Simple method for determination of cocaine and main metabolites in urine by CE coupled to MS

in this work, a simple method for the simultaneous determination of cocaine (COC) and five COC metabolites (benzoylecgonine, cocaethylene (CET), anhydroecgonine, anhydroecgonine methyl ester and ecgonine methyl ester) in human urine using CE coupled to MS via electrospray ionization (CE-ESI-MS) was developed and validated. Formic acid at 1 mol/L concentration was used as electrolyte whereas formic acid at 0.05 mol/L concentration in 1:1 methanol:water composed the coaxial sheath liquid at the ESI nozzle. The developed method presented good linearity in the dynamic range from 250 ng/mL to 5000 ng/mL (coefficient of determination greater than 0.98 for all compounds). LODs (signal-to-noise ratio of 3) were 100 ng/mL for COC and CET and 250 ng/mL for the other studied metabolites whereas LOQ`s (signal-to-noise ratio of 10) were 250 ng/mL for COC and CET and 500 ng/mL for all other compounds. Intra-day precision and recovery tests estimated at three different concentration levels (500, 1500 and 5000 ng/mL) provided RSD lower than 10% (except anhydroecgonine, 18% RSD) and recoveries from 83-109% for all analytes. The method was successfully applied to real cases. For the positive urine samples, the presence of COC and its` metabolites was further confirmed by MS/MS experiments.

New hydrazine sensors based on electropolymerized meso-tetra (4-sulphonatephenyl)porphyrinate manganese (III)/silver nanomaterial

A new electrocatalytic active porphyrin nanocomposite material was obtained by electropolymerization of meso-tetra(4-sulphonatephenyl) porphyrinate manganese(III) complex (MnTPPS) in alkaline solutions containing sub-micromolar concentrations of silver chloride. The modified glassy carbon electrodes efficiently oxidize hydrazine at 10 mV versus Ag/AgCl, dramatically decreasing the overpotential of conventional carbon electrodes. The analytical characteristics of this amperometric sensor coupled with batch injection analysis (BIA) technique were explored. Wide linear dynamic range (2.5 x 10(-7) to 2.5 x 10(-4) mol L-1), good repeatability (R.S.D. = 0.84%, n = 30) and low detection (3.1 x 10(-8) mol L-1) and quantification (1.0 x 10(-7) mol L-1) limits, as well as very fast sampling frequency (60 determinations per hour) were achieved. (c) 2007 Elsevier B.V. All rights reserved.

Biocompatible in-tube solid phase microextraction coupled with liquid chromatography-fluorescence detection for determination of interferon alpha in plasma samples

The present work demonstrates the successful application of automated biocompatible in-tube solid-phase microextraction coupled with liquid chromatography (in-tube SPME/LC) for determination of interferon alpha(2a) (IFN alpha(2a)) in plasma samples for therapeutic drug monitoring. A restricted access material (RAM, protein-coated silica) was employed for preparation of a lab-made biocompatible in-tube SPME capillary that enables the direct injection of biological fluids as well as the simultaneous exclusion of macromolecules by chemical diffusion barrier and drug pre-concentration. The in-tube SPME variables, such as sample volume, draw/eject volume, number of draw-eject cycles, and desorption mode were optimized, to improve the sensitivity of the proposed method. The IFN alpha(2a) analyses in plasma sample were carried out within 25 min (sample preparation and LC analyses). The response of the proposed method was linear over a dynamic range, from 0.06 to 3.0 MIU mL(-1), with correlation coefficient equal to 0.998. The interday precision of the method presented coefficient of variation lower than 8%. The proposed automated method has adequate analytical sensitivity and selectivity for determination of IFN alpha(2a) in plasma samples for therapeutic drug monitoring. (C) 2010 Elsevier B.V. All rights reserved.

THE POTENTIALITIES OF USING A GRAPHITE-SILICONE RUBBER COMPOSITE ELECTRODE IN THE DETERMINATION OF PROPRANOLOL

A graphite silicone-rubber composite electrode (GSR) was used for the determination of propranolol in drug formulation. Cyclic voltammetry (CV) at the GSR presented an irreversible oxidation peak at + 0.8V vs. SCE, in Britton Robinson (B-R) buffer pH 7.4. The quantitative determination was carried out using differential pulse voltammetry (DPV). Under optimized parameters a linear dynamic range from 5.0 to 80.6 mu mol L(-1) with a detection limit of 1.1 mu mol L(-1) was observed. A repeatability of 4.5 +/- 0.1 mu A (n = 10) peak current was found after 10 successive DPV voltammograms of propranolol in the same solution after surface renovations. Using the proposed electrode, propranolol was quantified in a pharmaceutical formulation with results that agreed within 95% confidence level (t-test) with those from an official method.

Infestação experimental em girinos de Rana catesbeiana Shaw por copepoditos de Lernaea cyprinacea Linnaeus (Copepoda, Lernaeidae)

The Lernaea cyprinacea Linnaeus, 1758 copepodids experimental contamination on the Rana catesbeiana Shaw, 1802 ladpoles was analized. Sixty percent (12) of infested tadpoles was found parasitized. High mortality range, lower appetence, equilibrium loss and apathy were observed. The parasites showed the preference for the mouth and cloaca: in 72 hours lhe egg saes had already developed.

Construção e validação de um receptor GPS para uso espacial

Global Positioning System, or simply GPS, it is a radionavigation system developed by United States for military applications, but it becames very useful for civilian using. In the last decades Brazil has developed sounding rockets and today many projects to build micro and nanosatellites has appeared. This kind of vehicles named spacecrafts or high dynamic vehicles, can use GPS for its autonome location and trajectories controls. Despite of a huge number of GPS receivers available for civilian applications, they cannot used in high dynamic vehicles due environmental issues (vibrations, temperatures, etc.) or imposed dynamic working limits. Only a few nations have the technology to build GPS receivers for spacecrafts or high dynamic vehicles is available and they imposes rules who difficult the access to this receivers. This project intends to build a GPS receiver, to install them in a payload of a sounding rocket and data collecting to verify its correct operation when at the flight conditions. The inner software to this receiver was available in source code and it was tested in a software development platform named GPS Architect. Many organizations cooperated to support this project: AEB, UFRN, IAE, INPE e CLBI. After many phases: defining working conditions, choice and searching electronic, the making of the printed boards, assembling and assembling tests; the receiver was installed in a VS30 sounding rocket launched at Centro de Lançamento da Barreira do Inferno in Natal/RN. Despite of the fact the locations data from the receiver were collected only the first 70 seconds of flight, this data confirms the correct operation of the receiver by the comparison between its positioning data and the the trajectory data from CLBI s tracking radar named ADOUR

A Novel Diagnostic Target in the Hepatitis C Virus Genome

BackgroundDetection and quantification of hepatitis C virus (HCV) RNA is integral to diagnostic and therapeutic regimens. All molecular assays target the viral 5'-noncoding region (59-NCR), and all show genotype-dependent variation of sensitivities and viral load results. Non-western HCV genotypes have been under-represented in evaluation studies. An alternative diagnostic target region within the HCV genome could facilitate a new generation of assays.Methods and FindingsIn this study we determined by de novo sequencing that the 3'-X-tail element, characterized significantly later than the rest of the genome, is highly conserved across genotypes. To prove its clinical utility as a molecular diagnostic target, a prototype qualitative and quantitative test was developed and evaluated multicentrically on a large and complete panel of 725 clinical plasma samples, covering HCV genotypes 1-6, from four continents (Germany, UK, Brazil, South Africa, Singapore). To our knowledge, this is the most diversified and comprehensive panel of clinical and genotype specimens used in HCV nucleic acid testing (NAT) validation to date. The lower limit of detection (LOD) was 18.4 IU/ml (95% confidence interval, 15.3-24.1 IU/ml), suggesting applicability in donor blood screening. The upper LOD exceeded 10(-9) IU/ml, facilitating viral load monitoring within a wide dynamic range. In 598 genotyped samples, quantified by Bayer VERSANT 3.0 branched DNA (bDNA), X-tail-based viral loads were highly concordant with bDNA for all genotypes. Correlation coefficients between bDNA and X-tail NAT, for genotypes 1-6, were: 0.92, 0.85, 0.95, 0.91, 0.95, and 0.96, respectively; X-tail-based viral loads deviated by more than 0.5 log10 from 5'-NCR-based viral loads in only 12% of samples (maximum deviation, 0.85 log10). The successful introduction of X-tail NAT in a Brazilian laboratory confirmed the practical stability and robustness of the X-tail-based protocol. The assay was implemented at low reaction costs (US$8.70 per sample), short turnover times (2.5 h for up to 96 samples), and without technical difficulties.ConclusionThis study indicates a way to fundamentally improve HCV viral load monitoring and infection screening. Our prototype assay can serve as a template for a new generation of viral load assays. Additionally, to our knowledge this study provides the first open protocol to permit industry-grade HCV detection and quantification in resource-limited settings.

Electroanalytical determination of carbendazim and fenamiphos in natural waters using a diamond electrode

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Potentiometric Sensor for Furosemide Determination in Pharmaceuticals, Urine, Blood Serum and Bovine Milk

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Potentiometric sensor for sorbic acid determination in food products

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Development of a potentiometric sensor for the determination of saccharin in instant tea powders, diet soft drinks and strawberry dietetic jam

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

A low-voltage wide-swing programmable-gain current amplifier

A CMOS low-voltage, wide-swing continuous-time current amplifier is presented. Exhibiting an open-loop architecture, the circuit is composed of transresistance and transconductance stages built upon triode-operating transistors. In addition to an extended dynamic range, the current gain can be programmed within good accuracy by a rapport involving only transistor geometries and tuning biases. Low temperature-drift on gain setting is then expected.In accordance with a 0.35 mum n-well CMOS fabrication process and a single 1.1 V-supply, a balanced current-amplifier is designed for a programmable gain-range of 6 - 34 dB and optimized with respect to dynamic range. Simulated results from PSPICE and Bsim3v3 models indicate, for a 100 muA(pp)-output current, a THD of 0.96 and 1.87% at 1 KHz and 100 KHz, respectively. Input noise is 120 pArootHz @ 10 Hz, with S/N = 63.2 dB @ 1%-THD. At maximum gain, total quiescent consumption is 334 muW. Measurements from a prototyped amplifier reveal a gain-interval of 4.8-33.1 dB and a maximum current swing of 120 muA(pp). The current-amplifier bandwidth is above 1 MHz.

A linearly tunable low-voltage CMOS transconductor with improved common-mode stability and its application to (gm)-C filters

A linearly tunable low-voltage CMOS transconductor featuring a new adaptative-bias mechanism that considerably improves the stability of the processed-signal common,mode voltage over the tuning range, critical for very-low voltage applications, is introduced. It embeds a feedback loop that holds input devices on triode region while boosting the output resistance. Analysis of the integrator frequency response gives an insight into the location of secondary poles and zeros as function of design parameters. A third-order low-pass Cauer filter employing the proposed transconductor was designed and integrated on a 0.8-mum n-well CMOS standard process. For a 1.8-V supply, filter characterization revealed f(p) = 0.93 MHz, f(s) = 1.82 MHz, A(min) = 44.08, dB, and A(max) = 0.64 dB at nominal tuning. Mined by a de voltage V-TUNE, the filter bandwidth was linearly adjusted at a rate of 11.48 kHz/mV over nearly one frequency decade. A maximum 13-mV deviation on the common-mode voltage at the filter output was measured over the interval 25 mV less than or equal to V-TUNE less than or equal to 200 mV. For V-out = 300 mV(pp) and V-TUNE = 100 mV, THD was -55.4 dB. Noise spectral density was 0.84 muV/Hz(1/2) @1 kHz and S/N = 41 dB @ V-out = 300 mV(pp) and 1-MHz bandwidth. Idle power consumption was 1.73 mW @V-TUNE = 100 mV. A tradeoff between dynamic range, bandwidth, power consumption, and chip area has then been achieved.

On designing OTA-C graphic-equalizers with MOSFET-triode transconductors

A CMOS audio-equalizer based on a parallel-array of 2nd-order bandpass-sections is presented and realized with triode transconductors. It has a programmable 12db-boost/cut on each of its three decade-bands, easily achieved through the linear dependence of gm on VDS. In accordance with a 0.8μm n-well double-metal fabrication process, a range of simulations supports theoretical analysis and circuit performance at different boost/cut scenarios. For VDD=3.3V, fullboosting stand-by prover consumption is 1.05mW. THD=-42.61dB@1Vpp and may be improved by balanced structures. Thermal- and I/f-noise spectral densities are 3.2μV/Hz12 and 18.2μV/Hz12@20Hz, respectively, for a dynamic range of 52.3dB@1Vpp. The equalizer effective area is 2.4mm2. The drawback of the existing transmission-zero due to the feedthrough-capacitance of a triode input-device is also addressed. The proposed topology can be extended to the design of more complex graphic-equalizers and hearing-aids.

A low-voltage programmable-gain CMOS amplifier with very-low temperature-drift

A new topology for a LVLP variable-gain CMOS amplifier is presented. Input- and load-stage are built around triode-transconductors so that voltage-gain is fully defined by a linear relationship involving only device-geometries and biases. Excellent gain-accuracy, temperature-insensitivity; and wide range of programmability, are thus achieved. Moreover, adaptative biasing improves the common-mode voltage stability upon gain-adjusting. As an example, a 0-40dB programmablegain audio-amplifier is designed. Its performance is supported by a range of simulations. For VDD=1.8V and 20dB-nominal gain, one has Av=19.97dB, f3db=770KHz and quiescent dissipation of 378μW. Over temperatures from -25°C to 125°C, the 0. ldB-bandwidth is 52KHz. Dynamic-range is optimized to 57.2dB and 42.6dB for gains of 20dB and 40dB, respectively. THD figures correspond to -60.6dB@Vout= 1Vpp and -79.7dB@Vout= 0.5 Vpp. A nearly constant bandwidth for different gains is also attained.