provide a new approach in treating animal wastes.

Animals↗

Burns associated with the use of microwave ovens.

This article reviews published reports of conventional and radiation burns associated with the use of microwave ovens. Conventional food burns can result from the ingestion of microwave heated food because consumers may overlook the differential temperature gradients within foods and between the food and the container. There are reports of accidental radiation injury associated with the use of microwave ovens, but they are difficult to evaluate because these reports lack definitive clinical data and verification of the actual radiation exposures. Only one study has provided useful insight into the clinical features of microwave radiation burns compared to conventional burns.

Burns↗

Synergistic effect of microwave heating and hydrogen peroxide on inactivation of microorganisms.

Escherichia coli K-12 isogenous strains and Pseudomonas aeruginosa 102 were used to study the synergistic effects of combined microwave heating at short-time processing with low concentrations of hydrogen peroxide. The effect of microwave heating to temperatures of 40, 50 and 60 degrees C, as well as the concentration of hydrogen peroxide (0.05, 0.08 and 0.1%), the sequence of the agents' use, the nature of microorganisms on the survival of cells, DNA damages and interaction factors were studied. A method of anomalous viscosity time dependencies (AVTD) was used for measurement of the changes of genome conformational state (GCS) simultaneously with bacterial survival determination. The synergistic effect of microwave heating and low concentrations of hydrogen peroxide was observed under combined application, and reached a maximum when the cells were exposed to microwave heating to 50 degrees C and 0.08% hydrogen peroxide simultaneously. Both maxima of cell destruction and DNA injuries have been achieved by successive exposure to (MW + 10 min H2O2) to 60 degrees C and 0.08% hydrogen peroxide. The mechanisms of synergistic effects, the role of a disturbance of DNA repair and the interaction of sublethal injuries caused by different agents are discussed.

Anti-Infective Agents, Local↗