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PubMed1995

Principles and applications of biosensors for bioprocess monitoring and control.

Biosensors are useful analytical devices that can be integrated with on-line process monitoring schemes. In this article, the principles and applications of these devices for bioprocess monitoring are considered. Several different types of biosensors are described, and the applications and limitations of flow injection analysis (FIA) for these applications are discussed. It is hoped that the background provided here can be useful to researchers in this area.

Animals↗
PubMed2005

A novel method for the filterless preconcentration of iron.

A novel method of analysis of iron by filterless preconcentration is presented. This is the first example of efficient preconcentration of a refractory transition metal where coprecipitation and columns were omitted. The method applies a manifold of flow injection analysis (FIA) to iron species that are preconcentrated on the inner walls of a tubular reactor. It was found that the adsorption of iron species to the walls was particularly pronounced in reactors of nylon material and enrichment factors of 30-35 could be attained, as dependent on the length of the reactor and on the time of preconcentration. In the preconcentration step of the FIA accessory, the optimum efficacy was obtained when the acidity of the samples was adjusted by HCl to pH = 2.5 whereas the ammonia preconcentration buffer should be kept alkaline at pH = 9.8. After being preconcentrated on the tubular reactor, the iron species were eluted by hydrochloric acid and analysed by flame atomic absorption spectrometry (FAAS). An unprecedented low limit of detection (LOD, 3sigma) of 1.8 microg L(-1) was thus obtained for the analysis of iron by FAAS, and the calibration line was linear up to 100 microg L(-1). A high sampling frequency of 40 per hour was obtained and the protocol allowed analysis of small amounts of iron in drinking water, in digested samples and in saline water. The major influence of interferences originated from ligands that are known to complex strongly to iron species. The method thus developed was uncomplicated in operation and it exhibited an excellent long-term stability and a high selectivity. Further, it was environmentally safe owing to production of non-toxic waste disposals. Equally high enrichment factors (EF) were obtained for Fe(ii) and Fe(iii), which is explained by the very low solubility product of both species.

Adsorption↗
PubMed2006

Sequential flow injection determination of chlorine species using a triiodide-selective electrode detector.

A flow injection analysis (FIA) method for the determination of four residual chlorine species, namely combined available chlorine (CAC), free available chlorine (FAC), total available chlorine (TAC) and chlorite (ClO2-) was developed using a flow-through triiodide-selective electrode as a detector. An important strategy of speciation studies utilized the kinetic discrimination of reactions between the CAC and FAC with Fe2+, which was applied to the speciation of FAC, CAC and TAC. The speciation of available chlorine species and chlorite (an oxychlorine species) was achieved by using the same set-up, but using flow streams of different pH. The effects of the pH of the carrier stream, the flow rate and the sample volume were studied. The method exhibited linearity from 2.8 x 10(-6) to 2.8 x 10(-4) M active chlorine (expressed as OCl-) with a detection limit of 1.4 x 10(-6) M. The selectivity of the method was studied by examining the minimum pH for the oxidation of iodide by other oxidants, and also by assessing the potentiometric selectivity coefficients. The proposed method was successfully applied to the determination of chlorine species in tap water, and disinfecting formulations where good agreement occurred between the proposed and standard methods were found.

Chlorides↗
PubMed2006

Optically specific detection of D- and L-lactic acids by a flow-injection dual biosensor system with on-line microdialysis sampling.

A flow-injection dual biosensor system with microdialysis sampling is proposed for the simultaneous determination of D-lactic and L-lactic acids. The dialysate from the microdialysis tube is delivered to a sample loop of the six-way autoinjector and then automatically injected into the flow-injection line with a dual enzyme electrode arranged in perpendicular to the flow direction. The dual enzyme electrode is constructed by hybridizing a poly(1,2-diaminobenzene) film into two sensing parts which respond selectively to D-lactic and L-lactic acids, respectively, without any cross-reactivity. The proposed flow-injection analysis method can be successfully applied to the simultaneous determination of D,L-lactic acids in alcoholic beverages.

Alcoholic Beverages↗
PubMed2001

FIA of sildenafil citrate using UV-detection.

A flow injection analysis (FIA) of sildenafil citrate (SLD) using UV detection is described in this study. The best solvent system was found to be consisting of 0.2 M phosphate buffer at pH 8 having 10% MeOH. A flow rate of 1 ml. min(-1) was pumped and active material was detected at 292 nm. The calibration equation was linear in the range of 1x10(-6)-5x10(-6) M. Limit of detection (LOD) and limit of quantitation (LOQ) were calculated to be 3x10(-7) and 8.9x10(-7) M with a R.S.D. 1.9 and 0.6% (n=7), respectively. The proposed method was applied to the determination of SLD in VIAGRA tablet, containing 50 mg active material. The results were compared with those obtained from UV-Spectrophotometry. The results showed that there is a good agreement between FIA method and the UV-Spectrophotometry. The validation studies were realised by the related applications and the results were evaluated statistically. According to the results, insignificant difference was observed between the methods.

Flow Injection Analysis↗
PubMedDate not supplied

The automation of dissolution testing of solid oral dosage forms.

Dissolution testing of solid oral dosage forms plays a very important part both in the development of new products and in quality control. A fully automated system for dissolution testing known as AUTO DISS is presented and its components are described. On-line determination of active ingredient concentration is possible with the aid of an integrated automatic sampler in combination with various measuring instruments (UV-vis spectrometry, liquid chromatography and flow injection analysis). The suitability of the system is demonstrated by determination of the dissolution of brotizolam from tablets by FIA and of bepafant from capsules by diode-array spectroscopy.

Azepines↗
PubMed2006

Automatic method for the determination of Folin-Ciocalteu reducing capacity in food products.

In the present work, an automatic flow procedure based on multi-syringe flow injection analysis was developed for the assessment of Folin-Ciocalteu reagent (FCR) reducing capacity in several types of food products using gallic acid as the standard. Different strategies for mixing of sample and reagent were tested (continuous flow of FCR, merging zones, and intercalated zones approaches); lower reagent consumption and higher determination throughput were attained for the merging zones approach (100 microL of sample+100 microL of FCR). The application of the proposed method to compounds with known antioxidant activity (both phenolic and nonphenolic) and to samples (wines, beers, teas, soft drinks, and fruit juices) provided results similar to those obtained by the conventional batch method. The detection limit was 0.6 mg L-1, and the determination frequency was about 12 h-1. Good repeatability was attained (RSD<1.3%, n=10).

Antioxidants↗
PubMed2007

NADH screen-printed electrodes modified with zirconium phosphate, Meldola blue, and Reinecke salt. Application to the detection of glycerol by FIA.

Bulk screen-printed electrodes (bSPEs) modified with zirconium phosphate (ZrP) and Meldola blue (MB) and by electrochemical deposition of a Reineckate film (bMBZrPRs-SPEs) have been constructed and used as NADH sensors. Cyclic voltammetric investigation of these bulk electrochemically modified screen-printed electrodes revealed stable catalytic activity in oxidation of the reduced form of the coenzyme nicotinamide adenine dinucleotide (NADH). Flow-injection analysis (FIA) coupled with amperometric detection confirmed the improved stability of the bMBZrPRs-SPEs (10(-4) mol L(-1) NADH, %RSD = 4.2, n = 90, pH 7.0). Other conditions, for example applied working potential (+50 mV relative to Ag|AgCl), flow rate (0.30 mL min(-1)) and pH-dependence (range 4.0-10.0) were evaluated and optimized. A glycerol biosensor, prepared by immobilizing glycerol dehydrogenase (GDH) on the working electrode area of a bMBZrPRs-SPE, was also assembled. The biosensor was most stable at pH 8.5 (%RSD = 5.6, n = 70, 0.25 mmol L(-1) glycerol). The detection and quantification limits were 2.8 x 10(-6) and 9.4 x 10(-6) mol L(-1), respectively, and the linear working range was between 1.0 x 10(-5) and 1.0 x 10(-4) mol L(-1). To assess the effect of interferences, and recovery by the probe we analyzed samples taken during fermentation of chemically defined grape juice medium and compared the results with those obtained by HPLC.

Beverages↗
PubMed2003

Flow injection amperometric determination of dipyrone in pharmaceutical formulations using a carbon paste electrode.

The behavior of a carbon paste electrode was investigated as an amperometric detector for the determination of dipyrone by flow injection analysis (FIA). The electrode presented low cost and easy construction by simple mixing of graphite powder and mineral oil. Initially, an electrochemical study of the dipyrone oxidation at a carbon paste electrode has been developed before its use in the FIA system. The oxidation currents monitored at +0.35 V versus Ag/AgCl, were proportional to the dipyrone concentrations. Experimental parameters, such as nature of supporting electrolyte, pH of the carrier solution, flow rate, sample volume injection and probable interferents were investigated. Under the best experimental conditions selected, the calibration curve for dipyrone was linear in the concentration range from 4.91 x 10(-6) to 2.50 x 10(-4) M l(-1) (I(anodic)/microA)=0.056+81.06 [dipyrone]) with a detection limit of 2.07 x 10(-6) M l(-1). Recoveries ranged from 93.8 to 100.8% and an analytical frequency of 130 h(-1) was achieved. The proposed flow procedure has been satisfactorily applied to the determination of dipyrone in several pharmaceutical formulations.

Carbon↗
PubMed2002

Co-immobilization of polymeric luminol, iron(II) tris(5-aminophenanthroline) and glucose oxidase at an electrode surface, and its application as a glucose optrode.

The anodic polymerization of 3-aminophthalhydrazide (luminol) and iron(II) tris 5-aminophenanthroline (Fe(phen-NH2)3(2+)) has been reported in this paper. A bilayer electrode was developed based on these polymers and the ITO conductive glass (denoted ITO[Fe(phen-NH2)3(2+)]luminol electrode). This electrode emitted light (lambdaem: 430 nm) as it was brought into contact with H2O2. At pH 10, the resulting electrochemiluminescence (ECL) showed a linear relationship with the concentration of H2O2 in the range of 10 microM(-1) mM. This bilayer electrode also showed an application potential for the detection of glucose after being further modified with glucose oxidase (denoted ITO[Fe(phen-NH2)3(2+)]luminol]GOx electrode). Although the resulting ECL decayed more rapidly in concentrated glucose solutions (e.g., I M) because of the consumption of luminol during use, the decay became less severe in diluted glucose solutions (e.g., 10 mM). According to the flow injection analysis, a linear relationship existed between the ECL and the concentration of glucose from 10(-5)-10(-3) M at pH 9. The detection limit could reach a level of 5 x 10(-5) M at this pH.

Electrochemistry↗
PubMed2000

Flow injection determinations of artificial sweeteners: a review.

A review is presented to show the advantages involved in the use of Flow Injection Analysis (FIA) for the determination of artificial sweeteners. The FI methods proposed for the determination of artificial sweeteners are described and compared on the basis of the detection technique used. Analytical data of interest and interferences are discussed for each sweetener.

Aspartame↗
PubMed1997

Biosensors based on flow-through systems.

When combined with biosensors as the sensing element microdialysis and flow injection analysis (FIA) systems become sophisticated tools for handling analytical processes. In particular a FIA system offers a high degree of automation together with high reproducibility and small sample volumes, whereas the biosensor, allows selective and sensitive measurements of the various analytes. Here we describe first a miniaturised microdialysis flow-through system developed for glucose determination, then we focus on amperometric immunosensors and on microbial sensors. In the former, antibodies against low molecular weight environmental contaminants or against high molecular weight proteins are responsible for analyte detection, whereas the latter use immobilised microorganisms as the recognising element for monitoring water pollutants.

2,4-Dichlorophenoxyacetic Acid↗
PubMed2005

Preparation and application of TiO2 photocatalytic sensor for chemical oxygen demand determination in water research.

In this work, a TiO(2) photocatalytic sensor was prepared and utilized into flow injection analysis (FIA) for chemical oxygen demand (COD) determination. With a positive bias potential of 0.4V (vs. Ag/AgCl) applied to the sensor and a 12-W quartz UV lamp illuminating it, photocurrent, due to the charge transfer at the interface of TiO(2) sensor and the passing solution, was recorded and its change (deltaI(Photo)) caused by the detected sample was calculated to characterize the COD value of the sample. Under the optimizing conditions, the sensor responded linearly to the COD of D-glucose solution in the range of 0.5-235 mg/L, with a linear correlation coefficient of 0.9998. Its application in artificial wastewater analysis has achieved results in good agreement with those from the conventional dichromate method; meanwhile, the process requires no hypertoxic reagents and less analysis time, suggesting that it would be another appropriate method for COD determination in water assessment.

Catalysis↗
PubMed2005

Flow-through chloroquine sensor and its applications in pharmaceutical analysis.

Poly (vinyl chloride) membrane electrodes that responded selectively towards the antimalarial drug chloroquine are described. The electrodes were based on the use of the lipophilic potassium tetrakis(4-chlorophenyl)borate as ion-exchanger and bis(2-ethylhexyl)adipate (BEHA), or trioctylphosphate (TOP) or dioctylphenylphosphonate (DOPP) as plasticizing solvent mediator. All electrodes produced good quality characteristics such as Nernstian- and rapid responses, and are minimally interfered with by the alkali and alkaline earth metal ions tested. The membranes were next applied to a flow-through device, enabling it to function as flow-injection analysis (FIA) detector. The performance of the sensor after undergoing the FIA optimization was further evaluated for its selectivity characteristics and lifetime. Results for the determination of chloroquine in synthetic samples that contained common tablet excipients such as glucose, starch, and cellulose, and other foreign species such as cations, citric acid or lactic acid were generally satisfactory. The sensor was also successfully used for the determination of the active ingredients in mock tablets, synthetic fluids and biological fluids. The sensor was applied for the determination of active ingredients and the dissolution profile of commercial tablets was also established.

Antimalarials↗
PubMed1998

"Reagentless" flow injection determination of ammonia and urea using membrane separation and solid phase basification.

Flow injection analysis instrumentation and methodology for the determination of ammonia and ammonium ions in an aqueous solution are described. Using in-line solid phase basification beds containing crystalline media. the speciation of ammoniacal nitrogen is shifted toward the un-ionized form. which diffuses in the gas phase across a hydrophobic microporous hollow fiber membrane into a pure-water-containing analytical stream. The two streams flow in a countercurrent configuration on opposite sides of the membrane. The neutral pH of the analytical stream promotes the formation of ammonium cations, which are detected using specific conductance. The methodology provides a lower limit of detection of 10 microgram/L and a dynamic concentration range spanning three orders of magnitude using a 315-microliters sample injection volume. Using immobilized urease to enzymatically promote the hydrolysis of urea to produce ammonia and carbon dioxide, the technique has been extended to the determination of urea.

Ammonia↗
PubMed1995

Optimization of a modified electrode for the sensitive and selective detection of alpha-dipeptides.

Sensitive and selective detection of dipeptides is important in neurochemistry. We have developed a flexible detection scheme for dipeptides based on a modified carbon electrode. The modification arises from the anodic treatment of the carbon electrode in alkaline solution. The flexibility of the detection scheme arises from the different conditions used in both the modification and the detection. It is shown that the modification step requires the presence of cupric ion, while the detection step does not. On the other hand, it is shown that the presence of copper in the detection eluent, as well as the pH of the environment, can be used in controlling the selectivity of the modified electrode. For example, the modified electrode is more selective for alpha-dipeptides over beta- and gamma-dipeptides as well as amino acids at pH 9.8, whereas it is selective for all dipeptides over amino acids at pH 8.0. Detection limits of dipeptides on the order of 10 nM were achieved at pH 8.0 by flow-injection analysis with a knotted Teflon tubing connecting the injector and the detector that gave a typical peak volume of about 0.50 ml at 1.0 ml/min. From surface analysis it is shown that the oxygenation of the glassy carbon electrode gives rise to the selectivity. The oxidation of dipeptides at the modified electrode is completely inhibited by 10 mM Mg2+ in the eluent.

Chromatography, Liquid↗
PubMed1997

Development and validation of a flow-injection method for the determination of albumin tannate, the active component of a pharmaceutical preparation.

A flow-injection analysis method for the determination of albumin tannate in tablets is reported. After optimization of the variables involved, the method has been characterized and validated in terms of calibration using three procedures: repeatability and reproducibility; ruggedness; and selectivity. Finally, it has been applied to real samples (tablets).

Albumins↗
PubMed1997

The lipoxygenase sensor, a new approach in essential fatty acid determination in foods.

Both an enzyme electrode and enzyme column with immobilized lipoxygenase, respectively, were used for the determination of essential fatty acids. The former was applied in a batch system, the latter was part of a fully automated flow injection analysis (FIA)-system. The oxygen consumption due to the lipoxygenase catalysed oxygenation of essential fatty acids was monitored amperometrically. Both systems were compared with regard to linear ranges of the calibration plots, sensitivities, detection limits, apparent Michaelis-Menten constants and lifetimes. The enzyme electrode showed different sensitivities for linoleic and alpha-linolenic acids, the most common essential fatty acids. The reason for this was not a second oxygenation step by lipoxygenase in case of alpha-linolenic acid, but a different dialytic behaviour of the two substrates. Hence, only the FIA-system was used for the determination of these fatty acids in real matrices such as vegetable oils and margarines. In the presence of detergent the triglycerides of the hydrophobic food samples were converted into water soluble glycerol and free fatty acids by a 15 min incubation with a ready to use lipase/esterase-mix, thus avoiding the use of organic solvents for analysis. Results obtained by the enzymatic FIA-system were in excellent agreement with those obtained by standard gas chromatography.

Biosensing Techniques↗