Simultaneous determination of tramadol and lidocaine in urine by end-column capillary electrophoresis with electrochemiluminescence detection

Tramadol and lidocaine, used as analgesic and local anesthetic in surgery, are partly excreted by kidney. For the first time, we developed a simple and sensitive method, based on capillary electrophoresis with electrochemiluminescence (ECL) detection by end column mode without joint to monitor tramadol and lidocaine in urine. To eliminate the influence of ionic strength of urine sample, analytes were extracted by ether. Tripropylamine (TPA) was used as internal standard. ne recoveries of tramadol and lidocaine were between 94% and 97% at different levels. The method exhibited the linear range for the tramadol and lidocaine from 1.0 X 10(-7) to 1.0 X 10(-4) mol/L with correlation efficient of 0.998. The relative standard deviation (RSD) was 2.9% and 2.7% (n = 8) for tramadol and lidocaine, respectively. The limit of detection (LOD) was 6.0 x 10(-8) mol/L and 4.5 x 10(-8), mol/L (S/N = 3) for tramadol and lidocaine, respectively. The application for detecting tramadol and lidocaine in urine of patients showed that the method was valuable in clinical and biochemical laboratories for detecting tramadol, lidocaine and other tertiary amine pharmaceuticals for various purpose, such as metabolism investigation.

Simultaneous spectrophotometric determination of trace iron (III) and aluminum (III) with hybrid linear analysis

Hybrid linear analysis (HLA) was applied to resolution of overlapping spectra of Fe3+-salicylfluorone and Al3+-salicylfluorone complexes and simultaneous spectrophotometric determination of Fe3+ and Al3+. The absorbance matrix of 7 standard mixtures at 41 measuring points ranged from the wavelength of 550 nm to 630 nm was used for calibration. To avoid the effect of interaction between the two components on the determination, the column vector of K matrix obtained from the standard mixtures with least squares was used as the pure spectrum of component. The recoveries of the two elements for the analysis of the synthetic samples were 93.3% similar to 107.5% in the range of the concentration ratio of Fe3+:Al3+ = 10:1 to 1:8. Comparing with the partial least squares (PIS) model, the HLA method was simple, accuracy and precise.

Voltammetric behavior of tetracine on glassy garbon electrode and its application

The anodic voltammetric behavior of anaesthetic tetracine and its application were studied. In 0.1 mol/L HClO4 solution, the potential of anodic peak for tetracine is 1.04 V(vs. Ag/AgCl) at a glassy carbon electrode. A linear relationship between the peak height and the concentration of tetracine in the range of 5 x 10(-4) similar to 1 x 10(-1) g/L was obtained. The peak current decreases with the decreasing acidity of the solution. the mehtod has been used for the direct determination of tetracine in injections. The average recoveries of tetracine in urine samples were 98.5%. The mechanism of the electrode reaction was also discussed.

Separation and determination of organogermanium compounds by ion chromatography

For nearly three decades, organogermanium compounds have become increasingly of interest owing to their extensive physiological and pharmaceutical activity. In this paper, two new high performance ion chromatographic methods for separation and determination of three kinds of organogermanium compounds beta-carboxyethylgermanium sesquioxide (I), beta-(alpha-methyl)-carboxyethylgermanium sesquioxide (II) and d-(beta-carboxyethyl)germanium hydroxide (III) were proposed. A Dionex DX-300 ion chromatograph equipped with a Dionex FED-II pulsed electrochemical detector (conductivity mode), and a Dionex AI-450 chromatography workstation was employed. The separation was achieved by using ion-exchange or ion-exclusion mechanism. The detection limits(S/N=3, expressed as germanium) for the three compounds were all below sub- mu g/mL level. The methods have been applied to the analysis of tonic oral drinks, and the average recoveries for the three compounds range from 95 - 108%. The results obtained were in agreement with those of hydride generation atomic fluorescence spectrometry (HG-AFS).

SIMULTANEOUS DETERMINATION OF GUANINE, URIC-ACID, HYPOXANTHINE AND XANTHINE IN HUMAN PLASMA BY REVERSED-PHASE HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY WITH AMPEROMETRIC DETECTION

A reversed-phase high-performance liquid chromatographic method with amperometric detection is described for the separation and quantification of uric acid, guanine, hypoxanthine and xanthine. The isocratic separation of a standard mixture of the compounds was achieved in 5 min on a Spherisorb 5 C-18 reversed-phase column, with a mobile phase of NaH2PO4 (300 mmol dm(-3) pH 3.0)-methanol-acetonitrile-tetrahydrofuran (97.8 + 0.5 + 1.5 + 0.2). Uric acid, guanine, hypoxanthine and xanthine were completely separated, with detection limits in the range 2-20 pmol per injection. The effect of pH and the composition of the mobile phase on the separation are described. The hydrodynamic voltammograms of these compounds were recorded at a glassy carbon electrode. The linear range of the calibration graph for each compound was: uric acid; 1-5000 mu mol dm(-3); guanine, 0.5-2000 mu mol dm(-3); hypoxanthine, 0.1-500 mu mol dm(-3) and xanthine, 0.5-5000 mu mol dm(-3). The within- and between-day precision was good. The uric acid and hypoxanthine content in human plasma was measured using the proposed method. Good recoveries of uric acid (97.9-103%), hypoxanthine (98.0-99.2%), guanine (96.0-98.3%) and xanthine (96.0-102%) were obtained from human plasma. The results of electrochemical detection were in good agreement with those of UV detection.

Comparison of effectiveness of different ashing auxiliaries for determination of phosphorus in natural waters, aquatic organisms and sediments by ignition method

An improved method for the determination of phosphorus in natural waters, aquatic organisms and sediments by ignition method is proposed. The recoveries of phosphorus (P) from selected inorganic and organic P-containing compound standards after ignition with different auxiliaries, such as MgSO4, Mg(NO3)(2), MgO2, Mg(Ac-2) and CaCl2, were compared. We found that the phosphorus from most compound standards could not be completely recovered when these compounds were ignited (450-500degreesC) with the MgSO4 as auxiliary and the baked residue was extracted with 0.2 mol l(-1) HCl for 30min at 80degreesC or at room temperature. P recoveries, for example, were poor, less than 85%, if pyrophosphate and metaphosphate were ignited with the addition Of MgSO4 prior to the extraction of the baked residue with 0.2 mol l(-1) HCl at 80degreesC for 30 min. In contrast, MgO2, Mg(Ac)(2) and CaCl2, as well as Mg(NO3)(2), could all yield complete P recoveries at routine ashing temperatures (450-500degreesC). The results demonstrate that MgC12 is a more effective auxiliary agent for the determination of phosphorus in natural waters, aquatic organisms and sediments by ignition method than MgSO4 which is commonly used. (C) 2003 Elsevier Science Ltd. All rights reserved.

Extraction of phosphorus in natural waters and sediments by ignition method

Phosphorus recoveries from selected inorganic and organic P-containing compounds after ignition with auxiliaries, such as MgSO4, Mg (NO3)(2), MgCl2, Mg (Ac)(2) and CaCl2 were studied. It was found that the phosphorus could not be completely recovered when most P-containing compounds were ignited with MgSO4 at temperature not higher than 500degreesC if the baked residue was extracted with 0.2 mol/L HCl for 30 min at 80degreesC or at room temperature. In contrast, MgCl2, Mg(Ac)(2) and CaCl2, as well as Mg(NO3)(2), could all yield complete P recoveries. We suggest that MgCl2 rather than MgSO4, which is usually used, should be utilized as ashing auxiliary agent in the P extraction by ignition method. Although Mg (NO3)(2) is a highly effective auxiliary agent, yet interference from MgSO4, danger of explosion, toxicity of nitrogen dioxide and more manipulation steps may limit its widespread utilization. It is suggested that if sediment is ignited with MgCl2, the extraction of residue with 0.2 mol/L HCl for 30 min at 80degreesC could give good result.

Determination of aliphatic amines from soil and wastewater of a paper mill by pre-column derivatization using HPLC and tandem mass spectrometry (HPLC-MS/MS)

A pre-column derivatization method for the sensitive determination of aliphatic amines using the labeling reagent 1,2-benzo-3,4-dihydrocarbazole-9-ethyl chloroformate (BCEOC) followed by HPLC with fluorescence detection and APCI/NIS identification in positive-ion mode has been developed. The chromophore of 2-(9-carbazole)-ethyl chloroformate (CEOC) reagent was replaced by the 1,2-benzo-3,4-dihydrocarbazole functional group, which resulted in a sensitive fluorescence derivatizing reagent, BCEOC, that could easily and quickly label amines. Derivatives were stable enough to be efficiently analyzed by HPLC and showed an intense protonated molecular ion corresponding m/z [M + H](+) with APCI/MS in positive-ion mode. The collision induced dissociation of the protonated molecular ion formed characteristic fragment ions at m/z 264.1, m/z 246.0 and m/z 218.1, corresponding to the cleavages of CH2CH2O-CO, CH2CH2-OCO, and N-CH2CH2O bonds. Studies on derivatization conditions demonstrated that excellent derivatization yields close to 100% were observed with a 3 to 4-fold molar reagent excess in acetonitrile solvent, in the presence of borate buffer (pH 9.0) at 40 degrees C for 10 min. In addition, the detection responses for BCEOC derivatives were compared with those obtained with CEOC and FMOC as labeling reagents. The ratios I-BCEOC/I-CEOC and I-BCEOC/I-FMOC were, respectively, 1.40-2.76 and 1.36-2.92 for fluorescence responses (here, I was the relative fluorescence intensity). Separation of the amine derivatives had been optimized on an Eclipse XDB-C-8 column. Detection limits calculated from an 0.10 pmol injection, at a signal-to-noise ratio of 3, were 18.65-38.82 fmol (injection volume 10 mu L for fluorescence detection. The relative standard deviations for intraday determination (n = 6) of standard amine derivatives (50 pmol) were 0.0063-0.037% for retention times and 3.36-6.93% for peak areas. The mean intra-and inter-assay precision for all amines were <5.4% and 5.8%, respectively. The recoveries of amines ranged from 96 to 113%. Excellent linear responses were observed with correlation coefficients of >0.9994. The established method provided a simple and highly sensitive technique for the quantitative analysis of trace amounts of aliphatic amines from biological and natural environmental samples.

Determination of amines using 2-(11H-benzo[a]carbazol-11-yl) ethyl chloroformate (BCEC-Cl) as labeling reagent by HPLC with fluorescence detection and identification with APCI/MS

A pre-column derivatization method for the sensitive determination of amines using a labeling reagent 2-(11H-benzo[a]-carbazol-11-yl) ethyl chloroformate (BCEC-Cl) followed by high-performance, liquid chromatography with fluorescence detection has been developed. Identification of derivatives was carried out by LC/APCI/MS in positive-ion mode. The chromophore of 1,2-benzo-3,4-dihydrocarbazole-9-ethyl chloroformate (BCEOC-Cl) reagent was replaced by 2-(11H-benzo[a]-carbazol-11-yl) ethyl functional group, which resulted in a sensitive fluorescence derivatizing reagent BCEC-Cl. BCEC-Cl could easily and quickly label amines. Derivatives were stable enough to be efficiently analyzed by HPLC and showed an intense protonated molecular ion corresponding m/z [M+ H](+) under APCI/MS in positive-ion mode. The collision-induced dissociation of the protonated molecular ion formed characteristic fragment ions at m/z 261.8 and m/z 243.8 corresponding to the cleavages of CH2O-CO and CH2-OCO bonds. Studies on derivatization demonstrated excellent derivative yields over the pH 9.0-10.0. Maximal yields close to 100% were observed with three- to four-fold molar reagent excess. In addition, the detection responses for BCEC-derivatives were compared to those obtained using 1,2-benzo-3,4-dihydrocarbazole-9-ethyl chloroformate (BCEOC-Cl) and 9-fluorenyl methylchloroformate, (FMOC-Cl) as labeling reagents. The ratios I-BCEC/I-BCEOC = 1.94-2.17 and I-BCEC/I-FMOC = 1.04-2.19 for fluorescent (FL) responses (here, I was relative fluorescence intensity). Separation of the derivatized amines had been optimized on reversed-phase Eclipse XDB-C-8 column. Detection limits calculated from 0.50 pmol injection, at a signal-to-noise ratio of 3, were 1.77-14.4 fmol. The relative standard deviations for within-day determination (n = 11) were 1.84-2.89% for the tested amines. The mean intra- and inter-assay precision for all amines levels were < 3.64% and 2.52%, respectively. The mean recoveries ranged from 96.6% to 107.1% with their standard deviations in the range of 0.8-2.7. Excellent linear responses were observed with coefficients of > 0.9996. (C) 2006 Elsevier B.V. All rights reserved.

Pretty good governance: balancing policy drivers and stakeholder interests in developing fisheries ecosystem plans

The central research question that this thesis addresses is whether there is a significant gap between fishery stakeholder values and the principles and policy goals implicit in an Ecosystem Approach to Fisheries Management (EAFM). The implications of such a gap for fisheries governance are explored. Furthermore an assessment is made of what may be practically achievable in the implementation of an EAFM in fisheries in general and in a case study fishery in particular. The research was mainly focused on a particular case study, the Celtic Sea Herring fishery and its management committee, the Celtic Sea Herring Management Advisory Committee (CSHMAC). The Celtic Sea Herring fishery exhibits many aspects of an EAFM and the fish stock has successfully recovered to healthy levels in the past 5 years. However there are increasing levels of governance related conflict within the fishery which threaten the future sustainability of the stock. Previous research on EAFM governance has tended to focus either on higher levels of EAFM governance or on individual behaviour but very little research has attempted to link the two spheres or explore the relationship between them. Two main themes within this study aimed to address this gap. The first was what role governance could play in facilitating EAFM implementation. The second theme concerned the degree of convergence between high-level EAFM goals and stakeholder values. The first method applied was governance benchmarking to analyse systemic risks to EAFM implementation. This found that there are no real EU or national level policies which provide stakeholders or managers with clear targets for EAFM implementation. The second method applied was the use of cognitive mapping to explore stakeholders understandings of the main ecological, economic and institutional driving forces in the Celtic Sea Herring fishery. The main finding from this was that a long-term outlook can and has been incentivised through a combination of policy drivers and participatory management. However the fundamental principle of EAFM, accounting for ecosystem linkages rather than target stocks was not reflected in stakeholders cognitive maps. This was confirmed in a prioritisation of stakeholders management priorities using Analytic Hierarchy Process which found that the overriding concern is for protection of target stock status but that wider ecosystem health was not a priority for most management participants. The conclusion reached is that moving to sustainable fisheries may be a more complex process than envisioned in much of the literature and may consist of two phases. The first phase is a transition to a long-term but still target stock focused approach. This achievable transition is mainly a strategic change, which can be incentivised by policies and supported by stakeholders. In the Celtic Sea Herring fishery, and an increasing number of global and European fisheries, such transitions have contributed to successful stock recoveries. The second phase however, implementation of an ecosystem approach, may present a greater challenge in terms of governability, as this research highlights some fundamental conflicts between stakeholder perceptions and values and those inherent in an EAFM. This phase may involve the setting aside of fish for non-valued ecosystem elements and will require either a pronounced mind-set and value change or some strong top-down policy incentives in order to succeed. Fisheries governance frameworks will need to carefully explore the most effective balance between such endogenous and exogenous solutions. This finding of low prioritisation of wider ecosystem elements has implications for rights based management within an ecosystem approach, regardless of whether those rights are individual or collective.

Overexpression of the cardiac beta(2)-adrenergic receptor and expression of a beta-adrenergic receptor kinase-1 (betaARK1) inhibitor both increase myocardial contractility but have differential effects on susceptibility to ischemic injury.

Cardiac beta(2)-adrenergic receptor (beta(2)AR) overexpression is a potential contractile therapy for heart failure. Cardiac contractility was elevated in mice overexpressing beta(2)ARs (TG4s) with no adverse effects under normal conditions. To assess the consequences of beta(2)AR overexpression during ischemia, perfused hearts from TG4 and wild-type mice were subjected to 20-minute ischemia and 40-minute reperfusion. During ischemia, ATP and pH fell lower in TG4 hearts than wild type. Ischemic injury was greater in TG4 hearts, as indicated by lower postischemic recoveries of contractile function, ATP, and phosphocreatine. Because beta(2)ARs, unlike beta(1)ARs, couple to G(i) as well as G(s), we pretreated mice with the G(i) inhibitor pertussis toxin (PTX). PTX treatment increased basal contractility in TG4 hearts and abolished the contractile resistance to isoproterenol. During ischemia, ATP fell lower in TG4+PTX than in TG4 hearts. Recoveries of contractile function and ATP were lower in TG4+PTX than in TG4 hearts. We also studied mice that overexpressed either betaARK1 (TGbetaARK1) or a betaARK1 inhibitor (TGbetaARKct). Recoveries of function, ATP, and phosphocreatine were higher in TGbetaARK1 hearts than in wild-type hearts. Despite basal contractility being elevated in TGbetaARKct hearts to the same level as that of TG4s, ischemic injury was not increased. In summary, beta(2)AR overexpression increased ischemic injury, whereas betaARK1 overexpression was protective. Ischemic injury in the beta(2)AR overexpressors was exacerbated by PTX treatment, implying that it was G(s) not G(i) activity that enhanced injury. Unlike beta(2)AR overexpression, basal contractility was increased by betaARK1 inhibitor expression without increasing ischemic injury, thus implicating a safer potential therapy for heart failure.

Un modelo de optimización del uso del suelo y del agua con fines agrícolas en el partido de Tandil

p.247-252

Production of lightweight aggregate from industrial waste and carbon dioxide

The concomitant recycling of waste and carbon dioxide emissions is the subject of developing technology designed to close the industrial process loop and facilitate the bulk-re-use of waste in, for example, construction. The present work discusses a treatment step that employs accelerated carbonation to convert gaseous carbon dioxide into solid calcium carbonate through a reaction with industrial thermal residues. Treatment by accelerated carbonation enabled a synthetic aggregate to be made from thermal residues and waste quarry fines. The aggregates produced had a bulk density below 1000 kg/m3 and a high water absorption capacity. Aggregate crushing strengths were between 30% and 90% stronger than the proprietary lightweight expanded clay aggregate available in the UK. Cast concrete blocks containing the carbonated aggregate achieve compressive strengths of 24 MPa, making them suitable for use with concrete exposed to non-aggressive service environments. The energy intensive firing and sintering processes traditionally required to produce lightweight aggregates can now be augmented by a cold-bonding, low energy method that contributes to the reduction of green house gases to the atmosphere.

The Afroporteña press and Afro-Argentine’s thought in the late nineteenth century

The journalistic boom that occurred in Argentina from the second half of the nineteenth century saw the emergence of an active afroporteña press that defend the interests of the black community. This paper, in addition to reviewing the history of the Afro-Argentines newspapers, emphasizes the role played by the elite of African descent in the promotion of modernity among his brothers, while exploring the possible bases for an identity in the ideas spread.

Reality Shows in Chile, origin and road map. Historical-Communication Dialogues

Reality shows are TV programs which represent a format used in television nowadays; however, the observation practices of individual and/or group intimacy dates from thousands years ago. Sometimes this was driven by voyeurism or morbid fascination, some others, by the purpose of guarding, supervising and maintaining status quo. This work offers an alternative answer to the explanation of this type of TV program emergence and relates this appearance to a government procedure bound up with modern State terrorism which began at the end of the eighteenth century and has been recalled by different regimes until present days.