A highly sensitive amperometric sensor for oxygen based on iron(II) tetrasulfonated phthalocyanine and iron(III) tetra-(N-methyl-pyridyl)-porphyrin multilayers

The development of a highly sensitive sensor for oxygen is proposed using a glassy carbon (GC) electrode modified with alternated layers of iron(II) tetrasulfonated phthalocyanine (FeTsPc) and iron(III) tetra-(N-methyl-pyridyl)-porphyrin (FeT4MPyP). The modified electrode showed excellent catalytic activity for the oxygen reduction. The reduction potential of the oxygen was shifted about 330 mV toward less negative values with this modified electrode, presenting a peak current much higher than those observed on a bare GC electrode. Cyclic voltammetry and rotating disk electrode (RDE) experiments indicated that the oxygen reduction reaction involves 4 electrons with a heterogenous rate constant (k_obs) of 3 × 10⁵ mol⁻¹ L s⁻¹. A linear response range from 0.2 up to 6.4 mg L⁻¹, with a sensitivity of 4.12 μA L mg⁻¹ (or 20.65 μA cm⁻² L mg⁻¹) and a detection limit of 0.06 mg L⁻¹ were obtained with this sensor. The repeatability of the proposed sensor, evaluated in terms of relative standard deviation (R.S.D.) was 2.0% for 10 measurements of a solution of 6.4 mg L⁻¹ oxygen. The sensor was applied to determine oxygen in pond and tap water samples showing to be a promising tool for this purpose.     

Flow injection analysis system based on amperometric thin-film transducers for free chlorine detection in swimming pool waters

This work reports on the performance of a user-friendly flow injection analysis (FIA) system for the monitoring of free chlorine. A methacrylate flow cell integrating a gold thin-film microelectrode, together with an on-chip gold counter electrode, both fabricated by microfabrication technology, provided robustness, low output impedance, rapid response and low cost to the proposed flow system. An external Ag/AgCl reference electrode placed downstream the chip completes the electrochemical cell. Amperometric detection of chlorine was carried out at a set potential of +350 mV, without oxygen interference. The proposed flow system responded linearly to chlorine concentrations in a range from 0.2 to 5 mg l⁻¹, with a sensitivity of 0.23 μA l mg⁻¹, the estimated limit of detection being 0.02 mg l⁻¹. In addition, the system response was kept stable for at least 10 days (±3σ criterion), by keeping the flow system in an inert atmosphere when not in use. Fifteen samples of swimming pool waters were analyzed and no matrix effects were detected. Also, results were in good agreement with those obtained by a standard method. The excellent analytical performance of the system together with its good working stability would also enable its application for the detection of chlorine in other matrices such as tap water or chlorine stock solutions.     

Determination of picloram in natural waters employing sequential injection square wave voltammetry using the hanging mercury drop electrode

This paper describes the development of a sequential injection analysis method to automate the determination of picloram by square wave voltammetry exploiting the concept of monosegmented flow analysis to perform in-line sample conditioning and standard addition. To perform these tasks, an 800 μL monosegment is formed, composed by 400 μL of sample and 400 μL of conditioning/standard solution, in medium of 0.10 mol L⁻¹ H₂SO₄. Homogenization of the monosegment is achieved by three flow reversals. After homogenization the mixture zone is injected toward the flow cell, which is adapted to the capillary of a hanging drop mercury electrode, at a flow rate of 50 μL s⁻¹. After a suitable delay time, the potential is scanned from −0.5 to −1.0 V versus Ag/AgCl at frequency of 300 Hz and pulse height of 25 mV. The linear dynamic range is observed for picloram concentrations between 0.10 and 2.50 mg L⁻¹ fitting to the linear equation I_p = (−2.19 ± 0.03)C_picloram + (0.096 ± 0.039), with R² = 0.9996, for which the slope is given in μA L mg⁻¹. The detection and quantification limits are 0.036 and 0.12 mg L⁻¹, respectively. The sampling frequency is 37 h⁻¹ when the standard addition protocol is followed, but can be increased to 41 h⁻¹ if the protocol to obtain in-line external calibration curve is used for quantification. The method was applied for determination of picloram in spiked water samples and the accuracy was evaluated by comparison with high performance liquid chromatography using molecular absorption at 220 nm for detection. No evidences of statistically significant differences between the two methods were observed.     

A novel high selective and sensitive metronidazole voltammetric sensor based on a molecularly imprinted polymer-carbon paste electrode

The design and construction of a highly selective voltammetric sensor for metronidazole by using a molecularly imprinted polymer (MIP) as recognition element were introduced. A metronidazole selective MIP and a nonimprinted polymer (NIP) were synthesized and then incorporated in the carbon paste electrodes (CPEs). The sensor was applied for metronidazole determination using cathodic stripping voltammetric method. The MIP-CP electrode showed very high recognition ability in comparison to NIP-CPE. Some parameters affecting the sensor response were optimized and then the calibration curve was plotted. Two dynamic linear ranges of 5.64 × 10⁻⁵ to 2.63 × 10⁻³ mg L⁻¹ and 2.63 × 10⁻³ to 7.69 × 10⁻² mg L⁻¹ were obtained. The detection limit of the sensor was calculated as 3.59 × 10⁻⁵ mg L⁻¹. This sensor was used successfully for metronidazole determination in biological fluids.     

An amperometric sensor based on hemin adsorbed on silica gel modified with titanium oxide for electrocatalytic reduction and quantification of artemisinin

The present work describes the development of an amperometric sensor based on hemin immobilized on a titanium oxide modified silica toward detection of artemisinin (ARN) in neutral medium at an applied potential of −0.5 V vs. Ag/AgCl. The sensor presented its best performance in 0.1 mol L⁻¹ phosphate buffer solution, at pH 7.0. After optimizing the operational conditions, the sensor provided a linear response range for ARN reduction from 50 nmol L⁻¹ to 1000 nmol L⁻¹ with a sensitivity, detection and quantification limits of 24.66 A L mol⁻¹, 15 nmol L⁻¹ and 52 nmol L⁻¹, respectively. The proposed sensor showed a stable response for at least 80 successive determinations. The repeatability of the measurements with the sensor and the preparation of a series of electrodes, evaluated in terms of relative standard deviation, were 4.1% and 5.0%, respectively, for n = 10. The developed sensor was applied for the determination of ARN in the crude extracts of A. vulgaris L and the average recovery for these samples is 101.4 (± 3.1)%.     

Voltammetric performance and application of a sensor for sodium ions constructed with layered birnessite-type manganese oxide

The preparation and electrochemical characterization of a carbon paste electrode modified with layered birnessite-type manganese oxide for use as a sodium sensor is described. The effects of powder synthesis process (sol-gel and redox precipitation) for birnessite on the electrochemical activity of the sensor was investigated by cyclic voltammetry. The carbon paste electrode modified with birnessite-type manganese oxide that was synthesized by the sol-gel method showed a best electrochemical for sodium ions. The detection is based on the measurement of anodic current generated by oxidation of Mn(III) to Mn(IV) at the surface of the electrode and consequently the sodium ions extraction into the birnessite structure. The best voltammetric response was obtained for an electrode composition of 15% (w/w) birnessite oxide in the paste, a TRIS buffer solution of pH 8.0 and a scan rate of 50 mV s⁻¹. A sensitive linear voltammetric response for sodium ions was obtained in the concentration range of 7.89 × 10⁻⁵ to 3.49 × 10⁻⁴ mol L⁻¹ with a slope of 37.5 μA L mmol⁻¹ and a detection limit (3σ/slope) of 3.43 × 10⁻⁵ mol L⁻¹ using cyclic voltammetry. Under the working conditions, the proposed method was successfully applied to determination of sodium ions in urine samples.     

Immobilization of uricase within polystyrene using polymaleimidostyrene as a stabilizer and its application to uric acid sensor

A novel amperometric uric acid (UA) sensor has been developed by coating the surface of a gold electrode with a polystyrene (PS) membrane formed by 30 μL of a 30 mg mL⁻¹ PS chloroform solution combined with 30 μL of a 5 mg mL⁻¹ polymaleimidostyrene (PMS) solution as a dispersant for enzyme, uricase; this membrane has been successfully employed as an immobilization support for uricase. In the PS membrane, PMS forms micelle-like structures containing uricase in an active state. This immobilized uricase membrane permits the permeation of oxygen, which is consumed by the uricase reaction. A good linear relationship is obtained over the concentration range of 5-105 μM. The concentration of uric acid was determined at a negative potential based on the decrease in the reduction current of oxygen and the interference of l-ascorbic acid can be completely eliminated.     

Catalytic activity of iron hexacyanoosmate(II) towards hydrogen peroxide and nicotinamide adenine dinucleotide and its use in amperometric biosensors

Hydrogen peroxide and nicotinamide adenine dinucleotide (NADH) may be determined amperometrically using screen-printed electrodes chemically modified with iron(III) hexacyanoosmate(II) (Osmium purple) in flow injection analysis (FIA). The determination is based on the exploitation of catalytic currents resulting from the oxidation/reduction of the modifier. The performance of the sensor was characterized and optimized by controlling several operational parameters (applied potential, pH and flow rate of the phosphate buffer). Comparison has been made with analogous complexes of ruthenium (Ruthenium purple) and iron (Prussian blue). Taking into account the sensitivity and stability of corresponding sensors, the best results were obtained with the use of Osmium purple. The sensor exhibited a linear increase of the amperometric signal with the concentration of hydrogen peroxide in the range of 0.1-100 mg L⁻¹ with a detection limit (evaluated as 3σ) of 0.024 mg L⁻¹ with a R.S.D. 1.5% for 10 mg L⁻¹ H₂O₂ under optimized flow rate of 0.4 mL min⁻¹ in 0.1 M phosphate buffer carrier (pH 6) and a working potential of +0.15 V versus Ag/AgCl. Afterwards, a biological recognition element - either glucose oxidase or ethanol dehydrogenase - was incorporated to achieve a sensor facilitating the determination of glucose or ethanol, respectively. The glucose sensor gave linearity between current and concentration in the range from 1 to 250 mg L⁻¹ with a R.S.D. 2.4% for 100 mg L⁻¹ glucose, detection limit 0.02 mg L⁻¹ (3σ) and retained its original activity after 3 weeks when stored at 6 °C. Optimal parameters in the determination of ethanol were selected as: applied potential +0.45 V versus Ag/AgCl, flow rate 0.2 mL min⁻¹ in 0.1 M phosphate buffer carrier (pH 7). Different structural designs of the ethanol sensor were tested and linearity obtained was up to 1000 mg L⁻¹ with a maximum R.S.D. of 5.1%. Applications in food analysis were also examined.     

Biosensors for determination of glucose with glucose oxidase immobilized on an eggshell membrane

A glucose biosensor using an enzyme-immobilized eggshell membrane and oxygen electrode for glucose determination has been fabricated. Glucose oxidase was covalently immobilized on an eggshell membrane with glutaraldehyde as a cross-linking agent. The glucose biosensor was fabricated by positioning the enzyme-immobilized eggshell membrane on the surface of a dissolved oxygen sensor. The detection scheme was based on the depletion of dissolved oxygen content upon exposure to glucose solution and the decrease in the oxygen level was monitored and related to the glucose concentration. The effect of glutaraldehyde concentration, pH, phosphate buffer concentration and temperature on the response of the glucose biosensor has been studied in detail. Common matrix interferents such as ethanol, d-fructose, citric acid, sodium benzoate, sucrose and l-ascorbic acid did not give significant interference. The resulting sensor exhibited a fast response (100 s), high sensitivity (8.3409 mg L⁻¹ oxygen depletion/mmol L⁻¹ glucose) and good storage stability (85.2% of its initial sensitivity after 4 months). The linear response is 1.0×10⁻⁵ to 1.3×10⁻³ mol L⁻¹ glucose. The glucose content in real samples such as commercial glucose injection preparations and wines was determined, and the results were comparable to the values obtained from a commercial glucose assay kit based on a spectrophotometric method.     

A composite thin film optical sensor for dissolved oxygen in contaminated aqueous environments

A robust optical composite thin film dissolved oxygen sensor was fabricated by ionically trapping the dye ruthenium(II) tris(4,7-diphenyl-1,10-phenanthroline) dichloride in a blended fluoropolymer matrix consisting of Nafion^® and Aflas^®. Strong phosphorescence, which was strongly quenched by dissolved oxygen (DO), was observed when the sensor was immersed in water. The sensor was robust, optically transparent, with good mechanical properties. Fast response, of a few seconds, coupled with sensitivity of about 0.1 mg L⁻¹ (DO) over the range 0-30 mg L⁻¹ and resistance to leaching, were also exhibited by this system. The Stern-Volmer (SV) plot exhibited slight downward turning at all oxygen concentrations. A linear plot was obtained when the SV equation was modified to account for the varying sensitivity of dye molecules in the matrix to the quencher. Good long term stability was observed.     

Effluent treatment using electrochemically bleached seawater-oxidative degradation of pollutants

Use of seawater electrolytically enriched with hypochlorite and the in situ generation of hypochlorite on the high seas, stand a good chance for disinfection and decrease of bio and non-biodegradable organics in effluent before discharged into estuaries and deep oceans. Enriched seawater effectively decreased the biological oxygen demand measured over 5 days (BOD) and chemical oxygen demand (COD) levels of semi-treated wastewater. The oxidative degradation of Brilliant Blue, a triaryl industrial dye by hypochlorite and electrolytically enriched seawater are compared at pH 6.5. Both had similar magnitude second-order rate constants (21±1 M⁻¹ s⁻¹) and procedure is feasible. Increase in acid concentration enhanced the reaction rate. With 1:1 and 1:100 molar ratios of dye to hypochlorite, the COD=140 mg L⁻¹ of 1.0×10⁻³ M dye reduced to 100 and 30 mg L⁻¹ respectively.     

Investigation on the application of titania nanorod arrays to the determination of chemical oxygen demand

In the present paper, the TiO₂ nanorod arrays electrode was developed as a sensor for the determination of chemical oxygen demand (COD) based on a photoelectrochemical degradation principle. Effects of common parameters, such as applied potential, light intensity and pH on its analytical performance were investigated. Under the optimized conditions, the nanorod arrays electrode was successfully applied in the COD determination for both synthetic and real samples. In the COD determination, the proposed method can achieve a practical detection limit of 18.3 mg L⁻¹ and a linear range of 20–280 mg L⁻¹. Furthermore, the results obtained by the proposed method were well correlated with those obtained using the conventional (i.e., dichromate) COD determination method. The main advantages of this COD determination method were its simplicity, long term stability and environmental friendly (corrosive and toxic reagents not consumed). This work would open a new application area (COD determination) of the TiO₂ nanorod arrays.     

Different strategies for the direct determination of amoxicillin in human urine by second-order multivariate analysis of kinetic-spectrophotometric data

The kinetic evolution of UV-visible absorption spectra of amoxicillin in the presence of copper(II) ions has been processed by the second-order multivariate methods parallel factor analysis (PARAFAC) and also by a novel approach based on partial least-squares with residual bilinearization (PLS/RBL). The latter one is employed for the first time to evaluate kinetic-spectral information. The mechanism of the analyte metal-catalyzed hydrolysis involves a reaction intermediate and a final reaction product, both with spectra which may allow for the determination of amoxicillin in human urine, even in the presence of unsuspected sample components. This is possible thanks to the second-order advantage exploited by the employed chemometric algorithms, among which PARAFAC and PLS/RBL gave the best results. Amoxicillin was determined in a series of spiked and real urine samples, which allowed to perform, respectively, a recovery study and a comparison with the reference high-performance liquid chromatographic technique. The best figures of merit were obtained with PLS/RBL, namely sensitivity, 0.5 AU L mg⁻¹ (AU = absorbance units), analytical sensitivity, 500 L mg⁻¹ and limit of detection, 6 mg L⁻¹. Relative advantages and disadvantages of the employed algorithms are discussed.     

Amperometric quantification of sodium metabisulfite in pharmaceutical formulations utilizing tetraruthenated porphyrin film modified electrodes and batch injection analysis

The performance of a glassy carbon electrode modified with a porphyrin film formed by the [Co(TPyP){Ru(bipy)₂Cl}₄](TFMS)₅·H₂O complex for the analysis of sodium metabisulfite in pharmaceuticals is described. The sensor can be rapidly and easily prepared by drop-casting of a microliter volume of a diluted methanolic solution of the complex onto the electrode surface. The modified electrode with a supramolecular cobalt porphyrin film led to more favorable responses than the bare electrode. This can be ascribed to the much faster electron transfer processes to the analyte mediated by the tetraruthenated porphyrin and to the protection of the electrode against fouling. The association of the amperometric sensor with the batch injection analysis technique led to results that combine good repeatability of the current responses (relative standard deviation of 0.94% for 30 measurements), wide linear dynamic range (2.5 × 10⁻⁷ mol L⁻¹ to 5.0 × 10⁻⁴ mol L⁻¹), high sensitivity and low limits of detection (8.1 × 10⁻⁸ mol L⁻¹) and quantification (2.7 × 10⁻⁷ mol L⁻¹). The system was successfully applied to sodium metabisulfite quantification in commercial samples of injection formulations of sodium (or potassium) diclofenac. The results compared well with those obtained by the polarographic method.     

An optical sensor for the determination of digoxin in serum samples based on a molecularly imprinted polymer membrane

This paper reports the synthesis and testing of a molecularly imprinted polymer membrane for digoxin analysis. Digoxin-specific bulk polymer was obtained by the UV initiated co-polymerisation of methacrylic acid and ethylene glycol dimethacrylate in acetonitrile as porogen. After extracting the template analyte, the ground polymer particles were mixed with plasticizer polyvinyl chloride to form a MIP membrane. A reference polymer membrane was prepared from the same mixture of monomers but with no template. The resultant membrane morphologies were examined by scanning electron microscopy. The imprinted membrane was tested as the recognition element in a digoxin-sensitive fluorescence sensor; sensor response was measured using standard solutions of digoxin at concentrations of up to 4 × 10⁻³ mg L⁻¹. The detection limit was 3.17 × 10⁻⁵ mg L⁻¹. Within- and between-day relative standard deviations RSD (n = 5) were in the range 4.5-5.5% and 5.5-6.5% respectively for 0 and 1 × 10⁻³ mg L⁻¹ digoxin concentrations. A selectivity study showed that compounds of similar structure to digoxin did not significantly interfere with detection for interferent concentrations at 10, 30 and 100 times higher than the digoxin concentration. This simply manufactured MIP membrane showed good recognition characteristics, a high affinity for digoxin, and provided satisfactory results in analyses of this analyte in human serum.     

A green analytical procedure for flow-injection determination of nitrate in natural waters

Nitrate determination in waters is generally carried out with cadmium filings and carcinogenic reagents or by reaction with phenolic compounds in highly concentrated sulfuric acid medium. In this work, it was developed a green analytical procedure for nitrate determination in natural waters based on direct spectrophotometric measurements in ultraviolet, using a flow-injection system with an anion-exchange column for separation of nitrate from interfering species. The proposed method employs only one reagent (HClO₄) in a minimum amount (equivalent to 18 μL concentrated acid per determination), and allowed nitrate determination within 0.50-25.0 mg L⁻¹, without interference of up to 200.0 mg L⁻¹ humic acid; 1.0 mg L⁻¹ NO₂⁻; 200.0 mg L⁻¹ PO₄³⁻; 75.0 mg L⁻¹ Cl⁻; 50.0 mg L⁻¹ SO₄²⁻ and 15.0 mg L⁻¹ Fe³⁺. The detection limit (99.7% confidence level) and the coefficient of variation (n = 20) were estimated as 0.1 mg L⁻¹ and 0.7%, respectively. The results obtained for natural water samples were in agreement with those achieved by the reference method based on nitrate reduction with copperized cadmium at the 95% confidence level.     

Self-assembled monolayer of nickel(II) complex and thiol on gold electrode for the determination of catechin

Self-assembled monolayers of a nickel(II) complex and 3-mercaptopropionic acid on a gold electrode were obtained for determination of catechin by square wave voltammetry. The complex [Ni^IIL] with L = [N-(methyl)-N′-(2-pyridylmethyl)-N,N′-bis(3,5-di-tert-butyl-2-hydroxybenzyl)-1,3-propanediamine[nickel(II)] was synthesized and characterized by ¹H NMR, IR, and electronic spectroscopies and electrochemical methods. The optimized conditions obtained for the electrodes were 0.1 mol L⁻¹ phosphate buffer solution (pH 7.0), frequency of 80.0 Hz, pulse amplitude of 60.0 mV and scan increment of 10.0 mV. Under these optimum conditions, the resultant peak current on square wave voltammograms increases linearly with the concentration of catechin in the range of 3.31 × 10⁻⁶ to 2.53 × 10⁻⁵ mol L⁻¹ with detection limits of 8.26 × 10⁻⁷ mol L⁻¹. The relative standard deviation for a solution containing 1.61 × 10⁻⁵ mol L⁻¹ catechin solution was 2.45% for eight successive assays. The lifetime of the Ni(II) complex-SAM-Au electrode was investigated through testing every day over 4 weeks. The results showed apparent loss of activity after 20 days. The results obtained for catechin in green tea samples using the proposed sensor and those obtained by electrophoresis are in agreement at the 95% confidence level.     

Biparametric potentiometric analytical microsystem for nitrate and potassium monitoring in water recycling processes for manned space missions

The construction and evaluation of a Low Temperature Co-fired Ceramics (LTCC)-based continuous flow potentiometric microanalyzer prototype to simultaneously monitor the presence of two ions (potassium and nitrate) in samples from the water recycling process for future manned space missions is presented. The microsystem integrates microfluidics and the detection system in a single substrate and it is smaller than a credit card. The detection system is based on two ion-selective electrodes (ISEs), which are built using all-solid state nitrate and potassium polymeric membranes, and a screen-printed Ag/AgCl reference electrode. The obtained analytical features after the optimization of the microfluidic design and hydrodynamics are a linear range from 10 to 1000 mg L⁻¹ and from 1.9 to 155 mg L⁻¹ and a detection limit of 9.56 mg L⁻¹ and 0.81 mg L⁻¹ for nitrate and potassium ions respectively.     

Evaluation of alternate lines of Fe for sequential multi-element determination of Cu, Fe, Mn and Zn in soil extracts by high-resolution continuum source flame atomic absorption spectrometry

The usefulness of the secondary line at 252.744 nm and the approach of side pixel registration were evaluated for the development of a method for sequential multi-element determination of Cu, Fe, Mn and Zn in soil extracts by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). The influence of side pixel registration on the sensitivity and linearity was investigated by measuring at wings (248.325, 248.323, 248.321, 248.329, and 248.332 nm) of the main line for Fe at 248.327 nm. For the secondary line at 252.744 nm or side pixel registration at 248.325 nm, main lines for Cu (324.754 nm), Mn (279.482 nm) and Zn (213.875 nm), sample flow-rate of 5.0 mL min⁻¹ and calibration by matrix matching, analytical curves in the 0.2-1.0 mg L⁻¹ Cu, 1.0-20.0 mg L⁻¹ Fe, 0.2-2.0 mg L⁻¹ Mn, 0.1-1.0 mg L⁻¹ Zn ranges were obtained with linear correlations better than 0.998. The proposed method was applied to seven soil samples and two soil reference materials (IAC 277; IAC 280). Results were in agreement at a 95% confidence level (paired t-test) with reference values. Recoveries of analytes added to soil extracts containing 0.15 and 0.30 mg L⁻¹ Cu, 7.0 and 14 mg L⁻¹ Fe, 0.60 and 1.20 mg L⁻¹ Mn, 0.07 and 0.15 mg L⁻¹ Zn, varied within the 94-99, 92-98, 93-101, and 93-103% intervals, respectively. The relative standard deviations (n = 12) were 2.7% (Cu), 1.4% (Fe - 252.744 nm), 5.7% (Fe - 248.325 nm), 3.2% (Mn) and 2.8% (Zn) for an extract containing 0.35 mg L⁻¹ Cu, 14 mg L⁻¹ Fe, 1.1 mg L⁻¹ Mn and 0.12 mg L⁻¹ Zn. Detection limits were 5.4 μg L⁻¹ Cu, 55 μg L⁻¹ Fe (252.744 nm), 147 μg L⁻¹ Fe (248.325 nm), 3.0 μg L⁻¹ Mn and 4.2 μg L⁻¹ Zn.     

Square wave voltammetric determination of nitrofurantoin in pharmaceutical formulations on highly boron-doped diamond electrodes at different boron-doping contents

The influence of the boron-doping levels in boron-doped diamond film electrodes on the electrochemical response of nitrofurantoin (NFT) and the development of an electroanalytical procedure for NFT determination were investigated. The investigations were carried out using the techniques of cyclic voltammetry and square wave voltammetry on diamond film electrodes with different boron-doping levels (i.e., 5000, 10,000 and 20,000 mg L⁻¹). The level of boron-doping in the diamond film electrodes influenced the electrochemical reduction of NFT. The appropriate cyclic voltammetric response of NFT was obtained with Britton-Robinson buffer at pH 4 and for diamond films doped with 10,000 and 20,000 mg L⁻¹ of boron. These two films were selected for the development of the electroanalytical procedure. The use of square wave voltammetry with the optimized parameters demonstrated a good linear relationship between the peak current and the NFT concentration for a wide range of concentration. The lower limit of detection for the electrodes doped with 10,000 and 20,000 mg L⁻¹ of boron were 2.69 × 10⁻⁸ mol L⁻¹ (6.40 μg L⁻¹) and 8.15 × 10⁻⁹ mol L⁻¹ (1.94 μg L⁻¹), respectively, while the lower limits of quantification were 8.96 × 10⁻⁸ mol L⁻¹ (21.33 μg L⁻¹) and 2.72 × 10⁻⁸ mol L⁻¹ (6.47 μg L⁻¹), respectively. The applicability of the proposed procedure was tested using a commercial pharmaceutical formulation of NFT, and the results were compared with the procedure recommended by the British Pharmacopeia. The proposed procedure was sensitive, accurate and precise for analysis of NFT and did not require complex preparations or renovations of the electrode surface. This presents the advantage of eliminating mercury waste and minimizing the adsorptive problems related to the use of other electrodic solid surfaces.