Stability indicating HPLC method for simultaneous determination of moxifloxacin hydrochloride and ketorolac tromethamine in pharmaceutical formulations

A simple, RP-HPLC method was established for determining moxifloxacin and ketorolac in pharmaceutical formulations. Moxifloxacin, ketorolac and their degradation products were separated using C8 column with methanol and phosphate buffer pH 3.0 (55:45 v/v) as the mobile phase. Detection was performed at 243 nm using a diode array detector. The method was validated using ICH guidelines and was linear in the range 20-140 µg mL-1 for both analytes. Good separation of both the analytes and their degradation products was achieved using this method. The developed method can be applied successfully for the determination of moxifloxacin and ketorolac.

Determinação de bussulfano em plasma através de cromatografia líquida de alta eficiência com detector de arranjo de diodos e derivatização com dietilditiocarbamato de sódio

A high performance liquid chromatographic-diode array detection method for the determination of busulfan in plasma was developed and validated. Sample preparation consisted of protein precipitation followed by derivatization with sodium diethyldithiocarbamate and liquid-liquid extraction with methyl-tert-butyl ether. Chromatograms were monitored at 277 nm. Separation was carried out on a Lichrospher RP 18 column (5 µm, 250 x 4 mm). The mobile phase consisted of water and acetonitrile (20:80, v/v). The method presented adequate specificity, linearity, precision and accuracy and allowed reliable determination of busulfan in clinical plasma samples, being applied to three patients submitted to bone marrow transplantation.

Máscaras mecânicas de sombra por eletrocorrosão para dispositivos eletro-ópticos

Shadow masks are used in manufacturing processes for electro-optic devices to transfer patterns with different shapes and dimensions. For fabrication of organic based devices, shadow masks should be made of materials stable against organic solvents, high temperature, and robust, remaining unchanged after multiple cycles of use and fixation. Thus, stainless steel is suitable for shadow masks. A simple, cheap and quick method of obtaining shadow masks by electrochemical corrosion of stainless steel is reported. The shadow mask was used to evaporate cathode material to obtain an organic light emitting diode with active area of 9 mm². This device exhibited a turn-on voltage of 5 V and luminance of 14 cd/m².

Isolamento do verbacosídeo e validação de método analítico para padronização do extrato bruto das partes aéreas de Buddleja stachyoides Cham. & Schltdl. (Scrophulariaceae)

Phenylpropanoid glycoside verbascoside was isolated and identified from the ethyl acetate fraction of the aerial parts of Buddleja stachyoides Cham. & Schltdl. by 1H-NMR. A method using high-performance liquid chromatography has been developed and validated for determination of verbascoside in alcoholic crude extract of the aerial parts of B. stachyoides. Analysis was performed on a Phenomenex® Gemini-NX C18 analytical column (250 mm × 4.6 mm; 5 µm) using a mobile phase (pump A - aqueous solution containing H2SO4 (0.01 M), H3PO4 (0.4%), and (C2H5)2NH (0.4%); pump B - methanol:aqueous (95:5) solution containing H2SO4 (0.05 M), H3PO4 (2%), and (C2H5)2NH (0.2%); pump C - acetonitrile:aqueous (90:10) solution containing H2SO4 (0.05 M) and H3PO4 (2%)) and a diode array detector at 325 nm. The method was validated in accordance with ANVISA guidelines and may be applied to quality control of herbal medicine with aerial parts of B. stachyoides.

Phenolic composition and antioxidant properties of Brazilian honeys

The antioxidant activities and polyphenolic levels of "assa peixe," "cambara," and "morrão de candeia" Brazilian honeys were investigated. Phenolic extracts of 11 honeys were evaluated spectrophotometrically to determine their total phenolic and flavonoid contents, and their antioxidant activities were measured using DPPH, ABTS, and FRAP assays. High-performance liquid chromatography coupled with diode array detection was applied to determine the phenolic composition of the honey extracts. The presence of fourteen phenolic compounds was established (eleven phenolic acids and three flavonoids), as well as HMF and abscisic acid. Principal component analysis was applied to classify the honey samples according to their floral origins.

DETECTION AND QUANTIFICATION OF PHYTOCHEMICAL MARKERS OF Ilex paraguariensis BY LIQUID CHROMATOGRAPHY

Ilex paraguariensis (yerba-mate) is used as a beverage, and its extract requires adequate quality control methods in order to guarantee quality and safe use. Strategies to develop and optimize a chromatographic method to quantify theobromine, caffeine, and chlorogenic acid in I. paraguariensis extracts were evaluated by applying a quality by design (QbD) model and ultra high-performance liquid chromatography (UHPLC). The presence of these three phytochemical markers in the extracts was evaluated using UHPLC-MS and was confirmed by the chromatographic bands in the total ion current traces (m/z of 181.1 [M+H]+, 195.0 [M+H]+, and 353.0 [M−H]−, respectively). The developed method was then transferred to a high-performance liquid chromatography (HPLC) platform, and the three phytochemical markers were used as external standards in the validation of a method for analyses of these compounds in extracts using a diode array detector (DAD). The validated method was applied to quantify the chlorogenic acid, caffeine, and theobromine in the samples. HPLC-DAD chromatographic fingerprinting was also used in a multivariate approach to process the entire data and to separate the I. paraguariensis extracts into two groups. The developed method is very useful for qualifying and quantifying I. paraguariensis extracts.

COMPARAÇÃO DE MÉTODOS POR CROMATOGRAFIA LÍQUIDA NA DETERMINAÇÃO DE MULTIRRESÍDUOS DE AGROTÓXICOS EM MORANGOS

Liquid chromatography is often used for the determination of pesticide multiresidues in foods. In Brazil, the strawberry crop is an example of a food with high levels of irregularities because of the application of pesticides. This is a major concern from the perspective of food safety, environmental protection, and certification for food export. The purpose of this study is to evaluate and compare chromatographic separation and detection methods in relation to a newly developed and validated method using ultra high performance liquid chromatography (LC) coupled with tandem mass spectrometry (MS/MS) for the analytical determination of pesticides in strawberries. The comparisons were based on evaluations of the analysis time, consumption of the solvent in the mobile phase, injection volume, detectability, matrix effect, and recovery. The results showed that the LC–MS/MS and UHPLC–MS/MS techniques were both extremely efficient at analyzing pesticide residues with different physico-chemical parameters that were present at low concentrations in a complex matrix. The UHPLC separation method provided better chromatographic performance and productivity, which contributed favorably to routine analytical determinations. Detection by MS/MS had better detectability and selectivity compared with the diode array detector.

ESTUDO FITOQUÍMICO, ATIVIDADE ANTIMICROBIANA E CITOTÓXICA DE ESPÉCIMES DE Leonotis nepetifolia L. R. (Br)

Specimens of Leonotis nepetiflolia were obtained from cultivated and wild environments to verify their influences in chemical composition. Phytochemical analyses were conducted for the ethyl acetate phase obtained by partitioning the crude ethanol extract from the cultivated leaves of L. nepetifolia. In doing so, flavonoid 3',4',5-trimethoxy-6,7-dihidroxyflavone (cirsiliol), a chemotaxonomic marker of the family Lamiaceae, was isolated. The results reveal that all phases and extracts tested exhibited weak to moderate antimicrobial activity against the strains of bacteria tested. The evaluation of in vitrocytotoxic and antitumor activity showed that the ethyl acetate phases obtained from both wild and cultivated leaves exhibit high potential cytotoxic and antitumor (> 78.0% of inhibition) activity. The major component of these phases was identified by high-performance liquid chromatography-diode array detector and nuclear magnetic resonance analyses using both 1D and 2D methods. The results further indicate that the flavonoid cirsiliol is the agent responsible for the activity observed in these phases.

MCR-ALS APLICADO NO MONITORAMENTO QUANTITATIVO DO PROCESSO DE ELETRODEGRADAÇÃO DA ATRAZINA USANDO ESPECTROS UV: RESULTADOS COMPARATIVOS COM HPLC-DAD COMO UM MÉTODO DE REFERÊNCIA

Electrodegradation of atrazine in water was performed using homemade (PA and PB) and purchased (PC) boron-doped diamond anodes. The degradation was monitored off-line by analyzing total organic carbon and high performance liquid chromatography with diode array detector (HPLC-DAD) and at-line by UV spectroscopy. The spectra were recorded every 2 min. The rank deficiency problem was resolved by assembling an augmented column-wise matrix. HPLC was employed to separate the original and byproducts degradation components. Aiming the same goal, multivariate curve resolution - alternating least squares (MCR-ALS) was applied to resolve the UV spectroscopic data. Comparison between HPLC and MCR-ALS separations is presented. By using MCR-ALS the spectra of atrazine and two byproducts were successfully resolved and the resulted concentration profiles properly represented the system studied. The ALS explained variance (R2) for PA, PB and PC was equal to 99.99% for all of them and the lack of fit for PA, PB and PC were 0.39, 0.34 and 0.54 respectively. The correlation (R) between the recovered and pure spectra were calculate for each electrodegradation, validating the MCR-ALS results. The average R was equal to 0.997. The spectral and concentration profiles described with this new approach are in agreement with HPLC-DAD results. The proposed method is an alternative to classical analyses for monitoring of the degradation process, mainly due to the simplicity, fast results and economy.

Tasajännitetason nosto polttokennosovelluksessa

Polttokennojen, erityisesti SOFC-kennojen, tutkimuksessa on viime vuosina saavutettu merkittäviä edistysaskelia ja mahdollisuudet kennojen laajamittaiseen hyödyntämiseen paranevat koko ajan. Polttokennojen yleistyessä tarvitaan tehoelektroniikkaa muokkaamaan kennojen tasajännite verkkoon sopivaksi vaihtojännitteeksi. Verkkovaihtosuuntaaja vaatii korkeamman jännitetason, kuin polttokennosta on saatavissa, joten tasajännitetasoa on ensin nostettava. Tässä diplomityössä esitellään kolme eri hakkuritopologiaa ja perehdytään kokosiltahakkurin optimointiin. Hakkurin pääasialliset häviölähteet olivat toision diodisilta ja transistorit. Diodien vaihtaminen piidiodeista piikarbididiodeihin ei parantanut hyötysuhdetta, koska toision jännite tarkastellussa sovelluksessa oli matala. Muuntajan käämiminen litz-johtimella paransi hyötysuhdetta merkittävästi.

Ledivalaisimet rautatiealueiden valaistuksessa

Leditekniikan kehitys viime vuosina on mahdollistanut niiden käytön yleisvalaistuksessa. Tässä työssä tehdään katsaus leditekniikan nykytilaan ja tulevaisuuteen, sekä osoitetaan, että ledivalaisimien energiankulutuksessa ja huoltokustannuksissa tehdyillä säästöillä voidaan kattaa suuremmat hankintakustannukset ja päästä yhtä suuriin tai pienempiin elinkaarikustannuksiin verrattuna perinteisiin kaasupurkausvalaisimiin. Valaisimien määrät on laskettu Dialux-valaistuslaskentaohjelmalla siten että rautatieasemien avolaitureiden ja katettujen laitureiden valaistusvaatimukset täyttyvät. Tuloksia voi soveltaa muihin vastaaviin tiloihin kuten asematunneleihin tai kevyen liikenteen väylille.

Tasasähkönjakeluverkon vaihtosuuntaaja galvaanisella erotuksella

Suomessa sähkönjakeluverkko koostuu pääasiassa 20 kV ja 400 V jännitetasoista. Tällöin sähkö viedään lähelle kuluttajia suuremmalla jännitetasolla ja muunnetaan alhaisemmaksi lähellä asiakkaita. Haittapuolena on se, että haja-asutusalueilla jakelumuuntajien määrä kasvaa suureksi, koska ne täytyy sijoittaa lähelle kuluttajaa. Vaihtoehtona on toteuttaa osa sähkönjakelusta tasajännitteellä, jolloin tehollinen jännite olisi suurempi. Tällöin sähköä voitaisiin siirtää pidempiä matkoja ilman, että asiakaskohtaisia tai muutaman asiakkaan kattavia 20 kV siirtolinjoja tarvitsisi käyttää. Tämä taasen edellyttää asiakaskohtaisien vaihtosuuntaajien käyttöä. Tässä työssä esiteltävällä 1 kVA vaihtosuuntaajalla muodostetaan tasasähköjakeluverkosta saatavasta 750 V tasasähköstä yksivaiheista (230 VRMS, 50 Hz) verkkojännitettä. Laite on suunniteltu toteuttamaan galvaaninen erotus mahdollisimman hyvän hyötysuhteen puitteissa. Vaihtosuuntaaja on toteutettu käyttämällä resonanssikonvertteria, joka vaihtosuuntaa jakelujännitteen korkeataajuiseksi vaihtojännitteeksi. Tämän jälkeen toteutetaan galvaaninen erotus käyttäen suurtaajuusmuuntajaa. Tätä seuraa syklokonvertteri, joka pulssintiheysmodulaatiota soveltaen muodostaa lähtöjännitteen. Tämä suodatetaan lopuksi LC- alipäästösuotimella säröltään standardin mukaiseksi. Laite on jaettu työssä kolmeen osaan, joista jokaisen toiminta on selitetty ja simuloitu itsenäisesti. Lopussa koko järjestelmä on simuloitu yhtenä kokonaisuutena. Hyötysuhteeksi arvioitiin karkeasti 94 % ja lopullisista tuloksista voidaan päätellä, että laitteen toteuttaminen prototyypiksi voisi olla kannattavaa.

Line filter optimization in elevator use

The purpose of this thesis was to create design a guideline for an LCL-filter. This thesis reviews briefly the relevant harmonics standards, old filter designs and problems faced with the previous filters. This thesis proposes a modified design method based on the “Liserre’s method” presented in the literature. This modified method will take into account network parameters better. As input parameters, the method uses the nominal power, allowed ripple current in converter and network side and desired resonant frequency of the filter. Essential component selection issues for LCL-filter, such as heating, voltage strength, current rating etc. are also discussed. Furthermore, a simulation model used to verify the operation of the designed filter in nominal power use and in transient situations is included in this thesis.

Centralized Motion Control of a Linear Tooth Belt Drive: Analysis of the Performance and Limitations

A centralized robust position control for an electrical driven tooth belt drive is designed in this doctoral thesis. Both a cascaded control structure and a PID based position controller are discussed. The performance and the limitations of the system are analyzed and design principles for the mechanical structure and the control design are given. These design principles are also suitable for most of the motion control applications, where mechanical resonance frequencies and control loop delays are present. One of the major challenges in the design of a controller for machinery applications is that the values of the parameters in the system model (parameter uncertainty) or the system model it self (non-parametric uncertainty) are seldom known accurately in advance. In this thesis a systematic analysis of the parameter uncertainty of the linear tooth beltdrive model is presented and the effect of the variation of a single parameter on the performance of the total system is shown. The total variation of the model parameters is taken into account in the control design phase using a Quantitative Feedback Theory (QFT). The thesis also introduces a new method to analyze reference feedforward controllers applying the QFT. The performance of the designed controllers is verified by experimentalmeasurements. The measurements confirm the control design principles that are given in this thesis.

Mössbauer spectra of iron oxides in the bulk and nanocrystalline states

Magnetic nanoparticles are very important in modern industry. These particles are used in many different spheres of life. Nanoparticles have unusual physical and chemical properties connected both with quantum dimensional effects and with the increased role of the surface atoms. Most clearly the difference between the properties of bulk materials and nanoparticles can be seen in the magnetic properties of these materials. The most typical magnetic properties of nanomaterials are superparamagnetism with the size of the cluster from 1 to 10 nm; single-domain magnetic state of nanoclusters and nanostructures up to 20 nm; magnetization processes connected with magnetic cluster ordering and with its forms and sizes; quantum magnetic tunneling effects when magnetization changes by jumps and giant magnetoresistance effects. For research of the magnetic properties of iron-containing nanostructures, it is convenient to apply Mӧssbauer spectroscopy. In this work a number of nano-sized samples of iron oxides were examined by Mössbauer spectroscopy. The Mössbauer spectra of nanoparticles with various sizes were obtained. Mössbauer spectra of iron oxide nanoparticles were compared with the spectra of bulk samples. It was shown how the spectra of iron oxide nanoparticles change depending on the particle sizes.