A New Flow‐Injection Chemiluminescence Method for the Determination of Acyclovir and Gancyclovir

Abstract

A rapid and sensitive flow‐injection chemiluminescence (FI‐CL) method, which is based on the CL intensity that generated from the redox reaction of Ce(IV)‐rhodamine B in H₂SO₄ medium, for the determination of acyclovir and gancyclovir is described. For acyclovir, the determination range is 3×10^?8 g mL^?1–7×10^?5 g mL^?1, with 1.56×10^?8 g mL^?1 as its determination limit. During 11 repeated measurements for 1×10^?6 g mL^?1 acyclovir, the relative standard deviation was 2.08%. For gancyclovir, the determination range was 5×10^?8 g mL^?1–7×10^?5 g mL^?1, with 2.35×10^?8 g mL^?1 as its determination limit. The relative standard deviation is 2.83% with 11 repeated measurements of 1×10^?6 g mL^?1 gancyclovir. This method can be successfully used to determine the content of acyclovir and gancyclovir in injections, acyclovir in eye drops, and, maybe, also for other ciclovirs.     

Simultaneous determination of fifteen multiclass organic pollutants in human saliva and serum by liquid chromatography–tandem ultraviolet/fluorescence detection: A validated method

A quick and inexpensive validated method, based on sample treatment by liquid–liquid microextraction followed by liquid chromatography (LC) coupled with ultraviolet tandem fluorescence detection is proposed for the determination of 15 multiclass pollutants both in serum and in saliva, as a simple and easy to draw matrix. The method was set up and validated according to European guidelines. The compounds of interest include some endocrine‐disrupting chemicals (i.e. bisphenol A, bisphenol B, bisphenol E, bisphenol F, bisphenol AF, bisphenol A diglycidyl ether, bisphenol M, diethylhexyl phthalate, monoethylhexyl phthalate, triclosan and 4‐nonylphenol), as well as other pollutants belonging to the class of volatile organic compounds (2‐chlorophenol, 1,2 dichlorobenzene, 1,2,4,5‐tetrachlorobenzene). The limits of quantifications ranged from 2.28 × 10^?3 μg mL^?1 (bisphenol A diglycidyl ether) to 6.29 μg mL^?1 (diethylhexyl phthalate), while those of detection ranged from 0.068 × 10^?3 μg mL^?1 (bisphenol A diglycidyl ether) to 1.031 μg mL^?1 (diethylhexyl phthalate). To test method suitability, it was applied to real saliva and serum samples of healthy human volunteers and was found to meet the demands of the laboratories handling simple and relatively inexpensive equipment for screening oriented at rapid and reliable contamination assessment of a population.     

The Determination of Perphenazine by a New Simple Flow‐Injection Chemiluminescence Method

Abstract

A rapid and simple flow‐injection chemiluminescence (CL) method is described for the determination of perphenazine, which is based on the CL intensity that generated from the redox reaction of Ce (IV)-perphenazine in HNO₃ medium is proportional to the perphenazine concentration without any sensitizers. The proposed method allows the determination range within 1.0×10^?7–7.0 ×10^?5 g mL^?1 with a detection limit of 8.0×10^?8 g mL^?1, and it has been successfully applied to the determination of the perphenazine in pharmaceutical tablet compared well with the official method.     

Subnanomolar Determination of Indium by Adsorptive Stripping Differential Pulse Voltammetry Using Factorial Design for Optimization

Abstract

A highly sensitive method to determine of indium is proposed by adsorption stripping differential pulse cathodic voltammetry (AdSDPCV) method. The complex of indium ions with xylenol orange is analyzed based on the adsorption collection onto a hanging mercury drop electrode (HMDE). After accumulation of the complex at ?0.20 V vs. Ag/AgCl reference electrode, the potential is scanned in a negative direction from ?0.40 to ?0.75 V with the differential pulse method. Then, the reduction peak current of In(III)–XO complex is measured. The influence of chemical and instrumental variables was studied by factorial design analysis. Under optimum conditions and accumulation time of 60 s, linear dynamic range was 0.1–10 ng/ml (8.7 × 10^?10 to 8.7 × 10^?8 M) with a limit of detection of 0.03 ng/ml (2.6 × 10^?10 M); at accumulation time of 5 min, linear dynamic range was 0.04–10 ng/ml (3.4 × 10^?10 to 8.7 × 10^?8 M) with a limit of detection of 0.013 ng/ml (1.1 × 10^?10 M). The applicability of the method to analysis of real samples was assessed by the determination of indium in water, alloy, and jarosite (zinc ore) samples.     

Rapid Flow-Injection Method for the Determination of Colistin by Sensitized Chemiluminescence Using the Acidic Permanganate–Sulfite System

Abstract

A simple, rapid, and sensitive chemiluminescence method for the determination of colistin (Polymyxin E), a cyclic polypeptide with antibiotic effect produced by certain strains of Bacillus polymyxa, has been developed by combining a flow-injection technique and the bacteria's sensitizing effect on the chemiluminescence reaction between sulfite and acidic permanganate. The optimum conditions for chemiluminescence emission were established. The chemiluminescence was proportional to the log of concentration of colistin over the range 4–100 µg mL^?1 (3.5–87 µM). The detection limit was 1.2 µg mL^?1 (1.0 µM) of colistin. The method has been satisfactorily used for the determination of colistin in pharmaceuticals.     

Catalytic Square-Wave Voltammetric Determination of Acrylamide in Potato Chips

Abstract

Square-wave voltammetry is a fast technique used for determination of trace amounts of acrylamide. When cobalt(II) ions were added to the acrylamide solution, a catalytic peak at about ?1.35 V vs. Ag/AgCl was observed, which was proportional to acrylamide concentration. The calibration curve showed good linearity in the range of 200–800 ng mL^?1 of acrylamide with a regression coefficient of 0.9989. The limit of detection of the method was 3.52 ng mL^?1, and the relative standard deviations for concentrations of 300 ng mL^?1 and 700 ng mL^?1 were 99.8% × 10^?2 and 79.7% × 10^?2, respectively.     

A Validated Voltammetric Procedure for Quantification of the Antifungal Drug Griseofulvin in Bulk Form,Tablets, and Biological Fluids at a Mercury Electrode

Abstract

Griseofulvin is an antifungal antibiotic used to treat various pathogenic mycotic diseases. The voltammetric behavior of griseofulvin at a hanging mercury drop electrode in Britton‐Robinson buffers of pH 2–11.5 was studied and discussed. A fully validated sensitive square‐wave adsorptive cathodic stripping voltammetric procedure was described for direct determination of bulk griseofulvin substance. The procedure was based on the reduction of the >C?O double bond of griseofulvin molecule following its preconcentration onto a hanging mercury drop electrode in a Britton‐Robinson buffer of pH 10. Limits of detection (LOD) and quantitation (LOQ) of 5.8×10^?10 M and 1.93×10^?9 M bulk griseofulvin were achieved, respectively. The proposed stripping voltammetric procedure was successfully applied to assay griseofulvin in tablets and in spiked human serum and urine samples. LOD of 8.65×10^?10 M and 6.6×10^?9 M and LOQ of 2.88×10^?9 M and 2.2×10^?8 M griseofulvin in spiked human serum and urine samples, respectively, were achieved.     

Determination of Cd(II) in Some Foodstuffs by Anodic Stripping Pulse Voltammetry (ASPV) using Glassy Carbon Electrode

Abstract

Cadmium in the presence of 0.04 M NaCl as the electrolyte was determined using stripping voltammetry with superimposed constant amplitude pulses of negative polarity (SVPNP) or positive polarity (SVPPP), and differential pulses stripping voltammetry using rotating disc glass carbon electrode (RDGCE). The SVPNP was found to give the greatest sensitivity. The anodic peak was obtained at potential ?850 to ?795 mV due to the oxidation of cadmium to cadmium(II). Linear calibration curves were obtained in the concentration range between 1.5×10^?9–2×10^?10 M. The relative standard deviation is 4.25% at very low concentration of 2×10^?10 M. This method was successfully applied to the determination of cadmium in some foodstuffs (wheat and its products, vegetables) after acid digestion.     

First Electroanalytical Methodology for the Determination of Hordenine in Dietary Supplements using a Boron‐doped Diamond Electrode

The present work describes the first electrochemical investigation and a simple, rapid and modification‐free electroanalytical methodology for quantification of hordenine (a potent phenylethylamine alkaloid) using a boron‐doped diamond electrode. At optimized square‐wave voltammetric parameters, the observed oxidation peak current in 0.1 M HClO₄ at +1.33 V (vs. Ag/AgCl) increased linearly from 5.0 to 100 μg mL^?1 (3.0×10^?5–6.1×10^?4 M), with detection limit of 1.3 μg mL^?1 (7.8×10^?6 M). The applicability of the developed method was tested with the determination of hordenine in the commercial dietary supplement formulations.     

Electrochemical Enzyme‐Linked Immunoassay for the Determination of Estriol Using Methyl Red as Substrate

Abstract

A new electrochemical substrate for horseradish peroxidase, methyl red, is reported. In this reaction system, horseradish peroxidase can catalyze the redox reaction of methyl red and H₂O₂. Methyl red exhibits a sensitive voltammetric peak at?0.51 V vs. Ag/AgCl reference electrode, the decrease of the peak current of methyl red is in proportion to the concentration of horseradish peroxidase (HRP). The linear range for determination of horseradish peroxidase is 5.0×10^?8～5.0×10^?7 g mL^?1 and the detection limit is 1.8×10^?8 g mL^?1. The relative standard deviation is 3.3% when 2.0×10^?7 g mL^?1 HRP was sequentially determined 11 times. A voltammetric enzyme‐linked immunoassay method for the determination of estriol was developed, based on this electrochemical system. The linear range for determination of estriol is 1.0～1000.0 ng mL^?1, and the detection limit is 0.33 ng mL^?1. The relative standard deviation for 11 parallel determinations with 200 ng mL^?1 estriol is 4.8%. Some pregnancy serum samples were analyzed with satisfactory results.     

Adsorptive Cathodic Stripping Voltammetry Determination of Ultra Trace of Lead in Different Real Samples

Abstract

In the present work, an adsorptive cathodic stripping voltammetric method using a hanging mercury drop electrode (HMDE) was described in order to determine the ultra trace of lead ions with carbidopa in different real samples. The method is based on accumulation of lead metal ion on mercury electrode using carbidopa as a suitable complexing agent. The potential was scanned to the negative direction and the differential pulse stripping voltammograms were recorded. The instrumental and chemical parameters were optimized. The optimized conditions were obtained in pH of 8.4, carbidopa amount of 1.0×10^?6 M, accumulation potential of 0. 0 V, accumulation time of 100 s, scan rate of 100 mV/s and pulse height of 50 mV. The relationship between the peak current versus concentration was linear over the range of 2.4×10^?10–4.8×10^?7 M. The limits of detection were 5.8×10^?11 M and the relative standard deviation at 4.8×10^?10, 2.1×10^?8, and 2.4×10^?7 M of lead ion were obtained 3.2, 2.9, and 2.7%, respectively (n=7).     

Voltammetric Determination of L‐Dopa Using a Carbon Nanotubes‐Nafion Modified Glassy Carbon Electrode

Abstract

A method for determination of L‐dopa by the adsorption stripping voltammetry (ASV) using a multiwalled carbon nanotubes (MWNTs)–Nafion modified glassy carbon electrode (GMGCE) was proposed. This chemically modified electrode (CME) shows a better stability. A sensitive oxidation peak was observed and the anodic peak potential is ca. 0.374V (vs. SCE). The influences of various experimental parameters on the current peak were completely studied. Under the optimized condition, the method has been applied to the determination of L‐dopa in samples. There is a good linear relationship between the peak current (i_p) and L‐dopa concentration in the range of 3.5×10^?7～1.5×10^?5 mol/L, with the limit of detection 5.0×10^?8 mol/L.     

Determination of Cysteine in the Presence of Copper in Diluted Alkaline Electrolyte by Adsorptive Stripping Voltammetry at the Mercury Film Electrode

Abstract

A stripping method for the determination of cysteine in the presence of copper at the submicromolar concentration levels is described. The method is based on controlled adsorptive accumulation of cysteine at mercury film electrode followed by linear cyclic voltammetry scan measurement of the surface species. Optimum experimental conditions were found to be the use of a 1×10^?3 M NaOH solution, an accumulation potential of ?0.50 V and a scan rate of 200 mV. s^?1. The response of cysteine is linear over the concentration range 0.04–0.20 ppm. For an accumulation time of 15 minutes, the detection limit was found to be 0.9 ppb (7.4×10^?9 M). The more convenient relation to measuring the cysteine in presence of metals, and others amino acids were also investigated. The utility of the method is demonstrated by presence of casein and ATP.     

Nonextractive Trace Level Simultaneous Determination of Mercury(II) and Zinc(II) in Environmental Samples with 2‐(5‐Bromo‐2‐pyridylazo)‐5‐diethylaminophenol and Cetylpyridinium Chloride

Abstract

A simple, rapid, selective, and sensitive method for the derivative spectrophotometric determination of Hg(II) and its simultaneous determination in the presence of Zn(II) using 2‐(5‐bromo‐2‐pyridylazo)‐5‐diethylaminophenol in the presence of cetylpyridinium chloride, a cationic surfactant, has been developed. The molar absorption coefficient and analytical sensitivity of the 1∶1 Hg(II) complex at 558 nm (λ_max) are 5.78×10⁴ L mol^?1 cm^?1 and 0.67 ng mL^?1, respectively. The detection limit of Hg(II) is 1.40×10^?2 ng mL^?1, and Beer's law is valid in the concentration range 0.05–2.40 µg mL^?1. Overlapping spectral profiles of Hg(II) and Zn(II) complexes in zero‐order mode interfere in their simultaneous determination. However, 0.10–2.00 µg mL^?1 of Hg(II) and 0.065–0.650 µg mL^?1 of Zn(II), when present together, can be simultaneously determined at zero cross point of the derivative spectrum, without any prior separation. The relative standard deviation for six replicate measurements of solutions containing 0.134 µg mL^?1 of Hg(II) and 0.620 µg mL^?1 of Zn(II) is 1.72 and 1.47%, respectively. The proposed method has successfully been evaluated for trace level simultaneous determination of Hg(II) and Zn(II) in environmental samples.     

Sensitive voltammetric assay of etoposide using modified glassy carbon electrode with a dispersion of multi-walled carbon nanotube

A sensitive electroanalytical method for the determination of anticancer drug etoposide (ETP) using adsorptive stripping differential pulse voltammetry (AdSDPV) at a multi-walled carbon nanotube-modified glassy carbon electrode (MWCNT-modified GCE) is presented. The surface morphology of modified electrode was characterized by scanning electron microscopy. The effects of accumulation time and potential, pH, scan rate, and amount of MWCNT suspension were investigated. The calibration curve was linear in the concentration range of 2.0?×?10^?8–2.0?×?10^?6 M with the detection limit of 5.4?×?10^?9 M. The reproducibility of the peak current was found at 1.55 % (n?=?5) RSD value in pH 6.0 Britton–Robinson buffer for the MWCNT-modified GCE. The method was then successfully utilized for the determination of ETP in pharmaceutical dosage form, and a recovery of 99.55 % was obtained. The possible oxidation mechanism of ETP was also discussed. The proposed electroanalytical method using MWCNT-modified GCE is the most sensitive method for the determination of ETP with lowest limit of detection in the previously published electrochemical methods.     

Ultratrace Xanthine Determination in Diluted Alkaline Electrolyte by Adsorptive Stripping Voltammetry at the Mercury Film Electrode

Abstract

A stripping method for the determination of xanthine at the submicromolar concentration level is described. The method is based on controlled adsorptive accumulation of xanthine at a thin-film mercury electrode followed by a linear scan voltammetry measurement of the surface species. Optimum experimental conditions were found to be the use of a 5.0 × 10^?3 M NaOH solution, an accumulation potential of 0.00 V, and a scan rate of 20 mV s^?1. The response of xanthine is linear over the concentration range 20–140 ppb. For an accumulation time of 30 min, the detection limit was found to be 36 ppt (2.3 × 10^?10 M). The more convenient relations for measuring xanthine in the presence of the metals, hypoxanthine, amino acids, and other nitrogenated bases were also investigated. The utility of the method is demonstrated by the presence of xanthine in adenosine-5′-triphosphate or DNA.     

Histidine Determination in the Presence of Copper in Diluted Alkaline Electrolyte by Adsorptive Stripping Voltammetry at the Mercury Film Electrode

Abstract

A stripping method for the determination of histidine at the submicromolar concentration levels is described. The method is based on controlled adsorptive accumulation of histidine-copper complex at mercury film electrode followed by linear cyclic scan voltammetry measurement of the surface species. Optimum experimental conditions were found to be the use of a 1.0 × 10^?3 M NaOH solution, an accumulation potential of ? 0.20 V, and a linear scan rate of 200 mV sec^?1. The response of histidine is linear over the concentration range 0.02–0.12 ppm. For an accumulation time of 20 min, the detection limit was found to be 0.5 ppb (3.2 × 10^?9 M). The more convenient relation to measuring the histidine in the presence of metals, cysteine, tyrosine, and other amino acids was also investigated. The utility of the method is demonstrated by presence of casein, ATP, and ss DNA.     

Simultaneous Square‐Wave Voltammetric Determination of Paracetamol,Caffeine and Orphenadrine in Pharmaceutical Formulations Using a Cathodically Pretreated Boron‐Doped Diamond Electrode

An electroanalytical method for the simultaneous determination of paracetamol (PAR), caffeine (CAF), and orphenadrine (ORPH) using the square‐wave voltammetry (SWV) and a cathodically pretreated boron‐doped diamond electrode was developed. The method exhibits linear responses to PAR, CAF, and ORPH in the concentration ranges 5.4×10^?7–6.1×10^?5 M, 7.8×10^?7–3.5×10^?5 M, and 7.8×10^?7–3.5×10^?5 M, respectively, with detection limits of 2.3×10^?7 M, 9.6×10^?8 M, and 8.4×10^?8 M, respectively. The proposed method was successfully applied in the simultaneous determination of these analytes in pharmaceutical formulations.     

Removal, preconcentration and spectrophotometric determination of U(VI) from water samples using modified maghemite nanoparticles

Arsenazo III modified maghemite nanoparticles (A-MMNPs) was used for removing and preconcentration of U(VI) from aqueous samples. The effects of contact time, amount of adsorbent, pH and competitive ions was investigated. The experimental results were fitted to the Langmuir adsorption model in the studied concentration range of uranium (1.0 × 10^?4–1.0 × 10^?2 mol L^?1). According to the results obtained by Langmuir equation, the maximum adsorption capacity for the adsorption of U(VI) on A-MMNPs was 285 mg g^?1 at pH 7. The adsorbed uranium on the A-MMNPs was then desorbed by 0.5 mol L^?1 NaOH solution and determined spectrophotometrically. A preconcentration factor of 400 was achieved in this method. The calibration graph was linear in the range 0.04–2.4 ng mL^?1 (1.0 × 10^?10–1.0 × 10^?8 mol L^?1) of U(VI) with a correlation coefficient of 0.997. The detection limit of the method for determination of U(VI) was 0.01 ng mL^?1 and the relative standard deviation (R.S.D.) for the determination of 1.43 and 2.38 ng mL^?1 of U(VI) was 3.62% and 1.17% (n = 5), respectively. The method was applied to the determination of U(VI) in water samples.     

Electrocatalytic determination of propranolol hydrochloride at carbon paste electrode based on multiwalled carbon-nanotubes and γ-cyclodextrin

A carbon paste electrode based on γ-cyclodextrin–carbon nanotube composite (γ-CD–CNT–CME) was developed for the determination of propranolol hydrochloride (PRO). The electrochemical behaviour of PRO was investigated employing cyclic voltammetry, electrochemical impedance spectroscopy and differential pulse adsorptive stripping voltammetry (DPAdSV). Surface morphology of the electrode has been studied by means of scanning electron microscopy. The results revealed that the oxidation of PRO is facilitated at γ-CD–CNT–CME. Under the optimized conditions in Britton–Robinson buffer pH 1.5, the peak currents were found to vary linearly with their concentrations in the range of 1.42 × 10^?7 to 4.76 × 10^?5 M. A detection limit (S/N = 3) of 4.01 × 10^?8 M was obtained for PRO by means of DPAdSV. The proposed method was employed for the determination of PRO in pharmaceutical formulations, urine and blood serum samples.