956 resultados para Multicatalytic tandem


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The purpose of this study was to develop a rapid, simple and sensitive quantitation method for pseudoephedrine (PSE), paracetamol (PAR) and loratadine (LOR) in plasma and pharmaceuticals using liquid chromatography-tandem mass spectrometry with a monolithic column. Separation was achieved using a gradient composition of methanol-0.1% formic acid at a flow rate of 1.0 mL min-1. Mass spectral transitions were recorded in SRM mode. System validation was evaluated for precision, specificity and linearity. Limit of detection for pseudoephedrine, paracetamol, and loratadine were determined to be 3.14, 1.86 and 1.44 ng mL-1, respectively, allowing easy determination in plasma with % recovery of 93.12 to 101.56%.

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A sensitive, accurate and simple method using HPLC-MS/MS was developed and validated for levodopa quantitation in human plasma. Analysis was achieved on a pursuit® C18 analytical column (5 µm; 150 x 4.6 mm i.d.) using a mobile phase (methanol and water , 90:10, v/v) containing formic acid 0.5% v/v, after extracting the samples using a simple protein plasma precipitation with perchloric acid. The developed method was validated in accordance with ANVISA guidelines and was successfully applied to a bioequivalence study in 60 healthy volunteers demonstrating the feasibility and reliability of the proposed method.

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Kirjallisuusarvostelu

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Kirjallisuusarvostelu

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Tässä kanditaatintyössä vertaillaan jauhekaari- ja tandem-MIG/MAG-hitsausta kirjallisuustutkimuksena. Vertailun kohteena ovat hitsausprosessien tuottavuus ja kustannukset sekä hitsausprosesseilla saavutettava laatu. Lisäksi kandidaatintyössä esitetään hitsausprosesseille tyypilliset käyttökohteet CASE -esimerkkeinä.

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Tämä kandidaatintyö on tutkimus hitsauslankojen kallistuskulmien vaikutuksesta hitsausliitoksen ominaisuuksiin tandem-MAG-pienahitsauksessa S355-rakenneteräkselle. Kokeellinen osuus suoritettiin Lappeenrannan teknillisen yliopiston hitsaustekniikan laboratoriossa jatkotutkimuksena Binbin Yanin diplomityölle ”Influence of wire configurations of welding S355 structural steel with tandem GMAW”. Tutkimuksen tavoitteena on määrittää tandem-MAG-hitsauksessa käytettyjen hitsauslankojen kallistuskulmien vaikutus hitsausliitoksen ominaisuuksiin. Teoriaosuuden tavoitteena on selvittää myös muiden hitsausparametrien vaikutus hitsausliitoksen ominaisuuksiin sekä perehtyä hitsisulan käyttäytymiseen terästen tandem-MAG-hitsauksessa.

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Free and total carnitine quantification is important as a complementary test for the diagnosis of unusual metabolic diseases, including fatty acid degradation disorders. The present study reports a new method for the quantification of free and total carnitine in dried plasma specimens by isotope dilution electrospray tandem mass spectrometry with sample derivatization. Carnitine is determined by looking for the precursor of ions of m/z = 103 of N-butylester derivative, and the method is validated by comparison with radioenzymatic assay. We obtained an inter- and intra-day assay coefficient of variation of 4.3 and 2.3, respectively. Free and total carnitine was analyzed in 309 dried plasma spot samples from children ranging in age from newborn to 14 years using the new method, which was found to be suitable for calculating reference age-related values for free and total carnitine (less than one month: 19.3 ± 2.4 and 23.5 ± 2.9; one to twelve months: 28.8 ± 10.2 and 35.9 ± 11.4; one to seven years: 30.7 ± 10.3 and 38.1 ± 11.9; seven to 14 years: 33.7 ± 11.6, and 43.1 ± 13.8 µM, respectively). No difference was found between males and females. A significant difference was observed between neonates and the other age groups. We compare our data with reference values in the literature, most of them obtained by radioenzymatic assay. However, this method is laborious and time consuming. The electrospray tandem mass spectrometry method presented here is a reliable, rapid and automated procedure for carnitine quantitation.

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Tämän työn tavoitteena on etsiä pinnoitushitsaukseen soveltuvat pulssituksen arvot tandem-MAG-hitsauksella. Työssä suoritettiin 14 koehitsiä S355-rakenneteräkselle. Koekappaleisiin hitsattiin kolme hitsauspalkoa 5 millimetrin välein. Koekappaleista otettiin makrokuvat, joista vertailtiin kappaleiden sekoittumisasteita. Kokeiden tuloksina saatiin vaihteluväliksi 11,1 %.

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Tämän työn tavoitteena oli hitsata tandem MAG –laitteistolla 25 mm paksua Ruukin E500 TMCP terästä. Työssä oli tarkoituksena vähentää railotilavuutta mahdollisimman paljon sekä suorittaa testihitsaukset 0.8 kJ/mm sekä 2.5 kJ/mm lämmöntuonneilla. Teoriaosuudessa käsiteltiin Tandem MAG-hitsaukseen, sen tuottavuuteen ja laatukysymyksiin liittyviä asioita sekä siinä perehdyttiin suurlujuusteräksien käyttöön hitsauksessa sekä laivanrakennuksessa. Kokeellisessa osuudessa perehdyttiin hitsauksessa huomattuihin etuihin, ongelmiin sekä ongelmien ratkaisumahdollisuuksiin. Hitsausliitoksen mekaaniset ominaisuudet tutkittiin rikkomattomin sekä rikkovin menetelmin. Alustavat hitsausohjeet luotiin kummallekin lämmöntuonnille. Testaukset aloitettiin 30 º railokulmalla pienentäen kulmaa mahdollisuuksien mukaan. Testauksissa ei saatu hitsattua onnistuneesti alle 30 º railokulmalla. Hitsaustestien aikana huomattiin magneettisen puhalluksen vaikutus hitsaustapahtumaan. Kaasunvirtausnopeuden tuli olla tietyn suuruinen jotta palkokerrokset onnistuivat ilman huokoisuusongelmaa. Pienemmällä lämmöntuonnilla hitsattaessa kaasunvirtausnopeudet olivat tärkeämpiä hitsatessa ylempiä palkokerroksia. Kääntämällä hitsauspoltinta sivuttaissuunnassa 7-10 astetta auttoi ehkäisemään reunahaavan syntymistä. Rikkovista menetelmistä testitulokset olivat hyväksyttyjä kaikkien muiden paitsi päittäishitsin sivutaivutuskokeen osalta.

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Acylcarnitine profiling by electrospray ionization tandem mass spectrometry (ESI-MS/MS) is a potent tool for the diagnosis and screening of fatty acid oxidation and organic acid disorders. Few studies have analyzed free carnitine and acylcarnitines in dried blood spots (DBS) of umbilical cord blood (CB) and the postnatal changes in the concentrations of these analytes. We have investigated these metabolites in healthy exclusively breastfed neonates and examined possible effects of birth weight and gestational age. DBS of CB were collected from 162 adequate for gestational age neonates. Paired DBS of heel-prick blood were collected 4-8 days after birth from 106 of these neonates, the majority exclusively breastfed. Methanol extracts of DBS with deuterium-labeled internal standards were derivatized before analysis by ESI-MS/MS. Most of the analytes were measured using a full-scan method. The levels of the major long-chain acylcarnitines, palmitoylcarnitine, stearoylcarnitine, and oleoylcarnitine, increased by 27, 12, and 109%, respectively, in the first week of life. Free carnitine and acetylcarnitine had a modest increase: 8 and 11%, respectively. Propionylcarnitine presented a different behavior, decreasing 9% during the period. The correlations between birth weight or gestational age and the concentrations of the analytes in DBS were weak (r £ 0.20) or nonsignificant. Adaptation to breast milk as the sole source of nutrients can explain the increase of these metabolites along the early neonatal period. Acylcarnitine profiling in CB should have a role in the early detection of metabolic disorders in high-risk neonates.

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Although 17β-estradiol (E2) deficiency has been linked to the development of osteoarthritis (OA) in middle-aged women, there are few studies relating other estrogens and estrogen metabolites (EMs) to this condition. We developed a high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry (HPLC-ESI-MS/MS) method to measure the levels of six EMs (i.e., estrone, E2, estriol, 2-hydroxyestrone, 2-hydroxyestradiol, and 16a-hydroxyestrone) in healthy pre- and postmenopausal women and women with OA. This method had a precision ranging from 1.1 to 3.1% and a detection limit ranging from 10 to 15 pg. Compared to healthy women, serum-free E2 was lower in the luteal and postmenopausal phases in women with OA, and total serum E2 was lower in postmenopausal women with OA. Moreover, compared to healthy women, total serum 2-hydroxyestradiol was higher in postmenopausal women with OA and total serum 2-hydroxyestrone was lower in both the luteal and follicular phases in women with OA. In conclusion, our HPLC-ESI-MS/MS method allowed the measurement of multiple biochemical targets in a single assay, and, given its increased cost-effectiveness, simplicity, and speed relative to previous methods, this method is suitable for clinical studies.

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Sequence repeats are an important phenomenon in the human genome, playing important roles in genomic alteration often with phenotypic consequences. The two major types of repeat elements in the human genome are tandem repeats (TRs) including microsatellites, minisatellites, and satellites and transposable elements (TEs). So far, very little has been known about the relationship between these two types of repeats. In this study, we identified TRs that are derived from TEs either based on sequence similarity or overlapping genomic positions. We then analyzed the distribution of these TRs among TE families/subfamilies. Our study shows that at least 7,276 TRs or 23% of all minisatellites/satellites is derived from TEs, contributing ∼0.32% of the human genome. TRs seem to be generated more likely from younger/more active TEs, and once initiated they are expanded with time via local duplication of the repeat units. The currently postulated mechanisms for origin of TRs can explain only 6% of all TE-derived TRs, indicating the presence of one or more yet to be identified mechanisms for the initiation of such repeats. Our result suggests that TEs are contributing to genome expansion and alteration not only by transposition but also by generating tandem repeats.