Gemifloxacin mesylate: UV spectrophotometric method for quantitative determination using experimental design for robustness

This study describes the validation of UV spectrophotometric method for quantitative determination of gemifloxacin mesylate (GFM) in tablets using methanol as solvent. The method was specific, linear, precise, exact and robust at 272 and 343 nm. The results confirmed that the method in both wavelengths is valid and useful to the routine quality control of GFM in coated tablets. The validate method was compared to liquid chromatography (HPLC), microbiological assay and visible (VIS) spectrophotometry, which were previously developed and validated to the same drug. There was not significative difference between the methods for GFM quantitation.

Optimisation of the lipase-catalysed preparation of a nucleoside prodrug model using an experimental design methodology

The preparation of 2', 3'-di-O-hexanoyluridine (2) by a Candida antarctica B lipase-catalysed alcoholysis of 2', 3', 5'-tri-O-hexanoyluridine (1) was optimised using an experimental design. At 25 ºC better experimental conditions allowed an increase in the yield of 2 from 80% to 96%. In addition to the yield improvement, the volume reaction could be diminished in a factor of 5 and the reaction time significantly shortened.

Nanoparticle-coated organic-inorganic microparticles: experimental design and gastrointestinal tolerance evaluation

The influences of the spray-drying parameters and the type of nanoparticles (nanocapsules or nanospheres) on the characteristics of nanoparticle-coated diclofenac-loaded microparticles were investigated by using a factorial design 3². Gastrointestinal tolerance following oral administration in rats was evaluated. Formulations were selected considering the best yields, the best encapsulation efficiencies and the lowest water contents, presenting surfaces completely coated by nanostructures and a decrease in the surface areas in relation to the uncoated core. In vitro drug release demonstrated the influence of the nanoparticle-coating on the dissolution profiles of diclofenac. Nanocapsule-coated microparticles presented a protective effect on the gastrointestinal mucosa.

Use of experimental design in the optimisation of a solid phase preconcentration system for Cobalt determination by GFAAS

In this work is proposed a solid phase preconcentration system of Co2+ ions and its posterior determination by GFAAS in which fractional factorial design and response surface methodology (RSM) were used for optimization of the variables associated with preconcentration system performance. The method is based on cobalt extraction as a complex Co2+-PAN (1:2) in a mini-column of polyurethane foam (PUF) impregnated with 1-(2-pyridylazo)-naphthol (PAN) followed by elution with HCl solution and its determination by GFAAS. The chemical and flow variables studied were pH, buffer concentration, eluent concentration and preconcentration and elution flow rates. Results obtained from fractional factorial design 2(5-1) showed that only the variables pH, buffer concentration and interaction (pH X buffer concentration) based on analysis of variance (ANOVA) were statistically significant at 95% confidence level. Under optimised conditions, the method provided an enrichment factor of 11.6 fold with limit of detection and quantification of 38 and 130 ng L-1, respectively, and linear range varying from 0.13 to 10 µg L-1. The precision (n = 9) assessed by relative standard deviation (RSD) was respectively 5.18 and 2.87% for 0.3 and 3.0 µg L-1 cobalt concentrations.

Docosahexaenoic acid ethyl esther (DHAEE) microcapsule production by spray-drying: optimization by experimental design

Docosahexaenoic acid is an essential polyunsaturated fatty acid with important metabolic activities. Its conjugated double bonds make it susceptible to decomposition. Its stability may be improved through fatty acid entrapment with a spray-drying technique; however, the many parameters involved in this technique must be considered to avoid affecting the final product quality. Therefore, this study aimed to evaluate the entrapment conditions and yields of fish oil enriched with docosahexaenoic acid ethyl ester. Microcapsules were obtained from Acacia gum using a spray-drying technique. The experimental samples were analyzed by chromatography and delineated by Statistica software, which found the following optimum entrapment conditions: an inlet temperature of 188 °C; 30% core material; an N2 flow rate of 55 mm; and a pump flow rate of 12.5 mL/minute. These conditions provided a 66% yield of docosahexaenoic acid ethyl ester in the oil, corresponding to 19.8% of entrapped docosahexaenoic acid ethyl ester (w/w). This result was considered significant since 30% corresponded to wall material.

Application of Doehlert experimental design in the optimization of experimental variables for the Pseudozyma sp. (CCMB 306) and Pseudozyma sp. (CCMB 300) cell lysis

This study aimed to verify the influence of pH and temperature on the lysis of yeast using experimental design. In this study, the enzymatic extract containing β-1,3-glucanase and chitinase, obtained from the micro-organism Moniliophthora perniciosa, was used. The experiment showed that the best conditions for lysis of Pseudozyma sp. (CCMB 306) and Pseudozyma sp. (CCMB 300) by lytic enzyme were pH 4.9 at 37 ºC and pH 3.9 at 26.7 ºC, respectively. The lytic enzyme may be used for obtaining various biotechnology products from yeast.

Inactivation of Staphylococcus aureus in raw salmon with supercritical CO2 using experimental design

Abstract Considering the microbial safety of consumption of raw foods (Asian food), this study aimed to explore the inactivation S. aureus in raw salmon by supercritical CO2 treatment (SC-CO2). For this purpose, experimental design methodology was employed as a tool to evaluate the effects of pressure (120-220 bar), the depressurization rate (10 to 100 bar.min–1) and the salmon:CO2 mass relation (1:0.2 to 1:1.0). It was observed that the pressure and the depressurization rate was statistically significant, i.e. the higher the system pressure and depressurization rate, the greater the microbial inactivation. The salmon: CO2 mass relation did not influence the S. aureus inactivation in raw salmon. There was a total reduction in S. aureus with 225 bar, a depressurizing rate of 100 bar.min–1, a salmon: CO2 mass relation of 1:0.6, for 2 hours at 33 °C.

Efeito da adição de precursores na produção de alcaloide anticancerígeno usando a técnica de planejamento experimental

The effect of precursors on the anticancer alkaloid production by submerged fermentation using M. anisopliae 3935 was studied, according to complete experimental design 2² with three central points. The results showed that lysine was the most important variable, however, when both lysine and glucose were added to the fermentation medium, the alkaloid production reached, approximately, 17 mg L-1 after 120 hours of fermentation. Then, the scale-up of the process was carried out and these results were confirmed. Finally, 35 mg L-1 of alkaloid at 192 h were attained after increment of added aminoacid lysine.

Otimização das condições de extração de saponinas em Ampelozizyphus amazonicus usando planejamento experimental e metodologia de superfície de resposta

This works describes the use of experimental design and surface response methodology for optimization of saponin extraction from Ampelozizyphus amazonicus. For this purpose, a method employing extraction based on maceration assisted by ultrasound technique was utilized. The following factors were studied: extraction length of time and solvent composition. The total saponin was determined by using a gravimetric method and the results expressed by their relative proportion to total crude extract. For the specific condition, 60% hydro-alcoholic solution and 18 minutes extraction length of time has shown the best results. This method can be useful for extraction of substances with biological importance

OTIMIZAÇÃO DO PROCESSO DE TRANSESTERIFICAÇÃO EM DUAS ETAPAS PARA PRODUÇÃO DE BIODIESEL ATRAVÉS DO PLANEJAMENTO EXPERIMENTAL DOEHLERT

In this work, Doehlert experimental design was used to optimize the Transesterification Double Step Process (TDSP) method of methyl soybean oil biodiesel production which starts with a basic catalysis followed by an acidic catalysis. The conversion values were calculated from NMR spectra. Response surface was used to show the results of the interactions between the variables. This experimental design evaluated variables like catalyst and alcohol amount for the basic catalysis and time and temperature for the acidic catalysis. According to results obtained after Doehlert design application the alcohol amount was the main factor that influenced on the basic catalysis but for the acidic catalysis both time and temperature are important and their effects are opposite. It resulted on excellent conversions for both steps obtaining for the basic catalysis about 100% when was used like optimal conditions catalyst amount equal to 0.40 g and volume of methanol equal to 60 mL and for the acidic catalysis about 99% when was used like optimal conditions temperature of 65 °C and 90 minutes for reaction time.

Development of experimental structure and influence of high CO2 concentration in maize cro

Maize is a C4 plant that shows few or no response to high [CO2]. Thus, this study aimed to analyze the photosynthetic rate and yield of maize under high [CO2] and develop open-top chambers (OTC) to create an atmosphere enriched with CO2. The experiment was conducted between October 2008 and March 2009. The OTCs were developed in modular scheme. Measurement of photosynthetic rates, transpiration, stomata conductance, grain yield and dry matter were performed. The experimental design was randomized blocks with four replications and three treatments: P1 - plants grown in OTC with 700 ppm [CO2], P2 - plants grown in OTC with environmental [CO2], and P3 - control, cultivated in open field. The results were analyzed by ANOVA and Tukey's test (Pr< 0.05). The chambers can reduce by 25% the photosynthetically active radiation and increase the air and leaf temperatures. Plants under high [CO2] (P1) showed the highest photosynthetic rates and the lowest stomata conductance and transpiration. The total weight of grains (g) and dry mass of shoots (g) showed no increases for P1, despite their higher photosynthetic rates.

Inoculation with Azospirillum, associated with nitrogen fertilization in maize

The biological nitrogen fixation is an alternative to supply the nitrogen needed for maize. The objective of this study was to evaluate the development and yield of maize in response to inoculation with Azospirillum associated with nitrogen fertilization. We conducted two field experiments in the summer harvest, the first in the 2000/2001 crop year in the region of Marechal Cândido Rondon, under conventional tillage, and second in the 2002/2003 agricultural year in the region of Cascavel, under no tillage. The experimental design in both experiments was a randomized complete block, with four replications, 2x2x2 factorial, with two levels of nitrogen at sowing (zero and 20 kg ha-1), two levels of inoculum (zero and 200 g ha-1) and two levels of nitrogen in topdressing (zero and 100 kg ha-1). There was evaluated the height of ear insertion, total plant height, leaf N content, shoot dry biomass and grain yield. The height of ear insertion and total plant height were not influenced by the factors under study. Nitrogen fertilization at sowing increased the leaf N content, causing the opposite effect when combined with inoculation. Inoculation with Azospirillum in the absence of nitrogen, provide productivity increases of 15.4% and 7.4% for 2000/2001 and 2002/2003 crops, respectively. The inoculation provided productivity similar to that obtained with 100 kg ha-1 in topdressing in crop 2000/2001, while in association with the topdressing, reduced productivity and shoot dry biomass in crop 2002/2003.

Availability of heavy metals in contaminated soil evidenced by chemical extractants

Heavy metals have been accumulating in Brazilian soils, due to natural processes, such as atmospheric deposition, or human industrial activities. For certain heavy metals, when in high concentrations in the soil, there is no specific extractant to determine the availability of these elements in the soil. The objective of the present study was to evaluate the availability of Cd, Cu, Fe, Mn, Pb and Zn for rice and soybeans, using different chemical extractants. In this study we used seven soil samples with different levels of contamination, in completely randomized experimental design with four replications. We determined the available concentrations of Cd, Cu, Fe, Mn, Pb and Zn extracted by Mehlich-1, HCl 0.1 mol L-1, DTPA, and organic acid extractants and the contents in rice and soybeans, which extracts were analyzed by ICP-OES. It was observed that Mehlich-1, HCl 0.1 mol L-1 and DTPA extractants were effective to assess the availability of Cd, Cu, Pb and Zn for rice and soybeans. However, the same was not observed for the organic acid extractant.

Soybean growth and yield after single tillage and species mixture of cover plants

The use of cover crops is important for the agricultural crop and soil management in order to improve the system and, consequently, to increase yield. Therefore, the present study analyzed the effect of crop residues of black oat (Avena strigosa Schreb.) (BO) and a cocktail (CO) of BO, forage turnip (Raphanus sativus L.) (FT) and common vetch (Vicia sativa L.) (V) on the emergence speed index (ESI), seedling emergence speed (SES) plant height and soybean yield in different intervals between cover crop desiccation with glyphosate 480 (3 L ha-1) and BRS 232 cultivar sowing. Plots of 5 x 2.5 m with 1 m of border received four treatments with BO cover crops and four with CO as well as a control for each cover crop, at random, with five replications. The plots were desiccated in intervals of 1, 10, 20 and 30 days before soybean seeding. The harvest was manual while yield was adjusted to 13% of moisture content. The experimental design was completely randomized with splitplots and means compared by the Scott and Knott test at 5% of significance. The results showed that CO of cover crops can be recommended for soybean to obtain a more vigorous seedling emergence, from 10 days after cover crop desiccation.

Morphology and stability of aggregates of an Oxisol according to tillage system and gypsum application

Morphological characterization and aggregate stability is an important factor in evaluating management systems. The aim of this paper is to evaluate the stability and morphology of the aggregates of a dystrophic Oxisol managed with no-tillage and conventional tillage with and without the residual action of gypsum. The experimental design was randomized blocks arranged in split-split plot, where the treatments were two soil management systems (plots) with 0 and 2000 kg ha-1 of gypsum (subplots) and five depths (0-0.05, 0.05-0.10, 0.10-0.15, 0.15-0.20 and 0.20-0.30 m) as the subsubplots, with four replications. The aggregate morphology was determined through images and later evaluated by the Quantporo software. Stability was determined by the wet method. The results showed that the no-tillage system, with or without gypsum residual effect, provided the aggregates with the largest geometric diameters. The combination of no-tillage system and the gypsum residual effect provided rougher aggregates.