Remarks on various applications of microwave energy.

Microwave energy is an alternative energy source that is receiving a considerable amount of attention from researchers for a wide spectrum of applications. The fundamentally different method of transferring energy from the source to the sample is the main benefit of utilizing microwave energy; by directly delivering energy to microwave-absorbing materials, conventional issues such as long heating periods, thermal gradients, and energy lost to the system environment can be minimized or avoided. Furthermore, the penetrating capacity of microwave allows volumetric heating of samples. These attributes of microwave energy make utilizing it very attractive for industrial applications as an alternative to conventional processing methods. The reality is otherwise however, and limited literature is found in any given area of work. Despite the lack of focus, in most published cases, the utilization of microwave energy has produced improved results compared to conventional methods with reduced heating times or reaction temperatures. This review provides a general overview of reported applications of microwave energy in the open literature. It also attempts to summarize the results obtained for various common uses and highlights some applications that have not gathered as much attention as anticipated.

Evaluation of Microwave-Assisted Process technology for HAPSITE's headspace analysis of volatile organic compounds (VOCs).

The use of microwave energy as a heating source for the field-based headspace sampling and the subsequent determination of various volatile organic compounds (VOCs) using a field-portable HAPSITE gas chromatograph-mass spectrometer has been evaluated. A significant advantage in time reduction has been observed when using microwave energy when compared to conventional resistive-based heating. Such time savings are critical in field operations involving equipment such as the HAPSITE where non-routine sampling is commonly performed and very quick turnaround time is usually needed. Further, the technology also showed significant improvements in terms of sensitivity, thus suggesting its applicability to a broader range of compounds and detection levels than current technologies.

Applications of microwave-assisted processes (MAP) to environmental analysis.

The use of microwave-assisted extraction has gained wide acceptance as a powerful tool for the recovery of environmental contaminants and their subsequent analysis. This paper reviews the historical and fundamental basis of the technology. It also provides a cursory review of the current state-of-the-art and literature (2000-2006) in the area of environmental analysis in addition to providing a critical review of the level of efforts being devoted to its further development.

Optimization of microwave-assisted extraction (MAP) for ginseng components by response surface methodology.

Response surface methodology (RSM) was applied to predict optimum conditions for microwave-assisted extraction-a MAP technology-of saponin components from ginseng roots. A central composite design was used to monitor the effect of ethanol concentration (30-90%, X(1)) and extraction time (30-270 s, X(2)) on dependent variables, such as total extract yield (Y(1)), crude saponin content (Y(2)), and saponin ratio (Y(3)), under atmospheric pressure conditions when focused microwaves were applied at an emission frequency of 2450 MHz. In MAP under pre-established conditions, correlation coefficients (R (2)) of the models for total extract yield and crude saponin were 0.9841 (p < 0.001) and 0.9704 (p < 0.01). Optimum extraction conditions were predicted for each variable as 52.6% ethanol and 224.7 s in extract yield and as 77.3% ethanol and 295.1 s in crude saponins, respectively. Estimated maximum values at predicted optimum conditions were in good agreement with experimental values.

MAP: microwave-assisted extraction of cockroaches.

A Microwave-Assisted Process (MAP is a Trade-Mark of Her Majesty the Queen in Right of Canada as represented by the Minister of the Environment) solvent extraction procedure was used in conjunction with GC-MS analysis to investigate the chemical composition of dried and live cockroaches. The main components extracted were classified into four groups: sterols. fatty acids and their esters, long chain alkanes and fused aromatic hydrocarbons.

Influence of operating parameters on the use of the microwave-assisted process (MAP) for the extraction of azadirachtin-related limonoids from neem (Azadirachta indica) under atmospheric pressure conditions.

The use of the microwave-assisted process (MAP) for the extraction of azadirachtin-related limonoids (AZRL) from various parts of the neem tree was investigated under different operating conditions. The influence of microwave power, solvent, and irradiation time on the recovery of AZRL was studied. The efficiency of the microwave-assisted extraction (MAE) of the seed kernel, the seed shell, the leaf, and the leaf stem was compared to that of conventional extraction methods. The content of AZRL in the extracts was estimated with a vanillin-based colorimetric assay and a multivariate calibration technique. The results showed that the MAE technique can enhance the extraction of AZRL from different parts of neem possessing microstructures. Investigation of the influence of the solvent also indicted that the solvent used not only influences the efficiency but also affects the selectivity of the MAE.

Multivariate calibration for the determination of total azadirachtin-related limonoids and simple terpenoids in neem extracts using vanillin assay.

Two-component and multivariate calibration techniques were developed for the simultaneous quantification of total azadirachtin-related limonoids (AZRL) and simple terpenoids (ST) in neem extracts using vanillin assay. A mathematical modeling method was also developed to aid in the analysis of the spectra and to simplify the calculations. The mathematical models were used in a two-component calibration (using azadirachtin and limonene as standards) for samples containing mainly limonoids and terpenoids (such as neem seed kernel extracts). However, for the extracts from other parts of neem, such as neem leaf, a multivariate calibration was necessary to eliminate the possible interference from phenolics and other components in order to obtain the accurate content of AZRL and ST. It was demonstrated that the accuracy of the vanillin assay in predicting the content of azadirachtin in a model mixture containing limonene (25% w/w) can be improved from 50% overestimation to 95% accuracy using the two-component calibration, while predicting the content of limonene with 98% accuracy. Both calibration techniques were applied to estimate the content of AZRL and ST in different parts of the neem plant. The results of this study indicated that the relative content of limonoids was much higher than that of the terpenoids in all parts of the neem plant studied.

MAP: microwave-assisted extraction of fatty acids and Py/GC/MS analysis of selected insects.

A Microwave-Assisted Process (MAP) solvent extraction procedure was used in conjunction with GC/MS analysis to investigate the chemical composition of dried silkworm, dried earthworm, silkworm droppings, and cicada nymph skin. Selected insect samples were also analyzed by pyrolysis-GC-MS. Silkworm and earthworm generated fatty acids, sterols and phenol derivatives. Cicada nymph skin was analyzed by pyrolysis/GC/MS and generated mainly heterocyclic compounds. The data indicated that insects can retain environmental contaminants such as 2,6-bis(1,1-dimethylethyl)-4-methyl phenol (BHT) and as such could be used as biological indicators. In addition, some of the therapeutic characteristics associated with insects could be attributed to the chemicals ingested from plant sources.

Microwave-assisted extraction of phenolic compounds from grape seed.

A microwave-assisted extraction technique was developed to optimize the extraction of phenolic compounds from grape seeds. The microwave power (300-150W) and time of extraction (20-200s) were varied during the optimization process. The polyphenol content of the resulting extracts were measured as mg of tannic acid equivalent per gram of crude extract (mg TAE/g of crude extract), using a Folin-Ciocalteau reagent. In general, neither the time nor the power had a significant effect on the overall % yield (average of 13.5%) and on the polyphenol content (392 mg TAE/g of crude extract) of the extracts. However, when the solvent polarity was changed by the addition of 10% water, the yield increased to 15.2% and the polyphenol content increased to 429 mg TAE/g of crude extract.

Extraction and colorimetric determination of azadirachtin-related limonoids in neem seed kernel.

A colorimetric method was developed for the determination of total azadirachtin-related limonoids (AZRL) in neem seed kernel extracts. The method employed acidified vanillin solution in methanol for the colorization of the standard azadirachtin or neem seed kernel extracts in dichloromethane. Through the investigation of various factors influencing the sensitivity of detection, such as the concentration of vanillin, acid, and the time required for the formation of color, optimum conditions were selected to perform the assay. Under the optimum conditions, a good linearity was found between the absorbance at 577 nm and the concentration of standard azadirachtin solution in the range of 0.01-0.10 mg/mL. In addition, different extraction procedures were evaluated using the vanillin assay. The HPLC analysis of the extracts indicated that if the extractions were performed in methanol followed by partitioning in dichloromethane, approximately 50% of the value determined by the vanillin assay represents azadirachtin content.

Use of the Microwave-Assisted Process in extraction of fat from meat, dairy, and egg products under atmospheric pressure conditions.

Fat from meat, dairy, and egg products was extracted by using Microwave-Assisted Process (MAP) technology under atmospheric pressure conditions. Fat content was determined gravimetrically after extraction with microwaves and organic solvents that are transparent to microwaves relative to the sample. (In situ hydrolysis was performed for dairy and egg products.) Fat from the food sample migrated completely to the extractant when samples were irradiated with focused microwave for a total of 3 min for meat products, 1 min for dairy products, and 4 min for egg products. Unlike current methods used for determining fat in meat products, the microwave-assisted method does not require a dry sample, because moisture in the sample (around 75%) enhances the efficiency of extraction. No preprocessing was required for meat samples other than homogenization, which is critical, as it is for other current methods. In addition to speed and ease of use, the features of this technology are low solvent consumption, low energy consumption, reproducibility, and recoveries similar to or even better than those of conventional extraction methods.

Isolation and structural characterization by spectroscopic methods of two glucuronide metabolites of mexiletine after N-oxidation and deamination.

Urine samples from control and mexiletine-treated human subjects or rabbits (test group) were collected and passed through an ion exchange resin to isolate polar compounds. Methanolic eluates from control and test urines were analyzed by TLC. Exposure to p-dimethylaminocinnamaldehyde gave an additional intense pink band at Rt 0.40-0.45 in TLC analysis of test urine eluate when compared to control urine eluate. Non-exposed silica at this Rt was scraped and metabolites were extracted with methanol. Hydrolysis of this methanolic extract at 100 degrees C with hydrochloric acid released mexiletine. GC/MS and fast atom bombardment mass spectrometry analyses of nonhydrolyzed methanolic extracts evidenced the presence of two conjugated metabolites of mexiletine, namely, N-hydroxymexiletine glucuronide and mexiletine alcohol glucuronide. Synthetic compounds corresponding to these metabolites were obtained and spectra compared with those of isolated metabolites from urine. Definite structure assignment of N-hydroxymexiletine glucuronide was obtained from NMR spectrometry which confirmed the structure to be a hydoxylamine glucuronide (N-O-C link) and showed that the glycoside moiety was in the beta configuration. Thus, it is proposed that N-hydroxymexiletine glucuronide corresponds to mexiletine acid-labile conjugate and represents a major metabolic pathway in the disposition of mexiletine.

Characterization of digoxin and related cardiac glycosides by fast atom bombardment mass spectrometry.

The potential of using fast atom bombardment mass spectrometry for the detection and the characterization of digoxin and a series of related cardenolide analogues was investigated. The spectra were dependent upon the type of support-matrix in which they were recorded; thioglycerol proved to be satisfactory for the characterization of digoxin and allowed for its detection in human urine extract spiked with ca 11 ng ml(-1).

Fast atom bombardment mass spectrometry in the pharmaceutical analysis of drugs.

The principles, techniques and value of fast atom bombardment mass spectrometry are summarized in this revïew. Applications of the method in such areas as molecular weight determination, standard and metabolic studies, and peptide sequencing, as well as direct quantitative analysis, are surveyed, with examples from several classes of compounds with pharmacological activity.