Extraction and isolation of dictamnine, obacunone and fraxinellone from Dictamnus dasycarpus Turcz. by supercritical fluid extraction and high-speed counter-current chromatography

Supercritical fluid extraction was used to extract active compounds from the Chinese traditional medicinal D. dasycarpus under the pressure of 30 MPa and temperature of 45 ºC. Further separation and purification was established by high-speed counter-current chromatography (HSCCC) with a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (1:0.8:1.3:0.9, volume ratio). The separation yielded a total of 47 mg of dictamnine, 24 mg of obacunone and 83 mg of fraxinellone from 1.0 g of the crude extract in one step separation with the purity of 99.2, 98.4 and 99.0%, respectively, as determined by HPLC. The chemical structures of these compounds were identified by ESI-MS, IR, ¹H-NMR and 13C-NMR.

Performance characteristics of high performance liquid chromatography, first order derivative UV spectrophotometry and bioassay for fluconazole determination in capsules

The bioassay, first order derivative UV spectrophotometry and chromatographic methods for assaying fluconazole capsules were compared. They have shown great advantages over the earlier published methods. Using the first order derivative, the UV spectrophotometry method does not suffer interference of excipients. Validation parameters such as linearity, precision, accuracy, limit of detection and limit of quantitation were determined. All methods were linear and reliable within acceptable limits for antibiotic pharmaceutical preparations being accurate, precise and reproducible. The application of each method as a routine analysis should be investigated considering cost, simplicity, equipment, solvents, speed, and application to large or small workloads.

Preparative separation and purification of bufadienolides from ChanSu by high-speed counter-current chromatography combined with preparative HPLC

Eight bufadienolides were successfully isolated and purified from ChanSu by high-speed counter-current chromatography (HSCCC) combined with preparative HPLC (prep-HPLC). First, a stepwise elution mode of HSCCC with the solvent system composed of petroleum ether - ethyl acetate - methanol - water (4:6:4:6, 4:6:5:5, v/v) was employed and four bufadienolides, two partially purified fractions were obtained from 200 mg of crude extract. The partially purified fractions III and VI were then further separated by prep-HPLC, respectively, and another four bufadienolides were recovered. Their structures were confirmed by ESI-MS and ¹H-NMR spectra.

Preparative separation of polyphenols from artichoke by polyamide column chromatography and high-speed counter-current chromatography

An efficient method for the rapid separation and purification of polyphenols from artichoke by polyamide column chromatography in combination with high-speed counter-current chromatography (HSCCC) was successfully built. The crude ethanol extracts from dry artichoke were first pre-separated by polyamide column chromatography and divided in two parts as sample 1 and sample 2. Then, the samples were further separated by HSCCC and yielded 7.8 mg of chlorogenic acid (compound I), 24.5 mg of luteolin-7-O-β-D-rutinoside (compound II), 18.4 mg of luteolin-7-O-β-D-glucoside (compound III), and 33.4 mg of cynarin (compound IV) with purity levels of 92.0%, 98.2%, 98.5%, and 98.0%, respectively, as determined by high-performance liquid chromatography (HPLC) method. The chemical structures of these compounds were identified by electrospray ionization-mass spectrometry (ESI-MS) and nuclear magnetic resonance (NMR).

Separation and purification of three stilbenes from the radix of Polygonum cillinerve (Nakai) Ohwl by macroporous resin column chromatography combined with high-speed counter-current chromatography

An effective method for the rapid separation and purification of three stilbenes from the radix of Polygonum cillinerve (Nakai) Ohwl by macroporous resin column chromatography combined with high-speed counter-current chromatography (HSCCC) was successfully established. In the present study, a two-phase solvent system composed of chloroform-n-butanol-methanol-water (4:1:4:2, v/v/v/v) was used for HSCCC separation. A one-step separation in 4 h from 150 mg of crude extract produced 26.3 mg of trans-resveratrol-3-O-glucoside, 42.0 mg of pieceid-2"-O-gallate, and 17.9 mg of trans-resveratrol with purities of 99.1%, 97.8%, and 99.4%, respectively, as determined by high-performance liquid chromatography (HPLC). The chemical structures of these compounds were identified by nuclear magnetic resonance (NMR) spectroscopy.

DESENVOLVIMENTO DE UMA TÉCNICA ULTRASSÔNICA PARA AVALIAR TEORES DE ÓLEO E GRAXA EM EFLUENTES DE BIOCOMBUSTÍVEIS

Ultrasound as a metrology tool has many applications in health care, industrial, and chemical analyses. Ultrasonic techniques are rapid, low-cost, non-invasive, and highly repeatable. Although ultrasound can be used to measure emulsions, no effort had been made thus far to optimize its sensitivity for metrological analysis. In this work, a technique for analyzing oil in water was validated. The wave velocity and attenuation were chosen as the ultrasonic parameters. The technique was implemented in the boundary region established by law for effluents from industrial plants involved with biofuel manufacturing. A technical effort of this study was to establish stable emulsions in concentrations close to the desired limit of study. The phase behaviours of pseudo-ternary oil, sodium chloride, and sodium lauryl sulphate were studied. The composition in the widest region of the diagram allowed for the formation of a stable emulsion, from which the ultrasound measurement was carried out. An analytical curve was obtained using ultrasonic attenuation to determine the content of oils and greases in wastewater ranging 15–240 ppm. The speed of sound did not appear to be an applicable parameter for this application. The technique was demonstrated to be an important alternative solution for the continuous monitoring of wastewater with regard to oil concentrations.

Performance of spray nozzles in land applications with high speed

The aim of this study was to evaluate different spray nozzles for land applications in high speed on the coverage and deposit in soybean plants pulverization. It was evaluated the AXI 110 04 plane jet nozzles operated at speed of 4.17m.s-1 (control), the grey APE and the AXI 110 08 plane jets, and the TD HiSpeed 110 06 and AXI TWIN 120 06 twin jets, at speed of 9.72m.s-1. The application volume was fixed in 120L ha-1. The application efficiency was evaluated by two different methods: analysis of the coverage area using fluorescent pigment and UV light and analysis of deposits through the recovery and quantification of FD&C N°1 brilliant blue marker by spectrophotometry. Both analyses were done in samples collected from top, middle and bottom parts of the plants. The spray nozzles showed differences in coverage and deposit pattern, so in the top part, the coverage was increased with smaller drops and the deposits were increased with medium drops. In the other parts of the plants, there were no statistical differences between the treatments for both coverage and deposits. The displacement speed did not influence the application efficiency for nozzles with the same drop pattern, and the obtained spray coverage and deposits at the medium and bottom parts of the plants were less than 50% of that found at the top of the soybean plants.

Spraying systems and traveling speed in the deposit and spectrum of droplets in cotton plant

ABSTRACT Tractor traveling speed can influence the quality of spraying depending on the application technology used. This study aimed to evaluate the droplet spectrum, the deposition and uniformity of spray distribution with different spraying systems and traveling speeds of a self-propelled sprayer in two phenological stages of the cotton plant (B9 and F13). The experimental design was randomized blocks and treatments were three spraying techniques: common flat spray tips; tilted flat jet with air induction, at 120 L ha-1; and rotary atomizer disk, 20 L ha-1, combined with four traveling speeds: 12, 15, 18 and 25 km h-1, with four replications. Spraying deposition was evaluated for both leaf surfaces from the cotton plant apex and base (stage B9) and middle part of the plant (stage F13) with a cupric marker. A laser particle analyzer also assessed the droplet spectrum. The centrifugal power spray system produces more homogeneous droplet spectrum and increased penetration of droplets into the canopy in both phenological stages. Variation on the operating conditions necessary for increased traveling speed negatively influences the pattern of spraying deposits.

Acute and chronic nervous signs in cattle associated with Phalaris angusta poisoning in Argentina

Phalaris angusta is a South American natural grass that produces poisoning in sheep and cattle in Argentina and Brazil. Phalaris spp. can produce unrelated forms of poisoning in ruminants, acute and chronic syndromes. The objective of this paper was to describe an outbreak of acute and chronic Phalaris nervous syndrome in 53 of 980 fattening steers and heifers in a farm of Buenos Aires province. On September of 2006 the animals developed nervous signs and died after 3-5 days. The herd was removed to a phalarisfree pasture. Three months later (on December) 15 new clinical cases developed in the herd. Necropsy performed in one affected calf showed neither grossly nor microscopic changes. Microscopically, there were no major alterations in tissues. Nervous signs had been described in some field cases where neither pigment deposition nor axonal degeneration could be detected. Clinical findings displayed by affected cattle after consumption of Phalaris angusta pastures resemble those observed by other authors in Phalaris staggers. This is the first report in Argentina where both syndromes were seen in the same herd.

Histopathology of dairy cows' hooves with signs of naturally acquired laminitis

The purpose of this study was to investigate histological changes in dairy cows' hooves with or without injuries from naturally acquired laminitis. Cull cows with no clinical signs of hoof abnormalities (G1, n=9) and those with macroscopic lesions associated with laminitis without (G2, n=23) or with lameness (G3, n=7) were used in the study. After slaughter, samples of dermo-epidermal junctions of sole, axial and dorsal regions of the hoof were obtained and histologically processed using HE and PAS staining. Congestion, hemorrhage and inflammatory infiltrate in the dermis of sole, axial and dorsal regions were blindly and semiquantitatively evaluated by the same researcher. Inflammatory infiltrate was evaluated in the dermal laminae of axial and dorsal regions. The morphology of epidermal cells and the presence of irregularities in three regions of the basement membrane (BM) length were examined using PAS staining. Scores of lesions in different regions of the hoof in the same group and in different groups for each region of the hoof were compared using non-parametric analyses. Inflammatory infiltrate in the dermis of all regions of the hoof was detected in all groups with no significant statistical difference. Cows with no clinical signs of hoof abnormalities secondary to laminitis (G1) have inflammation scores and epidermal cell changes similar to those of groups with laminitis injuries, suggesting the existence of a prodromal phase for this disease in bovines. BM had irregularities with a variable intensity along its length, however, with no difference among groups. The pattern of BM irregularities found has not been reported so far and does not resemble the BM collapse described in horses and cattle with induced acute laminitis. Is it concluded that even in the absence of macroscopic hoof signs associated to laminitis, dairy cows have histological injuries compatible with inflammation of the dermo-epidermal junction as in affected animals. Basement membrane of cows with or without laminitis associated lesions had irregularities with an irregular distribution along its length which need to be further studied.

Curving simulation and stability of a creep-controlled wheelset for high speed rail-vehicles

Higher travel speeds of rail vehicles will be possible by developing sophisticated top performance bogies having creep-controlled wheelsets. In this case the torque transmission between the right and the left wheel is realized by an actively controlled creep coupling. To investigate hunting stability and curving capability the linear equations of motion are written in state space notation. Simulation results are obtained with realistic system parameters from industry and various controller gains. The advantage of the „creep-controlled wheelset" is discussed by comparison the simulation results with the dynamic behaviour of the special cases „solid-axle wheelset" and „loose wheelset" (independent rotation of the wheels). The stability is also investigated with a root-locus analysis.

On the development of an unstructured grid solver for inert and reactive high speed flow simulations

An unstructured grid Euler solver for reactive compressible flow applications is presented. The method is implemented in a cell centered, finite volume context for unstructured triangular grids. Three different schemes for spatial discretization are implemented and analyzed. Time march is implemented in a time-split fashion with independent integrators for the flow and chemistry equations. The capability implemented is tested for inert flows in a hypersonic inlet and for inert and reactive supersonic flows over a 2-D wedge. The results of the different schemes are compared with each other and with independent calculations using a structured grid code. The strengths and the possible weaknesses of the proposed methods are discussed.

A modified contour error controller for a high speed XY table

This article deals with a contour error controller (CEC) applied in a high speed biaxial table. It works simultaneously with the table axes controllers, helping them. In the early stages of the investigation, it was observed that its main problem is imprecision when tracking non-linear contours at high speeds. The objectives of this work are to show that this problem is caused by the lack of exactness of the contour error mathematical model and to propose modifications in it. An additional term is included, resulting in a more accurate value of the contour error, enabling the use of this type of motion controller at higher feedrate. The response results from simulated and experimental tests are compared with those of common PID and non-corrected CEC in order to analyse the effectiveness of this controller over the system. The main conclusions are that the proposed contour error mathematical model is simple, accurate, almost insensible to the feedrate and that a 20:1 reduction of the integral absolute contour error is possible.

Speed Control of an Autonomous Mobile Robot: Comparison between a PID Control and a Control Using Fuzzy Logic

An Autonomous Mobile Robot battery driven, with two traction wheels and a steering wheel is being developed. This Robot central control is regulated by an IPC, which controls every function of security, steering, positioning localization and driving. Each traction wheel is operated by a DC motor with independent control system. This system is made up of a chopper, an encoder and a microcomputer. The IPC transmits the velocity values and acceleration ramp references to the PIC microcontrollers. As each traction wheel control is independent, it's possible to obtain different speed values for each wheel. This process facilities the direction and drive changes. Two different strategies for speed velocity control were implemented; one works with PID, and the other with fuzzy logic. There were no changes in circuits and feedback control, except for the PIC microcontroller software. Comparing the two different speed control strategies the results were equivalent. However, in relation to the development and implementation of these strategies, the difficulties were bigger to implement the PID control.

Clinical signs of pneumonia in children: association with and prediction of diagnosis by fuzzy sets theory

The present study compares the performance of stochastic and fuzzy models for the analysis of the relationship between clinical signs and diagnosis. Data obtained for 153 children concerning diagnosis (pneumonia, other non-pneumonia diseases, absence of disease) and seven clinical signs were divided into two samples, one for analysis and other for validation. The former was used to derive relations by multi-discriminant analysis (MDA) and by fuzzy max-min compositions (fuzzy), and the latter was used to assess the predictions drawn from each type of relation. MDA and fuzzy were closely similar in terms of prediction, with correct allocation of 75.7 to 78.3% of patients in the validation sample, and displaying only a single instance of disagreement: a patient with low level of toxemia was mistaken as not diseased by MDA and correctly taken as somehow ill by fuzzy. Concerning relations, each method provided different information, each revealing different aspects of the relations between clinical signs and diagnoses. Both methods agreed on pointing X-ray, dyspnea, and auscultation as better related with pneumonia, but only fuzzy was able to detect relations of heart rate, body temperature, toxemia and respiratory rate with pneumonia. Moreover, only fuzzy was able to detect a relationship between heart rate and absence of disease, which allowed the detection of six malnourished children whose diagnoses as healthy are, indeed, disputable. The conclusion is that even though fuzzy sets theory might not improve prediction, it certainly does enhance clinical knowledge since it detects relationships not visible to stochastic models.