Disposable Voltammetric Immunosensors Integrated with Microfluidic Platforms for Biomedical, Agricultural and Food Analyses: A Review.

Disposable immunosensors are analytical devices used for the quantification of a broad variety of analytes in different areas such as clinical, environmental, agricultural and food quality management. They detect the analytes by means of the strong interactions between antibodies and antigens, which provide concentration-dependent signals. For the herein highlighted voltammetric immunosensors, the analytical measurements are due to changes in the electrical signals on the surface of the transducers. The possibility of using disposable and miniaturized immunoassays is a very interesting alternative for voltammetric analyses, mainly, when associated with screen-printing technologies (screen-printed electrodes, SPEs), and microfluidic platforms. The aim of this paper is to discuss a carefully selected literature about different examples of SPEs-based immunosensors associated with microfluidic technologies for diseases, food, agricultural and environmental analysis. Technological aspects of the development of the voltammetric immunoassays such as the signal amplification, construction of paper-based microfluidic platforms and the utilization of microfluidic devices for point-of-care testing will be presented as well.

Electrochemical immunosensors - A powerful tool for analytical applications.

Immunosensors are biosensors based on interactions between an antibody and antigen on a transducer surface. Either antibody or antigen can be the species immobilized on the transducer to detect antigen or antibody, respectively. Because of the strong binding forces between these biomolecules, immunosensors present high selectivity and very high sensitivity, making them very attractive for many applications in different science fields. Electrochemical immunosensors explore measurements of an electrical signal produced on an electrochemical transductor. This signal can be voltammetric, potentiometric, conductometric or impedimetric. Immunosensors utilizing electrochemical detection have been explored in several analyses since they are specific, simple, portable, and generally disposable and can carry out in situ or automated detection. This review addresses the potential of immunosensors destined for application in food and environmental analysis, and cancer biomarker diagnosis. Emphasis is given to the approaches that have been used for construction of electrochemical immunosensors. Additionally, the fundamentals of immunosensors, technology of transducers and nanomaterials and a general overview of the possible applications of electrochemical immunosensors to the food, environmental and diseases analysis fields are described.

Fast analysis of terbutaline in pharmaceuticals using multi-walled nanotubes modified electrodes from recordable compact disc.

In this study, homemade disposable gold electrodes made from recordable compact disks were modified with carbon nanotubes for amperometric quantification of terbutaline sulfate in pharmaceutical products. A flow cell using an impingent jet of solution on the electrode surface was build and used for amperometric detection, and a series of experiments were carried out to find the best experimental conditions for the new electrode in a specially designed cell. A linear response for terbutaline was obtained in the range from 3.0 × 10(-6) to 5.0 × 10(-4) mol L(-1) (at 0.63 V vs. Ag/AgCl). The limits of detection and quantification were calculated as 5.8 × 10(-7) mol L(-1) (S/N = 3) and 1.9 × 10(-6) mol L(-1) (S/N = 10), respectively. A frequency of 30 injections h(-1) was attained. The proposed method was successfully applied to the analyses of commercial syrup samples, and all results were in good agreement with those obtained by using high performance liquid chromatography and capillary electrophoresis-tandem mass spectrometry.

Quantification of terbinafine in pharmaceutical tablets using capillary electrophoresis with contactless conductivity detection and batch injection analysis with amperometric detection.

Terbinafine hydrochloride (TerbHCl) is an allylamine derivative with fungicidal action, especially against dermatophytes. Different analytical methods have been reported for quantifying TerbHCl in different samples. These procedures require time-consuming sample preparation or expensive instrumentation. In this paper, electrochemical methods involving capillary electrophoresis with contactless conductivity detection, and amperometry associated with batch injection analysis, are described for the determination of TerbHCl in pharmaceutical products. In the capillary electrophoresis experiments, terbinafine was protonated and analyzed in the cationic form in less than 1 min. A linear range from 1.46 to 36.4 µg mL(-1) in acetate buffer solution and a detection limit of 0.11 µg mL(-1) were achieved. In the amperometric studies, terbinafine was oxidized at +0.85 V with high throughput (225 injection h(-1)) and good linear range (10-100 µmol L(-1)). It was also possible to determine the antifungal agent using simultaneous conductometric and potentiometric titrations in the presence of 5% ethanol. The electrochemical methods were applied to the quantification of TerbHCl in different tablet samples; the results were comparable with values indicated by the manufacturer and those found using titrimetry according to the Pharmacopoeia. The electrochemical methods are simple, rapid and an appropriate alternative for quantifying this drug in real samples.

Fast and accurate analysis of drugs using amperometry associated with flow injection analysis.

This review presents a general overview about the amperometric detection potentialities associated to flow injection analysis (FIA). Fundamental aspects, developments, applications and advantages accrued from the coupling of voltammetry with FIA for pharmaceutical analyses are discussed. The selected references present several examples for this association in various classes of drugs and support their advantages. Examples illustrate that the amperometric techniques coupled with flow system can usually be used in drug routine analysis without sample pretreatment. Amperometry/FIA has proved to be an excellent alternative to the chromatographic techniques and it has been used in routine analysis, from the simplest analytes to more complex species, solving even special cases such as the enantiomeric analysis of pharmaceutical compounds with a chiral moiety, which requires time-consuming sample preparation or expensive instrumentation. This revision also aims to contribute for reducing the gap between the vast possibilities enabled by electroanalytical techniques and their effective utilization for pharmaceutical analysis.

Flow injection analysis using carbon film resistor electrodes for amperometric determination of ambroxol.

Flow injection analysis (FIA) using a carbon film sensor for amperometric detection was explored for ambroxol analysis in pharmaceutical formulations. The specially designed flow cell designed in the lab generated sharp and reproducible current peaks, with a wide linear dynamic range from 5x10(-7) to 3.5x10(-4) mol L(-1), in 0.1 mol L(-1) sulfuric acid electrolyte, as well as high sensitivity, 0.110 Amol(-1) L cm(-2) at the optimized flow rate. A detection limit of 7.6x10(-8) mol L(-1) and a sampling frequency of 50 determinations per hour were achieved, employing injected volumes of 100 microL and a flow rate of 2.0 mL min(-1). The repeatability, expressed as R.S.D. for successive and alternated injections of 6.0x10(-6) and 6.0x10(-5) mol L(-1) ambroxol solutions, was 3.0 and 1.5%, respectively, without any noticeable memory effect between injections. The proposed method was applied to the analysis of ambroxol in pharmaceutical samples and the results obtained were compared with UV spectrophotometric and acid-base titrimetric methods. Good agreement between the results utilizing the three methods and the labeled values was achieved, corroborating the good performance of the proposed electrochemical methodology for ambroxol analysis.

Carbon film resistor electrode for amperometric determination of acetaminophen in pharmaceutical formulations.

Flow injection analysis (FIA) with amperometric detection was employed for acetaminophen quantification in pharmaceutical formulations using a carbon film resistor electrode. This sensor exhibited sharp and reproducible current peaks for acetaminophen without chemical modification of its surface. A wide linear working range (8.0x10(-7) to 5.0x10(-4) mol L(-1)) in phosphate buffer solution as well as high sensitivity (0.143 A mol(-1) L cm(-2)) and low submicromolar detection limit (1.36x10(-7) mol L(-1)) were achieved. The repeatability (R.S.D. for 10 successive injections of 5.0x10(-6) and 5.0x10(-5) mol L(-1) acetaminophen solutions) was 3.1 and 1.3%, respectively, without any memory effect between injections. The new procedure was applied to the analyses of commercial pharmaceutical products and the results were in good agreement with those obtained utilizing a spectrophotometric method. Consequently, this amperometric method has been shown to be very suitable for quality control analyses and other applications with similar requirements.

Epinephrine quantification in pharmaceutical formulations utilizing plant tissue biosensors.

A plant tissue biosensor associated with flow injection analysis is proposed to determine epinephrine in pharmaceutical samples. The polyphenol oxidase enzymes present in the fibers of a palm tree fruits (Livistona chinensis), catalyses the oxidation of epinephrine to epinephrinequinone as a primary product. This product is then electrochemically reduced (at -0.10 V versus Ag/AgClsat) on the biosensor surface and the resulting current is used for the quantification of epinephrine. The biosensor provides a linear response for epinephrine in the concentration range from 5.0 x 10(-5) to 3.5 x 10(-4) mol l(-1). The limit of detection estimated for this interval was 1.5 x 10(-5) mol l(-1) and the correlation coefficient of 0.998, working under a flow rate of 2.0 ml min(-1) and using a sample loop of 100 microl. The repeatability (R.S.D. for 10 consecutive determinations of a 3.0 x 10(-4) mol l(-1) epinephrine solution) was 3.1%. The results obtained by the method here proposed were compared with the official UV spectrophotometric procedure and also using a plant tissue reactor. The responses obtained with the proposed strategies were in good agreement with both ways of analyses, whereas the values obtained by the official spectrophotometric method was strongly affected by benzoic acid, present in the formulation of pharmaceutical product utilized for inhalation. Such favorable results obtained with the carbon paste biosensor or utilizing the bioreactor, joined with the simplicity of its preparation turns these procedures very attractive for epinephrine quantification in pharmaceutical products.

Determination of salbutamol in syrups by capillary electrophoresis with contactless conductivity detection (CE-C(4)D).

This paper describes the separation and quantification of salbutamol in pharmaceutical products (salbutamol syrups) by capillary electrophoresis (CE) with contactless conductivity detection (C(4)D). The system was studied by micellar electrokinetic capillary chromatography (MEKC) and free solution capillary electrophoresis (FSCE), being the latter chosen in function of best resolution and sensitivity in comparison with the MEKC method. CE-C(4)D was applied to analysis of salbutamol in syrups utilizing 1.0 x 10(-2) molL(-1) acetic acid/sodium acetate buffer (pH 4.9) as running electrolyte. Tetraethylammonium (TEA) solution was used as internal standard. The results obtained include a linear dynamic range from 7. x 10(-5) to 3.0 x 10(-4) molL(-1) and good repeatability (R.S.D.=4.7% for n=10 for a 7.0 x 10(-5) molL(-1) salbutamol solution). The detection limit was calculated as 1.0 x 10(-5) molL(-1) and the limit of quantification was estimated as 3.3 x 10(-5) molL(-1). For syrups analysis the reproducibility presented deviations between 1.5% and 2.5% (three different days) obtained for measurements in triplicate.

Fast ultrasound-assisted treatment of urine samples for chronopotentiometric stripping determination of mercury at gold film electrodes.

This work describes an efficient, fast, and reliable analytical methodology for mercury determination in urine samples using stripping chronopotentiometry at gold film electrodes. The samples were sonicated in the presence of concentrated HC1 and H2O2 for 15 min in order to disrupt the organic ligands and release the mercury. Thirty samples can be treated over the optimized region of the ultrasonic bath. This sample preparation was enough to allow the accurate stripping chronopotentiometric determination of mercury in the treated samples. No background currents and no passivation of the gold film electrode due to the sample matrix were verified. The samples were also analyzed by cold vapour atomic absorption spectrometry (CV-AAS) and good agreement between the results was verified. The analysis of NIST SRM 2670 (Toxic Metals in Freeze-Dried Urine) also validated the proposed electroanalytical method. Finally, this method was applied for mercury evaluation in urine of workers exposed to hospital waste incinerators.