Sugars and char formation on subcritical water hydrolysis of sugarcane straw.

Subcritical water has potential as an environmentally friendly solvent for applications including hydrolysis, liquefaction, extraction, and carbonization. Here, we report hydrolysis of sugarcane straw, an abundant byproduct of sugar production, in a semi-continuous reactor at reaction temperatures ranging from 190 to 260°C and at operating pressures of 9 and 16MPa. The target hydrolysis products were total reducing sugars. The main products of sugarcane straw hydrolysis were glucose, xylose, arabinose, and galactose in addition to 5- hydroxymethylfurfural and furfural as minor byproducts. Fourier transform infrared spectroscopy and thermogravimetric analysis provided additional information on the surface and bulk composition of the residual biomass. Char was present on samples treated at temperatures equal to and greater than 190°C. Samples treated at 260°C contained approximately 20wt% char, yet retained substantial hemicellulose and cellulose content. Hydrolysis temperature of 200°C provided the greatest TRS yield while minimizing char formation.

Comparison of different types of stationary phases for the analysis of soy isoflavones by HPLC.

Nowadays, there are new technologies in high-performance liquid chromatography columns available enabling faster and more efficient separations. In this work, we compared three different types of columns for the analysis of main soy isoflavones. The evaluated columns were a conventional reverse phase particle column, a fused-core particle column, and a monolithic column. The comparison was in terms of chromatographic parameters such as resolution, asymmetry, number of theoretical plates, variability of retention time, and peak width. The lower column pressure was provided by the monolithic column, although lower chromatographic performance was achieved. Conventional and fused-core particle columns presented similar pressure. Results also indicate that direct transfer between particle and monolithic columns is not possible requiring adjustment of conditions and a different method optimization strategy. The best chromatographic performance and separation speed were observed for the fused-core particle column. Also, the effect of sample solvent on the separation and peak shape was evaluated and indicated that monolithic column is the most affected especially when using higher concentrations of acetonitrile or ethanol. Sample solvent that showed the lowest effect on the chromatographic performance of the columns was methanol. Overall evaluation of methanol and acetonitrile as mobile phase for the separation of isoflavones indicated higher chromatographic performance of acetonitrile, although methanol may be an attractive alternative. Using acetonitrile as mobile phase resulted in faster, higher resolution, narrower, and more symmetric peaks than methanol with all columns. It also generated the lower column pressure and flatter pressure profile due to mobile phase changes, and therefore, it presents a higher potential to be explored for the development of faster separation methods.

Fast and simultaneous determination of phenolic compounds and caffeine in teas, mate, instant coffee, soft drink and energetic drink by high-performance liquid chromatography using a fused-core column.

A fast HPLC method with diode-array absorbance detector and fluorescence detector for the analysis of 19 phenolic acids, flavan-3-ols, flavones, flavonols and caffeine in different types of samples was developed. Using a C(18) reverse-phase fused-core column separation of all compounds was achieved in less than 5 min with an overall sample-to-sample time of 10 min. Evaluation of chromatographic performance revealed excellent reproducibility, resolution, selectivity and peak symmetry. Limits of detection for all analyzed compounds ranged from 0.5 to 211 µg L(-1), while limits of quantitation ranged between 1.5 and 704 µg L(-1). The developed method was used for the determination of analytes present in different samples, including teas (black, white, green), mate, coffee, cola soft drink and an energetic drink. Concentration of the analyzed compounds occurring in the samples ranged from 0.4 to 314 mg L(-1). Caffeine was the analyte found in higher concentrations in all samples. Phytochemical profiles of the samples were consistent with those reported in the literature.

Fast analysis of isoflavones by high-performance liquid chromatography using a column packed with fused-core particles.

The recent development of fused-core technology in HPLC columns is enabling faster and highly efficient separations. This technology was evaluated for the development of an fast analysis method for the most relevant soy isoflavones. A step-by-step strategy was used to optimize temperature (25-50°C), flow rate (1.2-2.7 mL/min), mobile phase composition and equilibration time (1-5 min). Optimized conditions provided a method for the separation of all isoflavones in less than 5.8 min and total analysis time (sample-to-sample) of 11.5 min. Evaluation of chromatographic performance revealed excellent reproducibility, resolution, selectivity, peak symmetry and low limits of detection and quantification levels. The use of a fused-core column allows highly efficient, sensitive, accurate and reproducible determination of isoflavones with an outstanding sample throughout and resolution. The developed method was validated with different soy samples with a total isoflavone concentration ranging from 1941.53 to 2460.84 µg g(-1) with the predominant isoflavones being isoflavone glucosides and malonyl derivatives.

Sample preparation for the analysis of isoflavones from soybeans and soy foods.

This manuscript provides a review of the actual state and the most recent advances as well as current trends and future prospects in sample preparation and analysis for the quantification of isoflavones from soybeans and soy foods. Individual steps of the procedures used in sample preparation, including sample conservation, extraction techniques and methods, and post-extraction treatment procedures are discussed. The most commonly used methods for extraction of isoflavones with both conventional and "modern" techniques are examined in detail. These modern techniques include ultrasound-assisted extraction, pressurized liquid extraction, supercritical fluid extraction and microwave-assisted extraction. Other aspects such as stability during extraction and analysis by high performance liquid chromatography are also covered.