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.

A new and improved strategy combining a dispersive-solid phase extraction-based multiclass method with ultra high pressure liquid chromatography for analysis of low molecular weight polyphenols in vegetables

This paper reports on the development and optimization of a modified Quick, Easy, Cheap Effective, Rugged and Safe (QuEChERS) based extraction technique coupled with a clean-up dispersive-solid phase extraction (dSPE) as a new, reliable and powerful strategy to enhance the extraction efficiency of free low molecular-weight polyphenols in selected species of dietary vegetables. The process involves two simple steps. First, the homogenized samples are extracted and partitioned using an organic solvent and salt solution. Then, the supernatant is further extracted and cleaned using a dSPE technique. Final clear extracts of vegetables were concentrated under vacuum to near dryness and taken up into initial mobile phase (0.1% formic acid and 20% methanol). The separation and quantification of free low molecular weight polyphenols from the vegetable extracts was achieved by ultrahigh pressure liquid chromatography (UHPLC) equipped with a phodiode array (PDA) detection system and a Trifunctional High Strength Silica capillary analytical column (HSS T3), specially designed for polar compounds. The performance of the method was assessed by studying the selectivity, linear dynamic range, the limit of detection (LOD) and limit of quantification (LOQ), precision, trueness, and matrix effects. The validation parameters of the method showed satisfactory figures of merit. Good linearity (View the MathML sourceRvalues2>0.954; (+)-catechin in carrot samples) was achieved at the studied concentration range. Reproducibility was better than 3%. Consistent recoveries of polyphenols ranging from 78.4 to 99.9% were observed when all target vegetable samples were spiked at two concentration levels, with relative standard deviations (RSDs, n = 5) lower than 2.9%. The LODs and the LOQs ranged from 0.005 μg mL−1 (trans-resveratrol, carrot) to 0.62 μg mL−1 (syringic acid, garlic) and from 0.016 μg mL−1 (trans-resveratrol, carrot) to 0.87 μg mL−1 ((+)-catechin, carrot) depending on the compound. The method was applied for studying the occurrence of free low molecular weight polyphenols in eight selected dietary vegetables (broccoli, tomato, carrot, garlic, onion, red pepper, green pepper and beetroot), providing a valuable and promising tool for food quality evaluation.

Morfologia em alta resolução espacial de estrelas de tipo Mira e R Corenae Borealis

Mira and R Coronae Borealis (R CrB) variable stars are evolved objects surrounded by circumstellar envelopes (CSE) composed of the ejected stellar material. We present a detailed high-spatial resolution morfological study of the CSE of three stars: IRC+10216, the closest and more studied Carbon-Rich Mira; o Ceti, the prototype of the Mira class; and RY Sagitarii (RY Sgr), the brightest R CrB variable of the south hemisphere. JHKL near-infrared adaptive optics images of IRC+10216 with high dynamic range and Vband images with high angular resolution and high depth, collected with the VLT/NACO and VLT/FORS1 instruments, were analyzed. NACO images of o Ceti were also analyzed. Interferometric observations of RY Sgr collected with the VLTI/MIDI instrument allowed us to explore its CSE innermost regions (»20 40 mas). The CSE of IRC+10216 exhibit, in near-infrared, clumps with more complex relative displacements than proposed in previous studies. In V-band, the majority of the non-concentric shells, located in the outer CSE layers, seem to be composed of thinner elongated shells. In a global view, the morphological connection between the shells and the bipolar core of the nebulae, located in the outer layers, together with the clumps, located in the innermost regions, has a difficult interpretation. In the CSE of o Ceti, preliminar results would be indicating the presence of possible clumps. In the innermost regions (.110 UA) of the CSE of RY Sgr, two clouds were detected in different epochs, embedded in a variable gaussian envelope. Based on a rigorous verification, the first cloud was located at »100 R¤ (or »30 AU) from the centre, toward the east-north-east direction (modulo 180o) and the second one was almost at a perpendicular direction, having aproximately 2£ the distance of the first cloud. This study introduces new constraints to the mass-loss history of these kind of variables and to the morphology of their innermost CSE regions

A multisampling time-domain CMOS imager with synchronous readout circuit

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

An algorithmic of analog-to-digital converter using current-mode and digital CMOS process

In this paper a new algorithmic of Analog-to-Digital Converter is presented. This new topology use the current-mode technique that allows a large dynamic range and can be implemented in digital CMOS process. The ADC proposed is very small and can handle high sampling rates. Simulation results using a 1.2um CMOS process show that an 8-b ADC can support a sampling rate of 50MHz.

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 tunable triode-MOSFET transconductor and its application to g(m)-C filters

A linear, tunable CMOS transconductance stage is introduced. Drain voltage of the input transistor operating in triode region is settled by a regulation loop and a first-order linear relationship between g(m) and a de bias voltage is achieved. In addition to easy tuning, this technique offers circuit simplicity, wide dynamic range, high input and output impedances and low consumption. The transconductor is presented on both single-ended and fully-differential versions. A 3rd-order elliptical low-pass g(m)-C filter with a nominal roll-off frequency of 2MHz is used as one example for the many applications of the proposed transconductor. SPICE data describe circuits performances and filter tunabilily Passband is tuned at a rate of 2.36KHz/mV and good linearity is indicated by a 0.89% THD for an 800mV(p-p) balanced-driven input.

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.

Damage Characterization Using Guided-Wave Linear Arrays and Image Compounding Techniques

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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.