Simultaneous determination of non-steroidal anti-inflammatory drugs in pharmaceutical formulations and human serum by reversed phase high performance liquid chromatography

A rapid and sensitive method using high performance liquid chromatography has been developed and validated for the simultaneous determination of non-steroidal anti-inflammatory drugs (NSAIDs) in pharmaceutical formulations and human serum. Six NSAIDs including: naproxen sodium, diclofenac sodium, meloxicam, flurbiprofen, tiaprofenic and mefenamic acid were analyzed simultaneously in presence of ibuprofen as internal standard on Mediterranea C18 (5 µm, 250 x 0.46 mm) column. Mobile phase comprised of methanol: acetonitrile: H2O (60:20:20, v/v; pH 3.35) and pumped at a flow rate of 1 mL min-1 using 265 nm UV detection. The method was linear over a concentration range of 0.25-50 µg mL-1 (r² = 0.9999).

Drogas de abuso em águas naturais e residuárias urbanas: ocorrência, determinação e aplicações forenses

Drugs of abuse are commonly used outside medical or legal settings where their production, marketing and consumption are subject to legal summons and/or intervention. Classified as emerging contaminants, these substances have been recently detected in samples of environmental concern, such as waters and wastewaters. This review presents the state-of-the-art on the methodological approaches used in sample preparation, the main techniques applied in analytical determination at trace levels, as well as the use of information related to the drug or its metabolite concentration in sewage samples to empirically estimate the consumption of drugs of abuse in a city or region.

Quantification of beta-lactam antibiotics in veterinary drugs: amoxicillin and ampicillin determination by high performance liquid chromatography

This work focused on the development and validation of an RP-HPLC-UV method for quantification of beta-lactam antibiotics in three pharmaceutical samples. Active principles analyzed were amoxicillin and ampicillin, in 3 veterinary drugs. Mobile phase comprised 5 mmol L-1 phosphoric acid solution at pH 2.00, acetonitrile with gradient elution mode and detection wavelength at 220 nm. The method was validated according to the Brazilian National Health Surveillance regulation, where linear range and linearity, selectivity, precision, accuracy and ruggedness were evaluated. Inter day precision and accuracy for pharmaceutical samples 1, 2 and 3 were: 1.43 and 1.43%; 4.71 and 3.74%; 2.72 and 1.72%, respectively, while regression coefficients for analytical curves exceeded 0.99. The method had acceptable merit figure values, indicating reliable quantification. Analyzed samples had active principle concentrations varying from -12 to +21% compared to manufacturer label claims, rendering the medicine unsafe for administration to animals.

Lipase-catalyzed Approaches towards Secondary Alcohols: Intermediates for Enantiopure Drugs

The use of enantiopure intermediates for drug synthesis is a trend in pharmaceutical industry. Different physiological effects are associated with the enantiomers of chiral molecules. Thus, the safety profile of a drug based on an enantiopure active pharmaceutical ingredient is more reliable. Biocatalysis is an important tool to access enantiopure molecules. In biocatalysis, the advantage of selectivity (chemo-, regio- and stereoselectivity) is combined with the benefits of a green synthesis strategy. Chemoenzymatic syntheses of drug molecules, obtained by combining biocatalysis with modern chemical synthesis steps usually consists of fewer reaction steps, reduced waste production and improved overall synthetic efficiency both in yields and enantio- and/or diastereoselectivities compared with classical chemical synthesis. The experimental work together with the literature review clearly indicates that lipase catalysis is highly applicable in the synthesis of enantiopure intermediates of drug molecules as the basis to infer the correct stereochemistry. By lipase catalysis, enantiopure secondary alcohols used as intermediates in the synthesis of Dorzolamide, an antiglaucoma drug, were obtained. Enantiopure _-hydroxy nitriles as potential intermediates for the synthesis of antidepressant drugs with 1-aryl-3- methylaminopropan-1-ol structure were also obtained with lipases. Kinetic resolution of racemates was the main biocatalytic approach applied. Candida Antarctica lipase B, Burkholderia cepacia lipase and Thermomyces lanuginosus lipase were applied for the acylation of alcohols and the alcoholysis of their esters in organic solvents, such as in diisopropyl ether and tert-butyl methyl ether. Candida Antarctica lipase B was used under solvent free conditions for the acylation of ethyl 3-hydroxybutanoate.

Wood consumption rates of forest species by subterranean termites (Isoptera) under field conditions

Termites are well -known for their capacity to damage and destroy wood and wood products of all kinds in the tropics and subtropics. A field test was undertaken to evaluate variations in wood consumption of Pinus sp. and three species of Eucalyptus by subterranean termites. The test consisted of wooden stakes of each species being initially submitted to water immersion for 0, 24, 48 and 72 h, and buried in the ground to natural infestation by subterranean termites for an exposure period of 30, 45 and 60 days. Three species of subterranean termites were identified: Heterotermes longiceps (Snyder), Coptotermes gestroi (Wasmann) (Isoptera: Rhinotermitidae), and Nasutitermes jaraguae (Holmgren) (Isoptera: Termitidae). This is the first record of occurrence of H. longiceps in the state of Rio de Janeiro. Although the wood-consumption rates were not correlated significantly with their wood densities, there was a tendency of the softwoods (E. robusta and Pinus sp.) to be more consumed by subterranean termites than the woods of intermediate hardness (E. pellita and E. urophylla). Among the eucalyptus, E. robusta showed to be more susceptible to attack by subterranean termites than E. pellita and E. urophylla

Reduction of specific energy consumption of a thermomechanical pulping plant

Kuumahiertoprosessi on erittäin energiaintensiivinen prosessi, jonka energianominaiskulutus (EOK) on yleisesti 2–3.5 MWh/bdt. Noin 93 % energiasta kuluu jauhatuksessa jakautuen niin, että kaksi kolmasosaa kuluu päälinjan ja yksi kolmasosa rejektijauhatuksessa. Siksi myös tämän työn tavoite asetettiin vähentämään energian kulutusta juuri pää- ja rejektijauhatuksessa. Päälinjan jauhatuksessa tutkimuskohteiksi valittiin terityksen, tehojaon ja tuotantotason vaikutus EOK:een. Rejektijauhatuksen tehostamiseen pyrittiin yrittämällä vähentää rejektivirtaamaa painelajittelun keinoin. Koska TMP3 laitoksen jauhatuskapasiteettia on nostettu 25 %, tavoite oli nostaa päälinjan lajittelun kapasiteettia saman verran. Toisena tavoitteena oli pienentää rejektisuhdetta pää- ja rejektilajittelussa ja siten vähentää energiankulutusta rejektijauhatuksessa. Näitä tavoitteita lähestyttiin vaihtamalla päälinjan lajittimiin TamScreen-roottorit ja rejektilajittimiin Metso ProFoil-roottorit ja optimoimalla kuitufraktiot sihtirumpu- ja prosessiparametrimuutoksin. Syöttävällä terätyypillä pystyttiin vähentämään EOK:ta 100 kWh/bdt, mutta korkeampi jauhatusintensiteetti johti myös alempiin lujuusominaisuuksiin, korkeampaan ilmanläpäisyyn ja korkeampaan opasiteettiin. Myös tehojaolla voitiin vaikuttaa EOK:een. Kun ensimmäisen vaiheen jauhinta kuormitettiin enemmän, saavutettiin korkeimmillaan 70 kWh/bdt EOK-vähennys. Tuotantotason mittaamisongelmat heikensivät tuotantotasokoeajojen tuloksia siinä määrin, että näiden tulosten perusteella ei voida päätellä, onko EOK tuotantotasoriippuvainen vai ei. Päälinjan lajittelun kapasiteettia pystyttiin nostamaan TS-roottorilla vain 18 % jääden hieman tavoitetasosta. Rejektilajittelussa pystyttiin vähentämään rejektimäärää huomattavasti Metso ProFoil-roottorilla sekä sihtirumpu- ja prosessiparametrimuutoksin. Lajittamokehityksellä saavutettu EOK-vähennys arvioitiin massarejektisuhteen pienentymisen ja rejektijauhatuksessa käytetyn EOK:n avulla olevan noin 130 kWh/bdt. Yhteenvetona voidaan todeta, että tavoite 300 kWh/bdt EOK-vähennyksestä voidaan saavuttaa työssä käytetyillä tavoilla, mikäli niiden täysi potentiaali hyödynnetään tuotannossa.

Water consumption when exposed to sun and shade for native goats in the semiarid of the State of Paraiba, Brazil

This work aimed to evaluate the preference and water consumption of native goats in the semiarid of Brazil. The water was freely supplied, in individual buckets, one exposed to the sun and the other in the shade. The experiment was realized using 18 animals of Moxotó, Graúna and Azul breeds, with average weight of 16,6 ± 2,4 kg, kept in confinement in individual stalls equipped with feeders and drinkers, during the period from January to February of 2009. The water temperature was measured by sensors (thermocouples type T - copper/constantan), which were coupled to a system of data acquisition. It was observed that the average water temperature exposed to the sun was 29.02 ºC, and 23.85 ºC in the shade. For all breeds there was a preference for the water exposed to the sun, corresponding to an average consumption of 64.71% of the total. Among the breeds, the greatest preference for water exposed to the sun was the Azul (71.18%), followed by the Moxotó (65.95%) and the Graúna (57.00%). The animals consumed more water during the day, and the average water consumption was 1.15 grams day-1, corresponding to 6.9 % of body weight of the animals.

Fuel consumption of a tractor in function of wear, of ballasting and tire inflation pressure

When using appropriate inflation pressures and load capacity (ballast), it may obtain a higher yield and prolongation of the life of the tire, besides it may minimize the problems of loss of traction, increased slippage and fuel consumption. This study aimed to evaluate the fuel consumption of a tractor operating with new and worn tires in three conditions of ballasting and three inflation pressures, when driving on compacted soil with vegetation cover. The experiment was conducted at the experimental unit from the Department of Animal Science, Federal University of Lavras, state of Minas Gerais, Brazil, in an agricultural soil compacted by cattle trampling and with vegetation cover. It was used a tractor 4x2 with front wheel assist, of a 65.62 kW engine power. The tires were of R1 type, diagonal (front: 12.4 to 24; and rear: 18.4 to 30), the average height of the clutches of the new tires were 0.3 and 0.35 m for front and rear tires, respectively, and for the worn tires were 0.018 and 0.0045 m, for the front and the rear tires, respectively. The results showed advantages for the tractor equipped with new tires.

Crop coefficient and water consumption of eggplant in no-tillage system and conventional soil preparation

Under organic management in Seropédica-RJ, Brazil, using a weighing lysimeter, the crop coefficients (kc), the maximum evapotranspiration and the productivity of eggplant cultivation under two cropping systems (no tillage with straw plus soil with conventional preparation) were determined. A whole randomized layout with two treatments (no tillage and conventional) and five replicates during 134 days of cultivation were adopted. There were no significant differences in the eggplant cultivation in the two cropping systems, with a maximum commercial productivity obtained from 47.42 Mg ha-1 for the no-tillage system, and 47.91 Mg ha-1 for the conventional tillage. The accumulated ETc was 285.15 and 323.44 mm for the no-tillage and conventional, respectively. The crop coefficients value for the phases: 1 - transplanting, flowering, 2 - flowering-fruiting, 3 - fruit- first harvesting, 4- first harvesting of the final crop cycle was 0.83, 0.77, 0.90 and 0.97 in no-tillage system for the respective phases and for the conventional one 0.81, 1.14, 1.17 and 1.05 for the same steps described above.

Identification and application of bile metabolites to assess the exposure of fish to pharmaceuticals in the environment

Thousands of tons of pharmaceuticals are consumed yearly worldwide. Due to the continuous and increasing consumption and their incomplete elimination in wastewater treatment plants (WWTP), pharmaceuticals and their metabolites can be detected in receiving waters, although at low concentrations (ng to low μg/L). As bioactive molecules the presence of pharmaceuticals in the aquatic environment must be considered potentially hazardous for the aquatic organisms. In this thesis, the biotransformation and excretion of pharmaceuticals in fish was studied. The main biotransformation pathways of three anti‐inflammatory drugs, diclofenac, naproxen and ibuprofen, in rainbow trout were glucuronidation and taurine conjugation of the parent compounds and their phase I metabolites. The same metabolites were present in fish bile in aquatic exposures as in fish dosed with intraperitoneal injection. Higher bioconcentration factor in bile (BCFbile) was found for ibuprofen when compared to diclofenac and naproxen. Laboratory exposure studies were followed by a study of uptake of pharmaceuticals in a wild fish population living in lake contaminated with WWTP effluents. Of the analyzed 17 pharmaceuticals and six phase I metabolites, only diclofenac, naproxen and ibuprofen was present in bream and roach bile. It was shown, that diclofenac, naproxen and ibuprofen excreted by the liver can be found in rainbow trout and in two native fish species living in the receiving waters. In the bream and roach bile, the concentrations of diclofenac, naproxen and ibuprofen were roughly 1000 times higher than those found in the lake water, while in the laboratory exposures, the bioconcentration of the compounds and their metabolites in rainbow trout bile were at the same level as in wild fish or an order of magnitude higher. Thus, the parent compounds and their metabolites in fish bile can be used as a reliable biomarker to monitor the exposure of fish to environmental pharmaceuticals present in water receiving discharges from WWTPs.