128 resultados para High temperature liquid chromatography
Resumo:
We examine a Lipkin based two-level pairing model at finite temperature and in the thermodynamic limit. Whereas at T = 0 the model exhibits a superconducting ground state for sufficiently high values of the coupling constant, a partially superconducting phase in which some of the particles are paired, is found to survive at high temperatures in a special treatment. This phase is a mixture of abnormally-occupied eigenstates, which lie at higher energy, of the interactionless model Hamiltonian.
Resumo:
A simultaneous method for the trace determination of acidic, neutral herbicides and their transformation products in estuarine waters has been developed through an on-line solid-phase extraction method followed by liquid chromatography with diode array and mass spectrometric detection. An atmospheric pressure chemical ionization (APCI) interface was used in the negative ionization mode after optimization of the main APCI parameters. Limits of detection ranged from 0.1 to 0.02 ng/ml for 50 mi of acidified estuarine waters preconcentrated into polymeric precolumns and using time-scheduled selected ion monitoring mode. Two degradation products of the acidic herbicides (4-chloro-2-methylphenol and 2,4-dichlorophenol) did not show good signal response using APCI-MS at the concentration studied due to the higher fragmentor voltage needed for their determination For molinate and the major degradation product of propanil, 3,4-dichloroaniline, positive ion mode was needed for APCI-MS detection. The proposed method was applied to the determination of herbicides in drainage waters from rice fields of the Delta del Ebro (Spain). During the S-month monitoring of the herbicides, 8-hydroxybentazone and 4-chloro-2-methylphenoxyacetic acid were successively found in those samples. (C) 2000 Elsevier B.V. B.V. All rights reserved.
Resumo:
The 2,4-dichlorophenoxyacetic acid (2,4-D) is one of the most applied herbicides around the world to control broad leave herbs in many crops: In this study, a method was developed for simultaneous extraction and determination of 2,4D and its major transformation product, i.e., the 2,4-dichlorophenol (2,4-DCP), in soil samples. The herbicide and its degradation product were extracted twice from soil samples, after acidification, by dichloromethane on ultrasound system for 1 h. Both extracts were combined and filtrated in qualitative filter paper and Celitee. The total extract was concentrated in rotatory evaporator, dried under N-2 and finally dissolved in 1 ml of methanol. High Performance Liquid Chromatography with UV detection at 230 nm was used for analysis. Recoveries were obtained from soil samples fortified at 0.1, 1.0, 2.0, 3.0 and 4.0 mg kg(-1) levels and the results varied from 85 to 111% (for 2,4-D) and from 95 to 98% (for 2,4-DCP). For both compounds, the limits of quantification were 0.1 mg kg(-1), which were the loss level at which the accuracy and the precision were studied. Nevertheless, the limits of detection, calculated by considering the blank standard deviation and the minimum concentration level, were 0.03 and 0.02 mg kg for 2,4-D and 2,4-DCP, respectively. This proposed method was applied to soil samples of eucalyptus crops, which was previously treated with the herbicide. Despite that, neither 2,4-D nor its degradation product were detected 30 days after the herbicide application. (C) 2003 Elsevier B.V. B.V. All rights reserved.
Resumo:
The surface oxidation of UO2 sintered plates at 170-275 ° C was studied in situ by high temperature X-ray diffractometry. At very low oxygen concentration, UO2 is oxidized to U4O9, while at 300°C and argon-20 vol% oxygen it is oxidized up to U3O7. X-ray diffraction profiles of the UO2, U4O9 and U3O7 phases were well characterized during the transformations. The activation energy for the transformation of UO2 to U4O9, obtained from X-ray diffraction data, was found to be 117 ± 9 kJ/mol and 90 ± 14 kJ/mol for the β-(311) and α-(200) reflections, respectively. © 1991.
Resumo:
A rapid and sensitive method is described for the determination of clofentezine residues in apple, papaya, mango and orange. The procedure is based on the extraction of the sample with a hexane:ethyl acetate mixture (1:1, v/v) and liquid chromatographic analysis using UV detection. Mean recoveries from 4 replicates of fortified fruit samples ranged from 81% to 96%, with coefficients of variation from 8.9% to 12.5%. The detection and quantification limits of the method were of 0.05 and 0.1 mg kg-1, respectively.
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The development of fast, inexpensive, and reliable tests to identify nontuberculous mycobacteria (NTM) is needed. Studies have indicated that the conventional identification procedures, including biochemical assays, are imprecise. This study evaluated a proposed alternative identification method in which 83 NTM isolates, previously identified by conventional biochemical testing and in-house M. avium IS1245-PCR amplification, were submitted to the following tests: thin-layer chromatography (TLC) of mycolic acids and PCR-restriction enzyme analysis of hsp65 (PRA). High-performance liquid chromatography (HPLC) analysis of mycolic acids and Southern blot analysis for M. avium IS1245 were performed on the strains that evidenced discrepancies on either of the above tests. Sixty-eight out of 83 (82%) isolates were concordantly identified by the presence of IS1245 and PRA and by TLC mycolic acid analysis. Discrepant results were found between the phenotypic and molecular tests in 12/83 (14.4%) isolates. Most of these strains were isolated from non-sterile body sites and were most probably colonizing in the host tissue. While TLC patterns suggested the presence of polymycobacterial infection in 3/83 (3.6%) cultures, this was the case in only one HPLC-tested culture and in none of those tested by PRA. The results of this study indicated that, as a phenotypic identification procedure, TLC mycolic acid determination could be considered a relatively simple and cost-effective method for routine screening of NTM isolates in mycobacteriology laboratory practice with a potential for use in developing countries. Further positive evidence was that this method demonstrated general agreement on MAC and M. simiae identification, including in the mixed cultures that predominated in the isolates of the disseminated infections in the AIDS patients under study. In view of the fact that the same treatment regimen is recommended for infections caused by these two species, TLC mycolic acid analysis may be a useful identification tool wherever molecular methods are unaffordable.
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Sparfloxacin, a third generation fluoroquinolone derivative, is a potent antibacterial agent active against a wide range of Gram-positive and Gram-negative organisms including Streptococcus pneuinoniae, Staphylococcus aureus, methicillin resistant S. aureus, Legionella spp., Mycoplasina spp., Chlamydia spp. and Mycobacterium spp. A drawback of fluoroquinolones is their photoreactivity. Sparfloxacin has been studied in terms of therapeutic activities. However, there are few published of analytical methods being applied to sparfloxacin. The aim in this study was to determine the photodegradation products of sparfloxacin, when submitted to UV light, and to characterize two of these products, designated SPAX-PDP1 and SPAX-PDP2. An accelerated study of stability in methanol solution was carried out by exposing a solution of sparfloxacin to UV light (peak wavelength 290 nm) for 36 hours at room temperature. The products were analyzed by NMR spectrophotometry, IR spectrometry and mass spectrophotometry. The results suggest that the products isolated here could be used to estimate the degradation of sparfloxacin in a stability study. However, the low activity exhibited by UV-irradiated sparfloxacin is a source of concern that demands further investigation of the mechanism of its photodegradation mechanism.
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High-speed countercurrent chromatography (HSCCC) is a leading method for the fast separation of natural products from plants. It was used for the preparative isolation of two flavone monoglucosides present in the capitula of Eriocaulon ligulatum (Veil.) L.B.Smith (Eriocaulaceae). This species, known locally as botão-dourado, is exported to Europe, Japan and North America as an ornamental species, constituting an important source of income for the local population of Minas Gerais State, Brazil. The solvent system, optimized in tests prior to the HSCCC run, consisted of the two phases of the mixture ethyl acetate: n-propanol: water (140:8:80, v/v/v), which led to the successful separation of 6-methoxyluteolin-7-O-β-D-allopyranoside and 6-methoxyapigenin-7-O-β-D-allopyranoside in only 3 hours. The two flavonoids were identified by NMR (1-D and 2-D) and ESI-MS, comparing their spectra with published data.
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Recent studies have been done to achieve biomedical alloys containing non-toxic elements and presenting low elastic moduli. It has been reported that Ti-Nb-Zr alloys rich in beta phase, especially Ti-13Nb-13Zr, have potential characteristics for substituting conventional materials such as Ti-6Al-4V, stainless steel and Co alloys. The aim of this work is to study the internal friction (IF) of Ti-13Nb-13Zr (TNZ) alloy due to the importance of the absorption impacts in orthopedic applications. The internal friction of this alloy produced by arc melting was measured using an inverted torsion pendulum with the free decay method. The measurements were performed from 77 to 700 K with heating rate of 1 K/min, in a vacuum better than 10-5 mBar. The results show a relaxation structure at high temperature strongly dependent on microstructure of the material. Qualitative discussions are presented for the experimental results, and the possibility of using the TNZ as a high damping material is briefly mentioned.
Resumo:
The experiment was conducted in the experimental area belonging to the Section of Crop Production and Aromatic Medicinal Plants of the FCAV-UNESP, Jaboticabal Campus - Sao Paulo, Brazil. Tolerance to high temperature was studied in six determinate genotypes of tomato (Lycopersicon esculentum L.): Agrocica 8, Apex 1000, Botu-13, Calmech VFAS, Nemadoro and Jab-2, which were cultivated in a greenhouse at temperatures above 33oC for at least 2 h/day during blooming. The objectives of the study were to identify the genetic diversity of the genotypes studied and to determine their performance associated with tolerance to high temperature. Dissimilarity was determined by the generalized Mahalanobis distance. Delineation groups were optimized with the Tocher technique. A random block design was utilized with six treatments and with three replications. Two similarity groups were identified: 1 - Apex 1000, Botu-13, Calmech VFAS, Jab-2, Nemadoro and 2 - Agrocica 8. Crossing of genotypes within one group has no advantage because little genetic divergence and no heterotic response would be expected. However, the crossing of genotypes between groups is suggested. Knowledge of these groups will be important for efficiency future breeding efforts.
Resumo:
The study was conducted at the Section of Crop Production and Aromatic Medicinal Plants of FCAV-UNESP, Jaboticabal Campus - Sao Paulo, Brazil. Nine indeterminate tomato (Lycopersicon esculentum Mill.) genotypes, Jumbo, Santa Clara, Cláudia VF, Concorde, Débora Plus, FM-9, Carmen, Príncipe Gigante, and CL 5915, were evaluated for high temperature tolerance. Three determinate tomato genotypes, FM-9, Suncoast and TSW-10, were cultivated in a greenhouse at more than 33°C air temperature for at least 2 h/day during bloom. The objective was to identify variable genotypes to determine their tolerance of high temperature. Four replications of fifteen treatments were planted in a randomized block design. Dissimilarity was determined by the generalized Mahalanobis distance. Delineation groups were optimized with the Tocher technique. The tomatoes were classified into six groups of similar temperature responses. CL 5915 was the most tolerant of high temperatures. Crossing of genotypes within one group has no advantage because little genetic divergence and no heterotic response would be expected. However, the crossing of genotypes between groups is suggested. Knowledge of these groups will be important for efficient future breeding efforts.
Resumo:
The synergistic effect of lemon seed extract with tert-butylhydroquinone (TBHQ) in soybean oil subjected to thermoxidation by Rancimat was investigated, and the influence of these antioxidants on α-tocopherol degradation in thermoxidized soybean oil. Control, LSE (2,400 mg/kg Lemon Seed Extract), TBHQ (50 mg/kg), Mixture 1 (LSE + 50 mg/kg TBHQ) and Mixture 2 (LSE + 25 mg/kg TBHQ) were subjected to 180°C for 20 h. Samples were taken at time 0, 5, 10, 15 and 20 h intervals and analysed for oxidative stability and α-tocopherol content. LSE and Mixtures 1 and 2 showed the capacity of retarding lipid oxidation when added to soya oil and also contributed to α-tocopherol retention in oil heated at high temperatures. However, Mixtures 1 and 2 added to the oil presented a greater antioxidant power, consequently proving the antioxidants synergistic effect.
Resumo:
Annona emarginata (Schldtl.) H. Rainer (araticum-de-terra-fria) is used as a rootstock for several species of Annonaceae. It is suggested that these seeds should be sown immediately after extraction and, therefore, they could be intolerant to desiccation. There are several mechanisms involved with desiccation tolerance. Soluble sugars, for example, can accumulate and act as osmoprotectants for the membrane system during desiccation. The aim of this study is to assess desiccation tolerance in A. emarginata seeds. In addition, we examined the soluble sugars involved in desiccation tolerance. Finally, we determined the effect of gibberellic acid (GA4+7) and N-(phenylmethyl)-aminopurine in promoting the germination of seeds with different water contents. The experiment consisted of a randomized 4×5 factorial design (desiccation levels × concentration of growth regulators). After drying, seeds containing 31 (control), 19, 12 and 5% water were incubated in different concentrations of GA4+7 N-(phenylmethyl)-aminopurine (0, 250, 500, 750 and 1000 mg L-1) for 60 hours. The experiment was conducted in a germination chamber with alternating temperature and photoperiod of 20oC for 18 hours of darkness and 30oC for 6 hours of light. We analyzed electrical conductivity, germination rate, mean germination time, germination speed, frequency and uniformity of germination, percentage of dormant seeds and soluble sugar profile in intact seeds through high-performance liquid chromatography (HPLC). The data were subjected to analysis of variance, and the means were compared using Tukey's test at a threshold of p<0.05. The results showed that seeds of A. emarginata appears to be desiccation tolerant and, also, that sucrose increases when seed water content is reduced to values as low as 12%, exogenous GA4+7+N-(phenylmethyl)-aminopurine improves its germinability.