Determination of phenobarbital in human plasma by a specific liquid chromatography method: application to a bioequivalence study

A liquid chromatography method was developed and validated for the determination of phenobarbital in human plasma using phenytoin as internal standard. The drugs were extracted from plasma by liquid-liquid extraction and separated isocratically on a C12 analytical column, maintained at 35 ºC, with water:acetonitrile:methanol (58.8:15.2:26, v/v/v) as mobile phase, run at a flow rate of 1.2 mL/min with detection at 205 nm. The method was linear in the range of 0.1-4 μg/mL (r²=0.9999) and demonstrated acceptable results for the precision, accuracy and stability studies. The method was successfully applied for the bioequivalence study of two tablet formulations (test and reference) of phenobarbital 100 mg after single oral dose administration to healthy human volunteers.

Comparação interlaboratorial para análise de dureza total e cloreto em água

Interlaboratorial comparison of the determination of hardness and chloride in water had been performed by 38 and 37 laboratories, respectively. In all cases the participating laboratories used its routine methods. Homogeneity and stability testing were performed on the samples sent to the laboratories. The codified results are graphically reported and compared to assigned value, determined by the consensus of the laboratories. Satisfactory results were obtained for 71 and 73% of the laboratories, considering hardness and chloride determination, respectively.

Sensitive method for determination of piplartine, an alkaloid amide from Piper species, in rat plasma samples by liquid chromatography-tandem mass spectrometry

Piplartine (PPTN) is an alkaloid amide found in Piper species that presents different activities. PPTN determination in rat plasma is necessary to better understand its biological effects. The aim of this study was to develop a sensitive LC-MS/MS method for the determination of PPTN in rat plasma. The performance criteria for linearity, sensitivity, precision, accuracy, recovery, and stability have been assessed and were within the recommended guidelines. The validated method proved to be suitable in a pilot study of PPTN kinetic disposition in rat plasma after a single intraperitoneal dose, and represents an appropriate tool to further pharmacokinetic studies.

A Theoretical investigation of a potential high energy density compound 3,6,7,8-tetranitro-3,6,7,8-tetraaza-tricyclo[3.1.1.1(2,4)]octane

The B3LYP/6-31G (d) density functional theory (DFT) method was used to study molecular geometry, electronic structure, infrared spectrum (IR) and thermodynamic properties. Heat of formation (HOF) and calculated density were estimated to evaluate detonation properties using Kamlet-Jacobs equations. Thermal stability of 3,6,7,8-tetranitro-3,6,7,8-tetraaza-tricyclo [3.1.1.1(2,4)]octane (TTTO) was investigated by calculating bond dissociation energy (BDE) at the unrestricted B3LYP/6-31G(d) level. Results showed the N-NO2 bond is a trigger bond during the thermolysis initiation process. The crystal structure obtained by molecular mechanics (MM) methods belongs to P2(1)/C space group, with cell parameters a = 8.239 Å, b = 8.079 Å, c = 16.860 Å, Z = 4 and r = 1.922 g cm-3. Both detonation velocity of 9.79 km s-1 and detonation pressure of 44.22 GPa performed similarly to CL-20. According to the quantitative standards of energetics and stability, TTTO essentially satisfies this requirement as a high energy density compound (HEDC).

Caracterización de cristales líquidos por microscopía óptica en sistemas surfactante polietoxilado-alcano-agua

The phase behavior of an alcohol polyethoxylated surfactant with decane and dodecane oil phase varying the water proportion from 5 to 90% to determine compositions in which the formation of liquid crystals and microemulsions ocurred was investigated. Pseudoternary phase diagrams were built to represent the regions of liquid crystals, biphases and microemulsions. Polarized light optical microscopy was used for the analysis and characterization of the separate phases. The micrographs obtained showed characteristics of hexagonal and lamellar phases of liquid crystal, isotropic phases, microemulsions and vesicles. This study is important to propose hypothesis regarding the factors determining the formation and stability of phases composed by surfactant/oil/water systems.

Advances in ethanol reforming for the production of hydrogen

Catalytic steam reforming of ethanol (SRE) is a promising route for the production of renewable hydrogen (H2). This article reviews the influence of doping supported-catalysts used in SRE on the conversion of ethanol, selectivity for H2, and stability during long reaction periods. In addition, promising new technologies such as membrane reactors and electrochemical reforming for performing SRE are presented.

Equilibrium studies of 2,2'-(5-bromo-6-methylpyrimidine-2,4-diyl)bis(azanediyl)dipropanoic acid with some transition-metal ions in aqueous solution

The stability constants of the 1:1 complexes formed between M2+ (M2+: Mn2+, Ni2+, Cu2+, or Cd2+) and BMADA2- (BMADA: 2,2'-(5-bromo-6-methylpyrimidine-2,4 diyl)bis(azanediyl)dipropanoic acid) were determined by potentiometric pH titration in aqueous solution (I = 0.1 mol L-1, NaNO3, 25 °C). The stability of the binary M - BMADA complexes is determined by the basicity of the carboxyl or amino groups. All the stability constants reported in this work exhibit the usual trend, and the order obtained was Mn2+< Ni2+ < Cu2+ > Cd2+. The observed stability order for BMADA approximately follows the Irving - Williams sequence. In the M - BMADA complexes, the M ion is able to form a macrochelate via the pyrimidine group of BMADA.

Efeito da variação de parâmetros reacionais na preparação de grafeno via oxidação e redução do grafite

This work shows the influence of several reactional parameters for obtaining graphene through successive steps of oxidation and exfoliation of bulk graphite (resulting in graphene oxide), followed by chemical reduction. The results showed that changes in temperature, reaction time, reducing agent and source of primary graphite lead to different surface compositions and stability in dispersion of graphene oxide. Also, the use of different reducing agents promoted different degrees of restoration of C=C bonds in the bidimensional structure of graphene.

Spectrophotometric determination of diclofenac in pharmaceutical preparations assisted by microwave oven

In this work, an effective and low-cost method for the determination of sodium or potassium diclofenac is proposed in its pure form and in their pharmaceutical preparations. The method is based on the reaction between diclofenac and tetrachloro-p-benzoquinone (p-chloranil), in methanol medium. This reaction was accelerated by irradiating of reactional mixture with microwave energy (1100 W) during 27 seconds, producing a charge transfer complex with a maximum absorption at 535 nm. The optimal reaction conditions values such as reagent concentration, heating time and stability of the reaction product were determined. Beer's law is obeyed in a concentration range from of 1.25x10-4 to 2.00x10-3 mol l-1 with a correlation coefficient of 0.9993 and molar absorptivity of 0.49 x10³ l mol-1 cm-1. The limit of detection (LOD) was 1.35x10-5 mol l-1 and the limit of quantification (LOQ) was 4.49x10-5 mol l-1. In the presence of the common excipients, such as glucose, lactose, talc, starch, magnesium stearate, sodium sulphite, titanium dioxide, polyethyleneglycol, polyvinylpirrolidone, mannitol and benzilic alcohol no interferences were observed. The analytical results obtained by applying the proposed method compare very favorably with those given by the United States Pharmacopeia standard procedure. Recoveries of diclofenac from various pharmaceutical preparations were within 95.9% to 103.3%, with standard deviations ranging from 0.2% to 1.8%.

Euroopan keskuspankin julkaisut

Euroopan keskuspankin (perustamisvuosi 1999) tehtävänä on ylläpitää hinta- ja rahoitusjärjestelmän vakautta ja toteuttaa rahapolitiikkaa euroalueella. Euroalueeseen kuuluvat kaikki euron käyttöönsä ottaneet jäsenmaat, joita on 17. Euroopan rahapoliittinen instituutti (EMI) toimi EKP:n edeltäjänä ja sen tehtävänä oli keskuspankkien välisen yhteistyön lujittaminen, rahapolitiikan yhteensovittaminen ja yhteiseen valuuttaan siirtyminen. Kokoelma sisältää Euroopan keskuspankin ja Euroopan rahapoliittisen instituutin (EMI) julkaisuja vuodesta 1994 lähtien. Tutkimusjulkaisuja on mm. EU-maiden hintavakaudesta, rahapolitiikasta, rahoitusmarkkinoista, maksujärjestelmistä, valuuttapolitiikasta, yhdentymisestä ja finanssivalvonnasta. Kokoelmassa on vuosikertomuksia, kuukausikatsauksia (Monthly Bulletin), lehtiä, tilastoja, työpapereita, raportteja ja tutkimusjulkaisuja. Kokoelmassa on n. 1655 nimekettä, ja painettu kokoelma kasvaa Euroopan keskuspankin julkaisuilla. Euroopan rahapoliittisen instituutin julkaisut loppuivat v. 1999. Kokoelman julkaisuista n. 80 % on ilmestynyt v. 2000 - 2009. Valtaosa on englanninkielisiä, mutta julkaisuja on myös suomeksi ja ruotsiksi. Painettu kokoelma on Suomen Pankin kirjaston avokokoelmassa vapaasti käytettävissä ja kopioitavissa maksutta. Suurin osa on saatavana myös verkkojulkaisuina Euroopan keskuspankin sivuilta http://www.ecb.int.

Soil physical attributes in chemigated banana plantation with wastewater

ABSTRACT The feasibility of using sewage wastewater as a water and nutrient source for plants is an alternative to harness agricultural natural resource, observing its influence on the organic matter dynamics and soil energy. Our objective here was to evaluate the effects of applying different doses of effluent from a sewage treatment plant, in Janaúba – MG, Brazil, over the physical attributes of a soil grown with “Prata Anã” banana. From soil sample collection at depths of 0-20, 20-40, and 40-60 cm, we determined the following soil properties: soil density, total porosity, macroporosity, microporosity, organic matter, clay dispersed in water and stability of soil aggregate. The experimental design was in randomized blocks with four repetitions. Wastewater raising doses promoted increase in suspended solids, contributing to macroporosity reduction at 20-40 and 40-60 cm depths; as well as a reduction in organic matter within 0-20 cm layer. Clay dispersal was observed in the depths of 0-20 cm, being derived from an increase in sodium content. Concurrently, there was a reduction of soil aggregate stability.

Muutos ja pysyvyys Turun Akatemian luonnonfilosofiassa 1600-luvulla

Kirjallisuusarvostelu

Täyteainepitoisuuden ja retentioainesysteemin optimointi

Työssä tutkittiin tarrapaperikoneen pohjapaperin täyteainepitoisuuden nostamisen vaikutusta koneen ajettavuuteen ja paperin ominaisuuksiin. Työn tavoitteena oli löytää ne prosessitekniset keinot, joilla voitaisiin saavuttaa raskaiden pintapapereiden tavoitetuhkatasot. Lisäksi pyrittiin optimoimaan retentioaineiden annokset ja ajotavat korkeilla tuhkatasoilla. Kirjallisuusosassa tarkasteltiin pinta- ja kolloidikemian perusteita sekä täyteainepitoisuuden vaikutusta paperin ominaisuuksiin ja prosessoitavuuteen. Lisäk-si syvennyttiin märänpään kemiaan selvittämällä mm. kalsiumkarbonaatin vesiliuoskemiaa ja erilaisten retentioaineiden ominaisuuksia ja niiden reaktiomekanismeja. Työn kokeellinen osa koostui kahdesta koeajosta. Ensimmäisessä koeajossa selvitettiin täyteainesaostumien muodostumismekanismeja ja paperikoneen ajettavuutta täyteainepitoisuutta nostettaessa yli raskaiden pintapapereiden tavoitetasojen. Saadut tulokset osoittivat, että märänpään kemiantila pysyi koeajon aikana muuttumattomana eikä mitään saostumien muodostumista havaittu. Täyteainepitoisuudessa päästiin 3 % yli lajikohtaisen tuhkatavoitteen ilman ajettavuusongelmia. Toisessa koeajossa keskityttiin erityisesti märänpään retentioaineiden määrien optimointiin ja paperin laatuominaisuuksiin. Koeajossa täyteainepitoisuutta nostettiin yli tavoitetasojen. Saadut tulokset osoittivat, että täyteainepitoisuuden nostolla ei ollut vaikutusta paperin laatuun tai paperikoneen ajettavuuteen. Massatärkkelyksen avulla pystyttiin korvaamaan kationisen polymeerin retentiovaste ja kompensoimaan täyteainepitoisuuden noston myötä tullut paperin lujuuksien lasku. Koeajoissa ja prosessin seurannassa tuli ilmi myös useita eri tekijöitä, joilla oli vaikutusta retentioon, retentioaineiden tehoon ja prosessin stabiilisuuteen. Tehdyistä yksittäisistä havainnoista on hyötyä pyrittäessä ymmärtämään märänpään prosessin tilaa ja sen vaikutusta paperikoneen ajettavuuteen. Työ saavutti sille asetetut tavoitteet ja sen ansiosta paperikoneen märänpään raaka-aineiden ja kemikaalien syöttösuhteita pystyttiin muuttamaan tavalla, joka vähensi paperinvalmistuksen kustannuksia ilman että paperin laatuominaisuudet huononivat.

Characterization of nitrate reductase activity in vitro in Gracilaria caudata J. Agardh (Rhodophyta, Gracilariales)

The marine red alga Gracilaria caudata J. Agardh has been used in Brazil for agar extraction, mainly in the northeast region of the country. Nitrogen availability is the most important abiotic factor in seawater that limits the growth of seaweeds. The enzyme nitrate reductase (NR) is the key regulatory point in the nitrogen assimilation in photosynthetic organisms. This study describes an in vitro assay, characterizing the enzymatic activity of NR in terms of kinetic constants and stability, its oscillation during the day and glucose effect on NR modulation. Maximal peaks of NR activity were recorded at 20 ºC and pH 8.0. The enzymatic stability in crude extracts stored at 3 ± 1 ºC decreased significantly after 48 hours. Apparent Michaelis-Menten constants (K M) for NADH and nitrate were 22 µM and 3.95 mM, respectively. Gracilaria caudata NR activity showed an oscillation under light:dark photoperiod (14:10 hours LD) with 3-fold higher activity during the light phase, peaking after 10 hours of light. Under optimal assay conditions, the maximal activity was 92.9 10-3 U g-1. The addition of glucose induced the enzymatic activity during the light and dark phase, evidencing a possible modulation of this enzyme by the photosynthesis. This relationship can be explained by the need of carbon skeletons, produced by the photosynthetic process, to incorporate the intermediary metabolites of nitrate assimilatory pathway, avoiding the toxic intracellular accumulation of nitrite and ammonium. The optimization of enzymatic assay protocols for NR is essential to establish appropriate conditions to study nutritional behaviour, compare different taxonomic groups and to understand its regulatory mechanism.

The effect of performing corrections on reported uterine cancer mortality data in the city of São Paulo

Reports of uterine cancer deaths that do not specify the subsite of the tumor threaten the quality of the epidemiologic appraisal of corpus and cervix uteri cancer mortality. The present study assessed the impact of correcting the estimated corpus and cervix uteri cancer mortality in the city of São Paulo, Brazil. The epidemiologic assessment of death rates comprised the estimation of magnitudes, trends (1980-2003), and area-level distribution based on three strategies: i) using uncorrected death certificate information; ii) correcting estimates of corpus and cervix uteri mortality by fully reallocating unspecified deaths to either one of these categories, and iii) partially correcting specified estimates by maintaining as unspecified a fraction of deaths certified as due to cancer of "uterus not otherwise specified". The proportion of uterine cancer deaths without subsite specification decreased from 42.9% in 1984 to 20.8% in 2003. Partial and full corrections resulted in considerable increases of cervix (31.3 and 48.8%, respectively) and corpus uteri (34.4 and 55.2%) cancer mortality. Partial correction did not change trends for subsite-specific uterine cancer mortality, whereas full correction did, thus representing an early indication of decrease for cervical neoplasms and stability for tumors of the corpus uteri in this population. Ecologic correlations between mortality and socioeconomic indices were unchanged for both strategies of correcting estimates. Reallocating unspecified uterine cancer mortality in contexts with a high proportion of these deaths has a considerable impact on the epidemiologic profile of mortality and provides more reliable estimates of cervix and corpus uteri cancer death rates and trends.