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PubMed2006

Application of internal universal calibration for determination of fully dissociated species in capillary electrophoresis using indirect UV detection and electrokinetic injection.

Although the electrokinetic injection suffers from quantitation problems arising from mobility and matrix bias, the application of electrokinetic injection and indirect photometric detection may provide a very simple, sensitive and universal determination of fully dissociated components. In this work a survey of the possibilities of quantitative analysis using EK injection with indirect UV detection is given and a simple procedure (internal universal calibration) for accurate quantitative determination of traces using EK injection is proposed. It was shown that the thiosulfate as an internal universal standard (IUS) can be applied for quantitative determination of fully dissociated analytes (e.g. Br(-), Cl(-), NO(2)(-), NO(3)(-), SO(4)(2-), S(2)O(3)(2-)) whose mobilities (migration times) do not differ from the mobilities of monitoring ion (chromate), counter-ion (potassium) and IUS with more than 10%. The proposed calibration procedure provides concentration data, which deviate generally less than 5% extent from the actual true values. The validity and the applicability of the method was studied in the analysis of samples containing different amount of matrix material.

Anions↗
PubMed2004

A single spectroscopic flow-through sensing device for determination of ciprofloxacin.

A simple flow injection UV spectrophotometric sensing device was developed for the determination of ciprofloxacin. The method is based on its transient retention and concentration on Sephadex SP C-25 cation-exchange gel beads packed in the flow cell and the continuous monitoring of its native absorbance on the solid phase at 277 nm. The procedure is carried out without any derivatisation. Formic acid/NaOH 1.75 M at pH 2.2 is used as carrier solution in a simple monochannel FIA manifold. When the analytical signal reached the maximum value, ciprofloxacin was eluted from the solid support by the carrier solution itself. The response of the sensor was linear in the concentration range 0.5-10 microg ml(-1) with an RSD (%) of 0.79, a detection limit (3sigma criterion) of 0.035microg ml(-1) and a sampling rate of 16 h(-1). Application to the analysis of pharmaceutical samples testifies the utility of this sensor.

Ciprofloxacin↗
PubMed2004

Sequential injection spectrophotometric determination of etilefrine hydrochloride.

A simple, fast, economical and automated sequential injection spectrophotometric method for the determination of etilefrine hydrochloride is developed. The method is based on the condensation reaction of etilefrine hydrochloride with 4-aminoantipyrine in the presence of alkaline potassium hexacyanoferrate and the absorbance of the colored product measured at 503 nm. Aspiration order, flow rate, reaction coil diameter, reaction coil length, concentration of 4-aminoantipyrine and potassium ferricyanide, as well as aspiration volume of reagents and sample has been optimized. Using these optimized parameters, a linear relationship between the relative peak height and concentration was obtained in the range 1-20 mg l(-1). The detection limit (as 3sigma value) was 0.1 mg l(-1) and precision was 2.7% and 1.5% at 1 and 2 mg l(-1), respectively. This method is superior over previously reported ones in terms of linear range, short analysis time, high sample throughput, excellent reagent economy and minimum waste generation.

Etilefrine↗
PubMedDate not supplied

Miniaturized detectors for a chemical analysis system.

Recently, several studies about miniaturized chemical analysis systems fabricated with micromachining methods were reported. These systems have some advantages, such as fast response, small amount of sample, and low consumption of reagents, as compared with the conventional system. With such a small system, design of the detector units is very important to monitor analytical performance. This paper introduces some examples of micromachined detectors for miniaturized chemical analysis systems.

Catecholamines↗
PubMed2002

Rapid determination of serum melatonin by ESI-MS-MS with direct sample injection.

This paper describes a rapid, simple and sensitive analytical method for the quantitative determination of melatonin in human serum by ESI-MS-MS with direct serum sample injection and on-line extraction. The method uses N-acetyltryptamine as the internal standard. It has high specificity and sensitivity for serum melatonin analysis. The internal calibration curve shows a wide linear range from 0.500 to 200 ng/ml with a correlation coefficient, R(2) > 0.999. The limit of quantitation is 0.500 ng/ml and the limit of detection is 0.100 ng/ml with 10-microl sample injection. The recoveries of serum melatonin at three levels are approximately 70%. The intra-assay precision (n = 5) is between 0.8 and 2.0% and the inter-assay precision (n = 3) is between 1.5 and 5.9% over the calibration range. This method has a total analysis time of less than 9 min. It can be used for the measurement of melatonin in human blood.

Flow Injection Analysis↗
PubMed2003

Optimization of a preparative capillary gas chromatography-mass spectrometry system for the isolation and harvesting of individual polycyclic aromatic hydrocarbons.

Operation parameters of a preparative capillary gas chromatography (pcGC) system were optimized to facilitate clean and efficient harvesting of individual polycyclic aromatic hydrocarbons (PAHs) for subsequent compound-specific radiocarbon analysis. For PAHs, the recommended optimized settings of the specially-designed pcGC cooled injection system (CIS) and preparative fraction collector (PFC) are: 5 s CIS solvent venting time, deactivation of CIS "stop flow" injection mode, autoinjector "fast injection" mode, 60 s CIS splitless time, 340 degrees C PFC switch temperature, and 30 degrees C (ambient) trapping temperature. These optimized conditions yielded highly reproducible, pure, and efficient pcGC harvesting of six PAHs with mass recoveries of 90-100% and purity of the isolates of 97-100%.

Flow Injection Analysis↗
PubMed2004

Determination of (+)-3,3',5-triiodo-L-thyronine (L-T3) from serum using a sequential injection analysis/immunosensor system.

A sequential injection analysis/immunosensor system is proposed for the analysis of T3 in serum with a rate of 75 samples/hr. The immunosensor design is based on the physical immobilization of anti-T3 in carbon paste. The working concentration range of the immunosensor in a sequential injection analysis system is between 3.4 and 340 ng/mL with a limit of detection of 2.19 ng/mL. The system is very reliable and very easy to design and operate.

Biosensing Techniques↗
PubMed2006

Sequential injection titration with spectrophotometric detection for the assay of acidity in fruit juices.

A simple sequential injection analysis (SIA) with spectrophotometric detection for an assay of acidity in fruit juice was investigated. An alkaline reagent (sodium hydroxide), a sample and an indicator (phenolphthalein) were first aspirated and stacked as adjacent zones in a holding coil. With flow reversal through a reaction coil to the detector, zone penetration occurred, leading to a neutralization reaction that caused a decrease in the color intensity of the indicator being monitored for absorbance at 552 nm. The effects of various parameters were studied. Linear calibration graphs for acidities of 0.2 - 1.0 and 0.5 - 2.5% w/v citric acid as a standard, with a relative standard deviation of 1% (acidity of 0.3 - 0.6% w/v as citric acid, n=11) and a sample throughput of 30 samples h(-1), were achieved. The developed method was validated by a standard titrimetric method for assaying the acidity of fruit juice samples.

Beverages↗
PubMed2001

Flow-injection manifold for the simultaneous spectrophotometric determination of Fe(II) and Fe(III) using 2,2'-dipyridyl-2-pyridylhydrazone and a single-line double injection approach.

A simple and rapid flow-injection (FI) method is reported for the simultaneous spectrophotometric determination of Fe(II) and Fe(III) in pharmaceutical products. The method is based on the reaction of Fe(II) with 2,2'-dipyridyl-2-pyridylhydrazone (DPPH) in acidic medium to form a water-soluble reddish complex (lambdamax=535 nm). Fe(III) reacts with DPPH under flow conditions only after its on-line reduction by ascorbic acid (AsA). Both analytes were determined in the same run via a double-injection valve, which enabled the simultaneous injection of two sample volumes in the same carrier stream (,,single-line double-injection" approach). The two well-defined peaks produced corresponded to total iron [Fe(II)+Fe(III)] and Fe(II). Speciation of the analytes in their mixtures was achieved by multiple regression analysis. The calibration curves obtained were linear over the ranges 0-30 and 0-50 mg L(-1) for Fe(II) and Fe(II), respectively, and the precision [s(r)=1.0% for Fe(II) and 1.5% for Fe(III)] was satisfactory. The method proved to be selective and adequately sensitive (cL=0.25 and 0.17 mg L(-1) for Fe(III) and Fe(II), respectively, in mixtures). Application of the method to the analysis of pharmaceutical samples resulted in excellent accuracy; the percent mean recoveries were in the range 99.0-102.0% for both Fe(II) and Fe(III) and the mean relative error was e(r)=1.0%.

2,2'-Dipyridyl↗
PubMed2002

An electrochemical ELISA procedure for the screening of 17beta-estradiol in urban waste waters.

A sensitive electrochemical enzyme-linked immunosorbent assay (ELISA) has been used for the detection of 17beta-estradiol in waste waters. The activity of the label enzyme (horseradish peroxidase) was measured electrochemically using 3,3',5,5'-tetramethylbenzidine as electrochemical substrate. The detection limit was estimated to be 5 pg mL(-1), interday and intraday precision (RSD), ranged from 1 to 3% and from 3 to 6%, respectively. Analysis of waste waters from three different treatment plants demonstrated no matrix effect both for samples diluted 1:1 in buffer and diethyl ether extracted. Data on 36 samples analysed by an LC-ESI-MS-MS procedure and by the electrochemical ELISA assay were compared. Results correlated well. The electrochemical enzyme immunoassay appears suitable as a screening tool for analysis of estradiol in waste waters.

Electrochemistry↗
PubMed2003

Flow NMR applications in combinatorial chemistry.

Flow NMR techniques are now well accepted and widely used in many areas of drug discovery. Although natural-product-, rational-drug-design-, and NMR-screening-programs have begun to use flow NMR more routinely, flow NMR has not yet gained widespread acceptance in combinatorial chemistry, even though it has been shown to be a potentially useful tool. Recent developments in DI-NMR, FIA-NMR, and LC-NMR will help flow NMR eventually gain a wider acceptance within combinatorial chemistry. These developments include LC-NMR-MS instrumentation, flow probe improvements, new pulse sequences, improved automation of NMR data analysis, and the application of flow NMR to related fields in drug discovery.

Animals↗
PubMed2003

Biosensors for the determination of ortho-acetyl-L-carnitine. Their utilization as detectors in a sequential injection analysis system.

In order to determine ortho-acetyl-L-carnitine, two biosensors were proposed. The biosensors were designed using physical immobilization of L-amino acid oxidase (L-AAOD) and horseradish peroxidase (HRP). Electrode characteristics were obtained and compared for the two carbon paste (graphite powder and paraffin oil) biosensors. The linear concentration ranges for the proposed biosensors were in the ranges of fmol/L to nmol/L, magnitude order with low limits of detection. Due to their reliability, the biosensors were used as detectors in a sequential injection analysis system, and gave reliable results for on-line assay of ortho-acetyl-L-carnitine in synthesis process control with a frequency of 75 samples per hour.

Acetylcarnitine↗
PubMed2006

Respirometric 13C flux analysis--Part II: in vivo flux estimation of lysine-producing Corynebacterium glutamicum.

A novel method for metabolic flux studies of central metabolism which is based on respirometric (13)C flux analysis, i.e., parallel (13)C tracer studies with online CO(2) labeling measurements is applied to flux quantification of a lysine-producing mutant of Corynebacterium glutamicum. For this purpose, 3 respirometric (13)C labeling experiments with [1-(13)C(1)], [6-(13)C(1)] and [1,6-(13)C(2)] glucose were carried out in parallel. All fluxes comprising the reactions of glycolysis, of TCA cycle, of C3- and C4-metabolite interconversion and of lysine biosynthesis as well as the net reactions in the pentose phosphate pathway could be quantified solely using experimental data obtained from CO(2) labeling and extracellular rate measurements. At key branch points, 68+/-5% of glucose 6-phosphate were observed to be metabolized into pentose phosphate pathway and 48+/-1% of pyruvate into TCA cycle via pyruvate dehydrogenase. The results showed a good agreement with the previous studies using (13)C tracer cultivation and GC/MS analysis of proteinogenic amino acids. Also, respiratory quotient calculated from flux estimates using redox balance showed a high accordance with the value determined directly from the measured specific rates of O(2) consumption and CO(2) production. The results strongly support that the respirometric (13)C metabolic flux analysis is suited as an alternative to the conventional methods to study functional and regulatory activities of cells. The developed method is applicable to study growing or non-growing cells, primary and secondary metabolism and immobilized cells. Due to the non-accumulating nature of CO(2) labeling and instantaneous nature of the resulting fluxes, the method can also be used for dynamic profiling of metabolic activities. Therefore, it is complementary to conventional methods for metabolic flux analysis.

Bioreactors↗
PubMed2006

Fast Hadamard transform capillary electrophoresis for on-line, time-resolved chemical monitoring.

We report a new approach for collecting and deconvoluting the data in Hadamard transform capillary electrophoresis, referred to as fast Hadamard transform capillary electrophoresis (fHTCE). Using fHTCE, total analysis times can be reduced by up to 48% per multiplexed separation compared to conventional Hadamard transform capillary electrophoresis (cHTCE) while providing comparable signal-to-noise ratio enhancements. In fHTCE, the sample is injected following a pseudorandom pulsing sequence derived from the first row of a simplex matrix (S-matrix) in contrast to cHTCE, which utilizes a sequence of twice the length. In addition to the temporal savings provided by fHTCE, a 50% reduction in sample consumption is also realized due to the decreased number of sample injections. We have applied fHTCE to the analysis of mixtures of neurotransmitters and related compounds to yield improved signal-to-noise ratios with a total analysis time under 10 s. In addition, we demonstrate the capability of fHTCE to perform time-resolved monitoring of changes in the concentration of model neurochemical compounds.

Electrophoresis, Capillary↗
PubMed1995

Determination of oxalate in urine and plasma using reversed-phase ion-pair high-performance liquid chromatography with tris(2,2'-bipyridyl)ruthenium(II)-electrogenerated chemiluminescence detection.

Oxalate is quantitated in both urine and plasma samples using reversed-phase ion-pair high-performance liquid chromatography (HPLC) with tris(2,2'-bipyridyl)ruthenium(II) [Ru(bpy)2+(3)]-electrogenerated chemiluminescent (ECL) detection. Underivatized oxalate was separated on a reversed-phase column (Zorbax ODS) using a mobile phase of 10% methanol in 100 mM phosphate buffer at pH 7.0. The eluted compounds were combined with a stream of 2 mM Ru(bpy)2+(3) at a mixing tee before the ECL flow-cell. In the flow-cell, Ru(bpy)2+(3) is oxidized to Ru(bpy)3+(3) at a platinum electrode, and reacts with oxalate to produce chemiluminescence (CL). Urine samples were filtered and diluted prior to injection. Plasma samples were deproteinized before injection. A 25-microliters aliquot of sample was injected for analysis. Possible interferants, including amino acids and indole-based compounds, present in biological samples were investigated. Without the separation, amino acids interfere by increasing the total observed CL intensity; this is expected because they give rise to CL emission on their own in reaction with Ru(bpy)3+(3). Indole compounds exhibit a unique interference by decreasing the CL signal when present with oxalate. Indoles inhibit their own CL emission at high concentrations. By use of the indicated HPLC separation, oxalate was adequately separated from both types of interferants, which thus had no effect on the oxalate signal. Urine samples were assayed by both HPLC and enzymatic tests, the two techniques giving similar results, differing only by 1%. Detection limits were determined to be below 1 microM (1 nmol/ml) or 25 pmol injected. The working curve for oxalate was linear throughout the entire clinical range in both urine and plasma.

2,2'-Dipyridyl↗
PubMed2001

Spectrophotometric determination of chloride in mineral and drinking waters using sequential injection analysis.

An on-line sequential injection system has been developed for spectrophotometric determination of chloride in drinking mineral, natural, and ground waters. Samples containing different concentrations of chloride were analyzed. The analysis is based on detection of the red iron(III) thiocyanate complex. The complex was monitored spectrophotometrically at 480 nm using de-ionized water as the carrier stream at a flow rate of 3.21 mL min(-1). The method was found to be linear within the range 0-50 mg L(-1) chloride; the detection limit was 3.01 mg L(-1). The fully automated method can be used to analyze 37 samples per hour with a relative standard deviation (RSD) better than 2.50%.

Chlorides↗
PubMed2001

Chromatographic analysis of compounds of pharmaceutical interest.

A set of 17,600 samples belonging to our compound collection is selectively examined by liquid chromatography with UV, evaporative light scattering, and mass spectrometric detection methods. At least 70% of this set consists of pure samples with the expected structures. Subsequent studies by flow injection mass spectrometry show that this value is a conservative estimate and that the actual percentage of pure and correct compounds is close to 80%. Because this is the first time that sample quality information becomes available on such a large scale for the compound collection, it offers an opportunity to perform chemi-informatic studies for which structural integrity is essential. Results of these studies can be used to improve the selection of compounds for screening and evaluate the quality of compounds from particular sources.

Chromatography, High Pressure Liquid↗
PubMed2007

Fluorescence optosensing implemented with sequential injection analysis: a novel strategy for the determination of labetalol.

The coupling of sequential injection analysis and optosensing has been developed for the first time. It has been applied to the determination of labetalol in both pharmaceuticals and urine samples, with the analytical signal (native fluorescence) being monitored directly on sensing zone microbeads. The solid support used was the nonionic silica gel C18, using 20% methanol-water (v:v) as a carrier. By using a 1.5-ml sample volume, we achieved a detection limit of 3.3 ng ml-1. This sensitivity allowed the determination of the compound in urine samples. A recovery study was carried out at the labetalol levels usually found in urine after pharmaceuticals administration, and recovery percentages close to 100% were obtained. The relative standard deviation was 3.4% for 100 ng ml-1 labetalol. No pretreatment was needed for urine samples, only an appropriate dilution, therefore minimizing the time required per sample analysis. In addition, the determination of the analyte was also carried out in one pharmaceutical, with a satisfactory result being obtained.

Flow Injection Analysis↗