THE APPLICATION OF AUTOMATED CORRELATION OPTIMIZED WARPING TO THE QUALITY EVALUATION OF Radix Puerariae thomsonii: CORRECTING RETENTION TIME SHIFT IN THE CHROMATOGRAPHIC FINGERPRINTS

The application of automated correlation optimized warping (ACOW) to the correction of retention time shift in the chromatographic fingerprints of Radix Puerariae thomsonii (RPT) was investigated. Twenty-seven samples were extracted from 9 batches of RPT products. The fingerprints of the 27 samples were established by the HPLC method. Because there is a retention time shift in the established fingerprints, the quality of these samples cannot be correctly evaluated by using similarity estimation and principal component analysis (PCA). Thus, the ACOW method was used to align these fingerprints. In the ACOW procedure, the warping parameters, which have a significant influence on the alignment result, were optimized by an automated algorithm. After correcting the retention time shift, the quality of these RPT samples was correctly evaluated by similarity estimation and PCA. It is demonstrated that ACOW is a practical method for aligning the chromatographic fingerprints of RPT. The combination of ACOW, similarity estimation, and PCA is shown to be a promising method for evaluating the quality of Traditional Chinese Medicine.

Gastrointestinal transit of extruded or pelletized diets in pacu fed distinct inclusion levels of lipid and carbohydrate

The objective of this work was to evaluate the effect of pelletized or extruded diets, with different levels of carbohydrate and lipid, on the gastrointestinal transit time (GITT) and its modulation in pacu (Piaractus mesopotamicus). One hundred and eighty pacu juveniles were fed with eight isonitrogenous diets containing two carbohydrate levels (40 and 50%) and two lipid levels (4 and 8%). Four diets were pelletized and four were extruded. Carbohydrate and lipid experimental levels caused no changes to the bolus transit time. However, the bolus permanence time was related to diet processing. Fish fed pelletized diets exhibited the highest gastrointestinal transit time. Regression analysis of bolus behavior for pelletized and extruded diets with 4% lipid depicted different fits. GITT regression analysis of fish fed 8% lipid was fitted to a cubic equation and displayed adjustments of food permanence, with enhanced utilization of the diets, either with extruded or pelletized diets. GITT of fish fed extruded diets with 4% lipid was adjusted to a linear equation. The GITT of pacu depends on the diet processing and is affected by dietary levels of lipid and carbohydrate.

Antibacterial activity of Ocimum gratissimum L. essential oil

The essential oil (EO) of Ocimum gratissimum inhibited Staphylococcus aureus at a concentration of 0.75 mg/ml. The minimal inhibitory concentrations (MICs) for Shigella flexineri, Salmonella enteritidis, Escherichia coli, Klebsiella sp., and Proteus mirabilis were at concentrations ranging from 3 to 12 mg/ml. The endpoint was not reached for Pseudomonas aeruginosa (>=24 mg/ml). The MICs of the reference drugs used in this study were similar to those presented in other reports. The minimum bactericidal concentration of EO was within a twofold dilution of the MIC for this organism. The compound that showed antibacterial activity in the EO of O. gratissimum was identified as eugenol and structural findings were further supported by gas chromatography/mass spectra retention time data. The structure was supported by spectroscopic methods.

Biomarkers for the assessment of chlorpyrifos effects on earthworms and on soil functional parameters

The objective of this work was to evaluate the effects of chlorpyrifos on earthworms and on soil functional parameters. An integrated laboratory-field study was performed in a wheat field in Argentina, sprayed with chlorpyrifos at two recommended application rates (240 or 960 g ha-1 style='vertical-align:baseline'> a.i.). Laboratory tests included neutral red retention time, comet assay (single cell gel electrophoresis), and avoidance behavior, each using the earthworm Eisenia andrei exposed in soil collected 1 or 14 days after pesticide application, and the bait-lamina test. Field tests assessed organic matter breakdown using the litterbag and bait-lamina assays. Earthworm populations in the field were assessed using formalin application and hand-sorting. The neutral red retention time and comet assays were sensitive biomarkers to the effects of chlorpyrifos on the earthworm E. andrei; however, the earthworm avoidance test was not sufficiently robust to assess these effects. Feeding activity of soil biota, assessed by the bait lamina test, was significantly inhibited by chlorpyrifos after 97 days, but recovered by the 118th day of the test. Litterbag test showed no significant differences in comparison to controls. Earthworm abundance in the field was too low to adequately test the sensitivity of this assessment endpoint.

Identificação de componentes de óleos voláteis: Análise espectroscópica de misturas de sesquiterpenos

This paper describes a chromatographic method to fractionate volatile oils and to identify their sesquiterpenic constituents. The fractionation process includes flash chromatography over silica gel and chromatography over silica gel/AgNO3, utilising pentane, CH2Cl2 and/or acetone as eluents. GC chromatograms were obtained in order to get the relative percentage of each constituent in the volatile oils, to get the retention time value of them as well as to analyse and combine the fractions eluted from the columns. Such procedure afford mixtures of sesquiterpenes which are analysed by GC/MS, 13C and ¹H NMR.

Avaliação da salinização de açudes no semi-árido brasileiro por ICP-AES

The salt accumulation process in some reservoirs of regular and irregular use (from 10 to 50 years of constrution), located in the Southeast of Bahia State was evaluated. Inductively coupled plasma atomic emission spectrometry was used to evaluate the concentrations of Na, K, Ca and Mg in water samples from inside and upstream of the reservoirs. The results showed that for reservoirs of irregular use, the salt accumulation, indicated by the tracer Na, increases with the age of the reservoirs, however for the reservoirs of regular use the hydraulic retention time is the main parameter.

Estudo do coeficiente de partição octanol-água de bifenilas policloradas (PCBs) utilizando parâmetros topológicos

A model based on chemical structure was developed for the accurate prediction of octanol/water partition coefficient (K OW) of polychlorinated biphenyls (PCBs), which are molecules of environmental interest. Partial least squares (PLS) was used to build the regression model. Topological indices were used as molecular descriptors. Variable selection was performed by Hierarchical Cluster Analysis (HCA). In the modeling process, the experimental K OW measured for 30 PCBs by thin-layer chromatography - retention time (TLC-RT) has been used. The developed model (Q² = 0,990 and r² = 0,994) was used to estimate the log K OW values for the 179 PCB congeners whose K OW data have not yet been measured by TLC-RT method. The results showed that topological indices can be very useful to predict the K OW.

Degradação de corantes reativos pelo sistema ferro metálico/peróxido de hidrogênio

In this work the degradation of aqueous solutions of reactive azo-dyes is reported using a combined reductive/advanced oxidative process based in the H2O2/zero-valent iron system. At optimized experimental conditions (pH 7, H2O2 100 mg L-1, iron 7 g L-1) and using a continuous system containing commercial iron wool, the process afforded almost total discolorization of aqueous solutions of three reactive azo-dyes (reactive orange 16, reactive black 5 and brilliant yellow 3G-P) at a hydraulic retention time of 2.5 min. At these conditions the hydrogen peroxide is almost totally consumed while the released total soluble iron reaches a concentration compatible with the current Brazilian legislation (15 mg L-1).

Otimização e validação intralaboratorial de método para análise de resíduos de cloranfenicol em leite caprino por cromatografia gasosa com detecção por captura de elétrons (CG/DCE)

The presence of chloramphenicol residues in goat milk can cause toxic effects in the population. The present work consists of the optimization and validation of analytical methodology for determination of chloramphenicol residues in goat milk by GC/ECD. The extraction was made with ethyl acetate and the clean-up with SPE-C18. The identification was made by comparison of retention time and GC/MS, and the quantification by external standard. The method was selective, linearity (0.998), precise (5.8-13.4%), exact (69.87-73.71%) and robust. The LOD and LOQ of method were 0.030 and 0.10 μg/kg, respectively. The method was efficiently for analysis of chloramphenicol in goat milk.

Determinação de 2,5-hexanodiona em urina empregando cromatografia líquida de alta eficiência, após derivatização com 2,4-dinitrofenil-hidrazina

A method for quantifying urinary 2,5-hexanedione was optimized and validated. Urine samples were hydrolyzed and derivatized with 2,4-dinitrophenylhydrazine. The analyte was separated in a high performance liquid chromatography system with a diode array detector, using a C18 column (150 x 4.6 mm, p.d. 5 µm) and a mobile phase composed of phosphate buffer pH 2.3:acetonitrile (40:60, v/v), at a flow rate of 1 mL/min. The chromatograms were monitored at 334 nm. Retention time was 7.3 minutes. Main validation parameters were: coefficient of determination: 0.9994, accuracy: 96 to 107%; intra-assay precision (RSD): 3.08 to 6.72%; inter-assay precision (RSD): 2.54 to 8.17% and limit of quantitation of 0.19 µg/mL.

Desenvolvimento de metodologia para avaliar remoção de estrogênios em estações de tratamento de esgotos

The present research aimed to study the parameters that affect the determination of estrogens in sewage upon the use of SPE and determination by using gas chromatography mass spectrometry (GC/MS). The study evaluated the stabilization pond technology with regard to estrogens removal. The results showed that the methodology was able to identify and quantify the estrogens E1, E2, E2-17A and EE2 in sewage. Moreover, the estrogens sometimes were not removed in the stabilization pond, showing that even the high hydraulic retention time (HRT) and high sunlight intensity were not enough to degrade these compounds completely during load peaks.

Removal of organic matter and nutrients from slaughterhouse wastewater by using Eichhornia crassipes and evaluation of the generated biomass composting

The objective of this research was to evaluate the performance of the aquatic macrophyte Eichhornia crassipes applied in situ in a slaughter house treatment system, located in the west of the Paraná state, Brazil, regarding the nutrients removal and organic matter. Moreover, it aimed to obtain data from the production, management and composting practices of the biomass generated in the system. During 11 months of macrophytes development, physic and chemical parameters were monitored and plant density was controlled by periodical removal of excess biomass, which was weekly monitored and it is expressed in kg of aquatic plant per m² covered area. The degradation of the macrophytes removed from the treatment system was evaluated at the pilot scale in eight composting piles of 0.60 m³ that underwent four different treatments and two repetitions: T1 - water hyacinth (Eichhornia crassipes); T2 - water hyacinth and swine excrement (7:1), T3 - water hyacinth, swine excrement and earth (7:1:0,67), and T4 - water hyacinth, swine excrement and cellulosic gut (7:1:0,67), for a period of 90 days. The results indicated maximum removal efficiencies of 77.2% for COD; 77.8% for BOD, 87.9% for total nitrogen, 47.5% for ammonia nitrogen and 38.9% for total phosphorus for a five-day retention time. For biomass stabilization by composting, considering the C:N ratio as an indicator of compost maturity, it was observed that treatment T4 resulted in the shortest stabilization period (60 days). No difference was verified in the biostabilization rates at 5% level by the F test.

Anaerobic biodigestion of pigs feces in the initial, growing and finishing stages fed with diets formulated with corn or sorghum

The objective of this study was to evaluate the quality and the production of biogas and biofertilizer obtained from biodigester supplied with pig feces in the initial, growing and finishing stages, fed with diets formulated based on corn or sorghum. Twenty bench biodigesters were used with hydraulic retention time of 30 days and daily loads that contained 4 to 6% of total solids (TS) and 3.6 to 5.2% of volatile solids (VS). In the effluent of the biodigesters, mean levels of TS were observed ranging between 1.6 and 2.0% and of VS between 1.2 and 1.6%. The mean reductions of TS were 57.7 to 64.7% and of VS from 61.7 to 69.0%, and there was only difference in the finishing phase, in which the major averages reductions were produced by the biodigesters supplied with feces from animals fed with diets based on corn. In biodigesters supplied with feces from animals in the initial and growing stages fed with diets based on corn, were observed higher average productions of biogas and the greatest average potentials of biogas production. The average potentials obtained were 0.033; 0.181; 0.685; 0.788 and 1.132 m³ per kg of affluent, manure, TS added, VS added and VS reduced, respectively. No differences were found on the average content of methane in the biogas between diets and stages. The average concentrations of nutrients N, P, K, Ca, Mg, Na, Fe, Mn, Zn and Cu in the biodigester affluent and effluent, ranged between diets and stages.

Start-up of horizontal anaerobic reactors with sludge blanket and fixed bed for wastewater treatment from coffee processing by wet method

In this study it was evaluated the start-up procedures of anaerobic treatment system with three horizontal anaerobic reactors (R1, R2 and R3), installed in series, with volume of 1.2 L each. R1 had sludge blanket, and R2 and R3 had half supporter of bamboo and coconut fiber, respectively. As an affluent, it was synthesized wastewater from mechanical pulping of the coffee fruit by wet method, with a mean value of total chemical oxygen demand (CODtotal) of 16,003 mg L-1. The hydraulic retention time (HRT) in each reactor was 30 h. The volumetric organic loading (VOL) applied in R1 varied from 8.9 to 25.0 g of CODtotal (L d)-1. The mean removal efficiencies of CODtotal varied from 43 to 97% in the treatment system (R1+R2+R3), stabilizing above 80% after 30 days of operation. The mean content of methane in the biogas were of 70 to 76%, the mean volumetric production was 1.7 L CH4 (L reactor d)-1 in the system, and the higher conversions were around at 0.20 L CH4 (g CODremoved)-1 in R1 and R2. The mean values of pH in the effluents ranged from 6.8 to 8.3 and the mean values of total volatile acids remained below 200 mg L-1 in the effluent of R3. The concentrations of total phenols of the affluent ranged from 45 to 278 mg L-1, and the mean removal efficiency was of 52%. The start-up of the anaerobic treatment system occurred after 30 days of operation as a result of inoculation with anaerobic sludge with active microbiota.

Performance of UASB reactors in two stages under different HRT and OLR treating residual waters of swine farming

In this study it was evaluated the effects of hydraulic retention time (HRT) and Organic Loading Rate (OLR) on the performance of UASB (Upflow Anaerobic Sludge Blanket) reactors in two stages treating residual waters of swine farming. The system consisted of two UASB reactors in pilot scale, installed in series, with volumes of 908 and 188 L, for the first and second stages (R1 and R2), respectively. The HRT applied in the system of anaerobic treatment in two stages (R1 + R2) was of 19.3, 29.0 and 57.9 h. The OLR applied in the R1 ranged from 5.5 to 40.1 kg CODtotal (m³ d)-1. The average removal efficiencies of chemical oxygen demand (COD) and total suspended solids (TSS) ranged, respectively, from 66.3 to 88.2% and 62.5 to 89.3% in the R1, and from 85.5 to 95.5% and 76.4 to 96.1% in the system (R1 + R2). The volumetric production of methane in the system (R1 + R2) ranged from 0.295 to 0.721 m³CH4 (m³ reactor d)-1. It was found that the OLR applied were not limiting to obtain high efficiencies of CODtotal and TSS removal and methane production. The inclusion of the UASB reactor in the second stage contributed to increase the efficiencies of CODtotal and TSS removal, especially, when the treatment system was submitted to the lowest HRT and the highest OLR.