Audit report on America’s Agricultural Industrial Heritage Landscape, Inc., d/b/a Silos and Smokestacks National Heritage Area, in Waterloo, Iowa for the years ended December 31, 2008 and 2007

Audit report on America’s Agricultural Industrial Heritage Landscape, Inc., d/b/a Silos and Smokestacks National Heritage Area, in Waterloo, Iowa for the years ended December 31, 2008 and 2007

Quantitative monitoring of tamoxifen in human plasma extended to 40 metabolites using liquid-chromatography high-resolution mass spectrometry: new investigation capabilities for clinical pharmacology.

Liquid-chromatography (LC) high-resolution (HR) mass spectrometry (MS) analysis can record HR full scans, a technique of detection that shows comparable selectivity and sensitivity to ion transitions (SRM) performed with triple-quadrupole (TQ)-MS but that allows de facto determination of "all" ions including drug metabolites. This could be of potential utility in in vivo drug metabolism and pharmacovigilance studies in order to have a more comprehensive insight in drug biotransformation profile differences in patients. This simultaneous quantitative and qualitative (Quan/Qual) approach has been tested with 20 patients chronically treated with tamoxifen (TAM). The absolute quantification of TAM and three metabolites in plasma was realized using HR- and TQ-MS and compared. The same LC-HR-MS analysis allowed the identification and relative quantification of 37 additional TAM metabolites. A number of new metabolites were detected in patients' plasma including metabolites identified as didemethyl-trihydroxy-TAM-glucoside and didemethyl-tetrahydroxy-TAM-glucoside conjugates corresponding to TAM with six and seven biotransformation steps, respectively. Multivariate analysis allowed relevant patterns of metabolites and ratios to be associated with TAM administration and CYP2D6 genotype. Two hydroxylated metabolites, α-OH-TAM and 4'-OH-TAM, were newly identified as putative CYP2D6 substrates. The relative quantification was precise (<20 %), and the semiquantitative estimation suggests that metabolite levels are non-negligible. Metabolites could play an important role in drug toxicity, but their impact on drug-related side effects has been partially neglected due to the tremendous effort needed with previous MS technologies. Using present HR-MS, this situation should evolve with the straightforward determination of drug metabolites, enlarging the possibilities in studying inter- and intra-patients drug metabolism variability and related effects.

Captura incidental de la flota industrial entre Casma y Pucusana. 2000-2002

Se determina el nivel de la captura incidental (CI) en las operaciones de la pesca pelágica industrial. Los recursos costeros capturados por la flota industrial generalmente se encontraron distribuidos dentro de la franja costera de 10 mn. En este período, entre Casma y Pucusana la flota industrial capturó un total de 6.401 t de recursos costeros, constituidos principalmente de lorna (76,5%), pejerrey (9,2%) y pampanito pintado (9,1%). La incidencia de juveniles de lorna en el 2001 fue 70,8% y de pejerrey 84,8%. Por puertos, el mayor desembarque de CI comparado con captura total se registró en Supe (32,9%), Huacho (26,1%) y Chancay (23,9%). El 2001 fue el más representativo en desembarques, se registró un total de 126 E/P industriales operando dentro de las 5 mn de la costa en esta zona de estudio.

Simple and fast methods based on solid-phase extraction coupled to liquid chromatography with UV detection for the monitoring of caffeine in natural and waste waters as marker of anthropogenic impact

Two concentration methods for fast and routine determination of caffeine (using HPLC-UV detection) in surface, and wastewater are evaluated. Both methods are based on solid-phase extraction (SPE) concentration with octadecyl silica sorbents. A common “offline” SPE procedure shows that quantitative recovery of caffeine is obtained with 2 mL of an elution mixture solvent methanol-water containing at least 60% methanol. The method detection limit is 0.1 μg L−1 when percolating 1 L samples through the cartridge. The development of an “online” SPE method based on a mini-SPE column, containing 100 mg of the same sorbent, directly connected to the HPLC system allows the method detection limit to be decreased to 10 ng L−1 with a sample volume of 100 mL. The “offline” SPE method is applied to the analysis of caffeine in wastewater samples, whereas the “on-line” method is used for analysis in natural waters from streams receiving significant water intakes from local wastewater treatment plants

Adaptació a l’EEES de les assignatures experimentals troncals de la titulació d'Enginyeria Tècnica Industrial en Química Industrial de l'EUETIT

L'objectiu d'aquest projecte s'ha centrat en l'estructuració coordinada del programa del bloc d'assignatures experimentals troncals de la titulació d'Enginyeria Tècnica en Química Industrial, amb especial atenció a la introducció i implementació de forma progressiva de determinades competències transversals com: treball en grup, comunicació oral i escrita i gestió del treball i del temps. Aquestes competències es corresponen amb les definides en la proposta del perfil de formació de la titulació en Enginyeria Química de la EUETIT i aquesta experiència presenta una proposta per a la seva implementació a través de les quatre assignatures experimentals troncals de la titulació en Química Industrial.L'experiència ha suposat una millora de la coordinació i qualitat de les assignatures del bloc experimental ja que aquest procés d'adaptació ha motivat la programació coordinada de cadascuna d'aquestes assignatures en una línia més coherent amb el que hauria de ser la docència en el nou marc del EEES, potenciant els següents aspectes: i) la definició dels objectius formatius de l'assignatura, incloent els de caràcter transversal, ii) la definicióadequada i ajustada al temps assignat a cada assignatura del pla d'activitats presencials i no presencials del curs, iii) la planificació d'un protocol de recollida de dades sobre la marxa del curs, la satisfacció dels estudiants i el temps de dedicació dels estudiants a les tasques delprograma, iv) el seguiment de les assignatures mitjançant l'elaboració d'un informe periòdic d'anàlisi i millora de l'assignatura, iv) l'adequació del Campus Digital de l'assignatura per a la difusió d'informació i una comunicació eficaç amb els estudiants.

Utilização do resíduo industrial ferkal na produção de mudas de Mimosa caesalpiniaefolia, em estéril de extração de argila, inoculadas com fungos micorrízicos arbusculares e rizóbio

Realizou-se um experimento em casa de vegetação com o objetivo de avaliar os efeitos da inoculação com fungos micorrízicos arbusculares (FMAs) e, ou, rizóbio, associados à adição de resíduo da fabricação de ácido láctico (Ferkal), na produção de mudas de Mimosa caesalpiniaefolia (sabiá) em estéril de extração de argila. Foram utilizados vasos plásticos de 6 L que continham estéril de extração de argila, adicionado do resíduo Ferkal (nas concentrações de 0, 50, 100 e 200 g dm-3). Foram empregados seis tratamentos microbiológicos (FMAs nativos; FMA Glomus clarum; rizóbio; FMAs nativos + rizóbio; FMA G. clarum + rizóbio, e controle não inoculado). Após 103 dias, as mudas foram coletadas, e analisados o peso da matéria seca dos nódulos, a taxa de colonização micorrízica, o peso da matéria seca e os teores de N e P na parte aérea das mudas. Os resultados demonstraram que adição de Ferkal no tratamento-controle (sem inoculação) aumentou significativamente o teor de P. Entretanto, as melhores respostas foram obtidas nas mudas inoculadas com FMAs e, ou, rizóbio, que apresentaram, em relação ao controle, aumentos significativos no peso da matéria seca e nos teores de N e P da parte aérea das mudas, em quase todos os tratamentos inoculados. Os FMAs nativos foram mais eficientes que o FMA G. clarum em promover o crescimento de M. caesalpiniaefolia.

Quantification of glucuronidated and sulfated steroids in human urine by ultra-high pressure liquid chromatography quadrupole time-of-flight mass spectrometry.

The urinary steroid profile is constituted by anabolic androgenic steroids, including testosterone and its relatives, that are extensively metabolized into phase II sulfated or glucuronidated steroids. The use of liquid chromatography coupled to mass spectrometry (LC-MS) is an issue for the direct analysis of conjugated steroids, which can be used as urinary markers of exogenous steroid administration in doping analysis, without hydrolysis of the conjugated moiety. In this study, a sensitive and selective ultra high-pressure liquid chromatography coupled to quadrupole time-of-flight mass spectrometer (UHPLC-QTOF-MS) method was developed to quantify major urinary metabolites simultaneously after testosterone intake. The sample preparation of the urine (1 mL) was performed by solid-phase extraction on Oasis HLB sorbent using a 96-well plate format. The conjugated steroids were analyzed by UHPLC-QTOF-MS(E) with a single-gradient elution of 36 min (including re-equilibration time) in the negative electrospray ionization mode. MS(E) analysis involved parallel alternating acquisitions of both low- and high-collision energy functions. The method was validated and applied to samples collected from a clinical study performed with a group of healthy human volunteers who had taken testosterone, which were compared with samples from a placebo group. Quantitative results were also compared to GC-MS and LC-MS/MS measurements, and the correlations between data were found appropriate. The acquisition of full mass spectra over the entire mass range with QTOF mass analyzers gives promise of the opportunity to extend the steroid profile to a higher number of conjugated steroids.

Determination of plasma levels of citalopram and its demethylated and deaminated metabolites by gas chromatography and gas chromatography-mass spectrometry.

Sensitive and specific methods based on gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS) for the determination of levels of citalopram, desmethylcitalopram and didesmethylcitalopram in the plasma of patients treated with citalopram are presented, as well as a GC-MS procedure for the assay of the citalopram propionic acid derivative. After addition of a separate internal standard for each drug, liquid-solvent extraction is used to separate the basic compounds from the acid compounds. The demethylated amines are derivatized with trifluoroacetic anhydride, and the acid metabolite with methyl iodide. GC-MS is performed in the electron impact mode, as mass spectrometry by the (positive-ion) chemical ionization mode (methane and ammonia) appeared to be unsuitable. The limits of quantification were 1 ng/ml for citalopram and desmethylcitalopram and 2 ng/ml for the other metabolites. The correlation coefficients for the calibration curves (range 10-500 ng/ml) were &gt; or = 0.999 for all compounds, whether determined by GC or GC-MS.

Hydrogen sulfide measurement by headspace-gas chromatography-mass spectrometry (HS-GC-MS): application to gaseous samples and gas dissolved in muscle.

The aim of our study was to present a new headspace-gas chromatography-mass spectrometry (HS-GC-MS) method applicable to the routine determination of hydrogen sulfide (H(2)S) concentrations in biological and gaseous samples. The primary analytical drawback of the GC/MS methods for H(2)S measurement discussed in the literature was the absence of a specific H(2)S internal standard required to perform quantification. Although a deuterated hydrogen sulfide (D(2)S) standard is currently available, this standard is not often used because this standard is expensive and is only available in the gas phase. As an alternative approach, D(2)S can be generated in situ by reacting deuterated chloride with sodium sulfide; however, this technique can lead to low recovery yield and potential isotopic fractionation. Therefore, N(2)O was chosen for use as an internal standard. This method allows precise measurements of H(2)S concentrations in biological and gaseous samples. Therefore, a full validation using accuracy profile based on the β-expectation tolerance interval is presented. Finally, this method was applied to quantify H(2)S in an actual case of H(2)S fatal intoxication.

Audit report on America’s Agricultural Industrial Heritage Landscape, Inc., d/b/a Silos and Smokestacks National Heritage Area (Silos and Smokestacks), in Waterloo, Iowa for the years ended December 31, 2009 and 2008

Audit report on America’s Agricultural Industrial Heritage Landscape, Inc., d/b/a Silos and Smokestacks National Heritage Area (Silos and Smokestacks), in Waterloo, Iowa for the years ended December 31, 2009 and 2008

Multiplex liquid chromatography-tandem mass spectrometry assay for simultaneous therapeutic drug monitoring of ribavirin, boceprevir, and telaprevir.

New directly acting antivirals (DAAs) that inhibit hepatitis C virus (HCV) replication are increasingly used for the treatment of chronic hepatitis C. A marked pharmacokinetic variability and a high potential for drug-drug interactions between DAAs and numerous drug classes have been identified. In addition, ribavirin (RBV), commonly associated with hemolytic anemia, often requires dose adjustment, advocating for therapeutic drug monitoring (TDM) in patients under combined antiviral therapy. However, an assay for the simultaneous analysis of RBV and DAAs constitutes an analytical challenge because of the large differences in polarity among these drugs, ranging from hydrophilic (RBV) to highly lipophilic (telaprevir [TVR]). Moreover, TVR is characterized by erratic behavior on standard octadecyl-based reversed-phase column chromatography and must be separated from VRT-127394, its inactive C-21 epimer metabolite. We have developed a convenient assay employing simple plasma protein precipitation, followed by high-performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS) for the simultaneous determination of levels of RBV, boceprevir, and TVR, as well as its metabolite VRT-127394, in plasma. This new, simple, rapid, and robust HPLC-MS/MS assay offers an efficient method of real-time TDM aimed at maximizing efficacy while minimizing the toxicity of antiviral therapy.