Biamperometric and Differential Pulse Polarographic Methods for the Assay of Nomifensine Maleate

Abstract

Biamperometric titration and differential pulse polarography (DPP) are described for the analysis of nomifensine maleate powder and commercial capsules (Merital^R -50 mg). The biamperometric method involved the titration in cold dil. HCl medium against 0.01 M - NaN0₂ and electrometric detection of end point. The mean percent recoveries obtained were 100.0 ± 0.87 and 99.2 ± 0.95 for the authentic powder and capsules, respectively. The DPP method was performed by measuring the peak current, i_P, obtained from the recorded differential polarogram under constant 50mV modulation amplitude. The peak current was measured at the peak potential of ? 1.02 V on the dropping mercury electrode (DME) versus Ag/AgCl/KCl (sat.) reference electrode at pH 5.0 (acetate buffer). A linear relationship between peak current and concentration was demonstrated in the range 3 to 30μg ml^?1. The mean percent recovery for the capsules was 103.1 ± 1.26.     

High Performance Liquid Chromatographic Determination of Sertraline in Presence of Its Degradation Product

A simple, stability – indicating, reversed phase liquid chromatographic method has been developed for the determination of sertraline in the presence of its oxidative degradation product. Reversed phase chromatography was conducted using a phenyl (250 × 4.6 mm id) stainless steel column at ambient temperature with UV-detection at 226 nm. A mobile phase consisting of potassium dihydrogen phosphate buffer: acetonitrile (50:50, v/v) adjusted to pH 4.5 with phosphoric acid, has been used for the separation of sertraline and its oxidative degradation product at a flow rate of 1 ml/min. The calibration curve was rectilinear over the concentration range of 1–20 μg/ml with a detection limit (LOD) of 0.09 μg/ml, and quantification limit (LOQ) of 0.27 μg/ml. The proposed method was successfully applied for the analysis of sertraline in its tablets, with mean % recoveries of 100.17 ± 0.62 for sertraline in pure form and 100.14 ± 0.68, 100.29 ± .77, and 100.06 ± 0.67 for seserine®, serlift®, and sirto® tablets, respectively. The obtained results were favorably compared with those obtained by a reference method. The drug was exposed to forced alkaline, acidic, hydrolytic, and oxidative degradation according to the ICH Guidelines. Moreover, the method was utilized to investigate the kinetics of the photoinduced oxidative degradation of the drug. The first-order rate constant, half-life time, and activation energy of the degradation reaction were calculated.     

Differential Pulse Polarographic Determination of Orthophosphate in Nonaqueous Media

Abstract

The method is based on the polarographic behavior of 12-tungstophosphoric acid in nonaqueous media at the DME utilizing the differential pulse polarographic technique. In this procedure, orthophosphate is converted to 12-tungstophosphoric acid H₃ PW ₁₂ O ₄₀ by reacting with tungstate under acidic conditions and at 100°C. The H₃ PW ₁₂ O ₄₀ is extracted into 1-pentanol and its polarographic measurement is made in 1-pentanol-ethanoi mixture containing sodium perchlorate as supporting electrolyte. The differential pulse polarogram of H₃ PW ₁₂ O ₄₀ in this solution shows three peaks between 0.00 and -0.90 V vs. Ag/ AgCl. The most cathodic peak at -0.78 V exhibited the highest peak current value and was used for the analytical measurement. A linear calibration graph in the range 0.10 - 5.00 pg/ml P in the final solution was obtained. The method has a relative standard deviation of 0.90% at the 4 pg/ml P level and 1.32% at the 1 μg/ml P level in the final solution. Arsenate, borate and silicate do not interfere.     

The role of Fe(II) in the increased medicinal potency of curcumin analyzed by electrochemical methods

The formation of complexes of curcumin and Fe(II) was studied in aqueous media at pH 5.7 ± 0.1 by polarography, amperometry and spectrophotometry. The polarogram indicated formation of complexes between curcumin and Fe(II). Curcumin produces a well-defined direct current polarogram and differential pulse polarogram in 0.1 M ammonium tartrate (supporting electrolyte) at pH 5.7 ± 0.1. The stoichiometry of the Fe(II)-curcumin complex is 1 : 1. Anticancer studies on the drug and its metal complex have been performed against sarcoma cells (in-vitro), revealing the complex to be more potent in anticancer activity compared to the parent drug.     

Differential Pulse Polarographic Determination of Moxifloxacin Hydrochloride in Pharmaceuticals and Biological Fluids

Abstract

A simple, fast, sensitive and fully validated differential pulse polarographic (DPP) method for the determination of trace amounts of moxifloxacin in pharmaceutics, serum and urine is reported. Moxifloxacin exhibited irreversible cathodic peak over the pH 5.00–11.00 in Britton–Robinson (B–R) buffer. At pH 10.00 (the analytical pH), a well‐defined peak at ?1.61 V versus saturated calomel electrode was obtained. The current has been characterized as being diffusion‐controlled process. The diffusion current constant (i_d) was 1.48±0.12 and the current–concentration plot was rectilinear over the range from 5×10^?7 to 1×10^?4 M with correlation coefficient (n=10) of 0.995.

The proposed method was applied to commercial tablets and average percentage recovery was in agreement with that obtained by spectrophotometric comparison method. The method was extended to the in vitro determination of moxifloxacin in spiked human serum and urine.     

New Labdane diterpenes from Hedychium yunnanense with cytotoxicity and inhibitory effects on nitric oxide production

Two new labdane diterpenes, hedychenoids A (1) and B (2), were isolated from the rhizomes of Hedychium yunnanense, together with four known ones hedychenone (3), forrestin A (4), villosin (5) and calcaratarin C (6). Their structures were determined on the basis of NMR (1D and 2D) and mass spectroscopic analysis. Compounds 2, 3 and 5 exhibited cytotoxicity against SGC-7901 with IC₅₀ values of 14.88 ± 0.52, 7.08 ± 0.21 and 7.76 ± 0.21 μg/ml, 3 and 5 against HeLa with IC₅₀ values of 9.76 ± 0.48 and 13.24 ± 0.63 μg/ml, respectively. Compounds 2, 5 showed inhibitory effects against nitric oxide production in LPS and IFN-γ-induced RAW 264.7 murine macrophages with IC₅₀ values of 6.57 ± 0.88 and 5.99 ± 1.20 μg/ml, respectively.     

Trace Analysis of Iron in Environmental Water and Snow Samples from Poland

Abstract

A voltammetric method for the determination of iron at detection limit of 4 μg/l is described, using the catalytic current of the reduction of the Fe(III)-triethanolamine (TEA) complex in the presence of bromate ions. the determination was performed at a mercury hanging drop electrode without preconcentration, using the TEA alkaline solution as a supporting electrolyte and the differential pulse technique. A peak current for the Fe(III)-TEA catalytic reduction was observed at a potential of-1.0 V (Ag/AgCl saturated electrode). the influence of TEA, BrO³ and NaOH concentrations on the peak height was studied. It was found that a 100-fold excess of Mn, a 50-fold excess of Cr(VI) and Zn did not interfere in the determination. This method was applied to the determination of iron in water, snow and waste water samples.     

Spectrophotometric Determination of Acebutolol Hydrochloride and Nicoumalone with Metol and Potassium Permanganate

Abstract

A spectrophotometric method is described for the determination of Nicoumalone and Acebutolol hydrochloride based on the formation of molecular complex with the reduction product of Nicoumalone or hydrolysis product of Acebutolol hydrochloride and p-N-methyl benzoguinone monoimine [formed in situ from met01 (p-N-methylaminophenol sulfate) and potassium permanganate, PMBQMI] at pH 3.3. Quantitative measurements were made at the maximum absorption of 525 nm. Beer's law is obeyed in the range of 5–50 μg ml^?1 and 5–60 μg ml^?1 for Nicoumalone and Acebutolol hydrochloride respectively. The proposed method is comparable with the reference method when applied to pharmaceutical preparations, and tablets, An average percentage recovery of 99.5 ± 0.8 was obtained.     

Development of a New Voltammetric Methodology for the Determination of Ciprofloxacin in Beef Samples Using a Carbon Paste Electrode Modified with Nafion and Fullerenes

A sensitive, selective, and low cost electrochemical new methodology was developed for the quantification of ciprofloxacin (Cip) in beef samples by cyclic voltammetry and differential pulse voltammetry, using a CPE electrode modified with Nafion and Fullerenes (N−F/CPE). The optimum parameters for the composition of the N−F/CPE electrode are 0.19 g mineral oil, 0.01 g Nafion, 50 μL fullerene, and graphite powder 0.3 g. The electrochemical characterization was carried out by obtaining maximum anodic peak current associated with the oxidation of ciprofloxacin at 1.1 V, where the electrochemical process resulted to be irreversible and diffusion-controlled. The analytical characterization of the proposed methodology was carried out resulting in a LOD of 1.0 μmol L⁻¹, a LOQ of 3.0 μmol L⁻¹, a sensitivity of 0.37±0.006 μA/μmolL⁻¹, and repeatability of 5.38 %.     

牡丹皮中丹皮酚的二阶导数差示脉冲极谱法定量研究

建立了中草药牡丹皮中丹皮酚的二阶导数差示脉冲极谱定量分析方法。丹皮酚在１ｍｍｏｌ／Ｌ－１ｍｍｏｌ／Ｌ氯化钾－水（１：１：２３）的溶液中,于－１．６．３０Ｖ（ｓ ａｇ／ＡｇＣｌ）处出现一良好的二阶导数差示脉冲极谱峰,其峰幅值与丹皮酚在０．１～０．６ｍｍｏｌ／Ｌ范围内呈非常显著的线性关系（Ｐ〈０．０１）,检测限为９．２ｍｍｏｌ／Ｌ。本法简便、快速、灵敏,且结果准确。     

Determination of Pseudoephedrine Hydrochloride in Some Pharmaceutical Drugs by Potentiometric Membrane Sensor Based on Pseudoephedrine–Phosphotungstate Ion Pair

Abstract

An ion-selective electrode (ISE) was developed for the rapid determination of pseudoephedrine hydrochloride (PSEHCl) in pharmaceutical preparations. The electrode incorporates a PVC membrane with a pseudoephedrine–phosphotungstate ion pair complex. The influences of membrane composition, temperature, pH of the test solution, and the interfering ions on the electrode performance were investigated. The sensor exhibits a Nernstian response for pseudoephedrine hydrochloride ions over a relatively wide concentration range (1.0 × 10^?1 to 1.0 × 10^?5 mol L^?1) with a slope of 56.2 ± 0.5 mV per decade at 25°C. It can be used in the pH range 4.0–10.5. The isothermal temperature coefficient of this electrode amounted to 0.0009 V/°C. The membrane sensor was successfully applied to determination of PSEHCl in its tablets and syrup.     

Simultaneous voltammetric determination of uric acid and ascorbic acid using carbon paste/cobalt Schiff base composite electrode

Differential pulse and cyclic voltammetry were applied for the oxidation of mixture of uric acid and ascorbic acid at the surface of carbon paste/cobalt Schiff base composite electrode. The electrooxidation of these compounds at bare electrode is sluggish, and there is no suitable peak separation between them. However, using cobalt methyl salophen as modifier, two well-defined anodic waves with a considerable enhancement in the peak current and a remarkable peak potential separation near 315 mV are obtained. It can improve the kinetics of electron transfer for both compounds remarkably. All these improvements are created because of the electrocatalytic property of cobalt Schiff base complex. The effect of some parameters such as pH and scan rates were studied. All the anodic peak currents for the oxidation of ascorbic acid and uric acid shifted toward more negative potential with an increase in pH, revealing that protons have taken part in their electrode reaction processes. The best peak separation with appropriate current was obtained for pH 4.0. A linear range of 5.0?×?10^?4 to 1.0?×?10^?8 and 1.0?×?10^?3 to 1.0?×?10^?8 M with detection limit of 8.0?×?10^?9 and 8.0?×?10^?9 M was obtained for ascorbic acid and uric acid using differential pulse voltammetry at the surface of modified electrode, respectively. Analytical utility of the modified electrode has been examined successfully using human urine samples and vitamin C commercial tablets.     

A highly sensitive method for determination of paracetamol by adsorptive stripping voltammetry using a carbon paste electrode modified with nanogold and glutamic acid

A reliable and simple sensor was fabricated by modifying a carbon paste electrode with nanosized gold particles and poly (glutamic acid) for determination of paracetamol (PAR). The modified electrode exhibited an effective catalytic response to the oxidation and reduction of PAR with good reproducibility and stability. The determination was carried out by differential pulse adsorptive stripping voltammetry after a 30 s accumulation time with an open circuit potential and under stirring. The calibration curve is linear in the range from 0.05 to 70 μM of PAR (with a correlation coefficient of 0.9990), and the sensitivity is 1.51 μA·μM^-1. The modified electrode was used to detect PAR in commercial tablets.     

Polarity guided extraction,HPLC based phytochemical quantification,and multimode biological evaluation of Otostegia limbata (Benth.) Boiss

Purpose of studyOtostegia limbata (Benth.) Boiss. (Family: Lamiacae) is an important underexplored ethnomedicinal plant that has been used as antinflammatory, anticancer and antibacterial herbal remedy previously. The present work was aimed to evaluate the antioxidant, antimicrobial, antileishmanial, and anticancer prospective of O. limbata stem and leaf extracts.ResultsThe highest amount of phenolic and flavonoid content was obtained in the methanol-acetone and methanol stem extracts i.e., 53.29 ± 1.33 and 28.64 ± 1.16, respectively with highest DPPH scavenging in MeH stem extract (IC₅₀ = 34.5 ± 1.34 μg/ml). Significant amount of catechin, gallic acid, apigenin and rutin was quantified. A moderate antibacterial and substantial antifungal activity was observed. Cytotoxicity against brine shrimps categorized 21% of stem (3 out of 14 extracts) and 57% (8 out of 14 extracts) of leaf extracts as potent. Substantial cytotoxicity against THP-1 cell line (IC₅₀ = 3.46 ± 0.25 μg/ml) and Leishmania (IC₅₀ = 1.50 ± 0.23 μg/ml) was exhibited by methanol-distilled water leaf extract while noteworthy antiproliferative activity against Hep-G2 (IC₅₀ = 0.44 ± 0.45 μg/ml) was manifested by n-hexane stem extract. Absence of hemolysis in normal RBCs signified plant’s selective cytotoxicity. Methanol-distilled water and chloroform stem extracts displayed prominent protein kinase inhibition and antidiabetic potential of plant.ConclusionThe results of present study recommend O. limbata as a potential source of antifungal, antileishmanial, anticancer, and α-amylase inhibitory agents.     

A Simple and Rapid CZE Determination of Tiapride Hydrochloride and Related Impurities in Pharmaceutical Formulations

A simple, fast, inexpensive capillary zone electrophoresis method for the separation and determination of tiapride hydrochloride and its two related impurities in pharmaceutical formulations has been developed and validated. The successful separation of these compounds was achieved in less than 3 min using a fused silica capillary and photodiode array detector at 218 nm. The best conditions were obtained using a 10 mM sodium tetraborate (pH 8.0) as the running buffer. The linear responses covered the ranges from 1.0 to 100 μg mL^?1 (R = 0.9989) for tiapride hydrochloride. The detection (LOD) and quantitation limits (LOQ) for tiapride hydrochloride were 2.7 and 9.0 μg mL^?1, respectively. The intra- and inter-day relative standard deviations for migration times and peak areas were less than 0.47 and 5.7%, respectively. The method was validated for the determination of tiapride hydrochloride in commercial tablets.     

Highly selective determination of ascorbic acid,epinephrine, and uric acid by differential pulse voltammetry using poly(Adizol Black B)-modified glassy carbon electrode

A polymerized film of Adizol Black B (ABB) on the surface of glassy carbon (GC) electrode was prepared for the simultaneous determination of ascorbic acid (AA), epinephrine (EP), and uric acid (UA). This new electrode presented an excellent electrocatalytic activity towards the oxidation of AA, EP, and UA by differential pulse voltammetry method. The oxidation peaks of the three compounds were well defined and had the enhanced peak currents. The separation of the oxidation peak potentials for AA–EP and EP–UA were about 180 and 130 mV, respectively. The calibration curves obtained for AA, EP, and UA were in the ranges of 2.0–1,970.0, 0.1–64.0, and 0.1–1,700.0 μmol L^–1, respectively. The detection limits (S/N?=?3) were 0.01, 0.007, and 0.02 μmol L^–1 for AA, EP, and UA, respectively. The diffusion coefficient and the catalytic rate constant for the oxidation reaction of EP at poly(ABB) film-coated GC electrode were calculated as 1.54(±0.10)?×?10^?4 cm² s^?1 and 4.5?×?10³ mol^?1 L s^?1, respectively. The present method was applied to the determination of EP in pharmaceutical, AA in commercially available vitamin C tablet, and UA in urine samples.     

聚酸性铬蓝K修饰电极测定对乙酰氨基酚

研究对乙酰氨基酚(ACOP)在聚酸性铬蓝K(PACBK)修饰石墨电极上的电化学行为,并利用该电极建立测定对乙酰氨基酚的电化学方法。采用循环伏安法制备了聚酸性铬蓝修饰石墨电极,利用脉冲伏安法对对乙酰氨基酚的含量进行测定。对乙酰氨基酚的浓度在0.8~100μmol/L范围与脉冲峰电流呈现良好的线性关系(r~2=0.998 2),检出限为0.1μmol/L(S/N=3),实际样品的平均加标回收率为96.5%~101.7%,测定结果的相对标准偏差为1.2%(n=6)。该方法可用于药物对乙酰氨基酚片的质量控制。     

Microcystin-(Leucine-Arginine) Immunosensor Based on Iron(II,III) Magnetic Nanoparticles

An electrochemical immunosensor for microcystin-(leucine-arginine) based on magnetic bionanoparticles and iron(II, III) oxide was developed. The bionanoparticles were prepared by cross-linking antibodies of microcystin-(leucine-arginine) and amino-functionalized magnetic iron(II, III) oxide nanoparticles with glutaraldehyde, followed by immobilization on the surface of a magnetic electrode. The immunosensor was based on the model of direct competition, as microcystin-(leucine-arginine) and horseradish peroxidase-conjugated microcystin-(leucine-arginine) competitively combined with immobilizing antibodies. The peak current of differential pulse voltammetry (DPV) decreased with an increase of microcystin-(leucine-arginine) concentration after antigen-antibody reaction. When the background current was stabilized, the anodic peak current response and change in peak response were recorded. Under the optimized conditions, the change in response was proportional to the microcystin-(leucine-arginine) concentration between 0.010 and 100 µg/L with a limit of detection equal to 0.009 µg/L. Amperometry was adopted to determine microcystin-(leucine-arginine); the linear dynamic range was 0.10 to 100 µg/L with a detection limit of 0.08 µg/L. The method was successfully applied in the determination of microcystin-(leucine-arginine) in river water and the recoveries were between 90.2% and 110.5%.     

Reversed-Phase High Performance Liquid Chromatographic and Thin Layer Chromatographic Methods for the Simultaneous Determination of Benazepril Hydrochloride and Hydrochlorothiazide in Cibadrex Tablets

ABSTRACT

Two procedures were developed for simultaneous determination of benazepril hydrochloride (I) and hydrochlorothiazide (II) in pure, laboratory made mixtures and in pharmaceutical dosage form “Cibadrex tablets® using reversed phase high performance liquid chromatographic and thin layer chromatographic methods.

For reversed phase HPLC, a new very sensitive, rapid, selective method was developed. The linearity ranges were 32-448 ng/20 μl and 40-560 ng/20 μl for benazepril hydrochloride and hydrochlorothiazide, respectively. The corresponding recoveries were 99.38 ± 1.526 and 99.2 ± 1.123.

The minimum detection limits were 7 ng/20 μl and 14 ng/20 μl for benazepril hydrochloride and hydrochlorothiazide respectively.

On the other hand, a new, simple, sensitive and fast thin layer chromatographic scanning densitometric method was developed for simultaneous determination of benazepril hydrochloride and hydrochlorothiazide using ethyl acetate: methanol: ammonia (85: 20: 10 v/v) as the developing system. The R_f values were 0.33 & 0.68 for benazepril hydrochloride and hydrochlorothiazide respectively. The minimum detection limit obtained was 0.12 μg/spot for benazepril hydrochloride and 0.24 μg/spot for hydrochlorothiazide. The mean percentage recoveries were 100.04 ± 1.102 and 99.31 ± 1.009 for benazepril hydrochloride and hydrochlorothiazide respectively.

The two proposed methods were simple, precise, sensitive and could be successfully applied for the determination of pure, laboratory made mixtures and pharmaceutical dosage forms. The results obtained were compared with those obtained by A ^1%.     

Electrochemical Oxidation of Phenothiazine Derivatives at Glassy Carbon Electrodes and Their Differential Pulse and Square‐wave Voltammetric Determination in Pharmaceuticals

Abstract

Three 2,10‐disubstituted phenothiazines—chlorpromazine hydrochloride (CPM), thioridazine hydrochloride (TR) and propericiazine (PRC)—were electrochemically studied in various buffer systems at different pH values, using a glassy carbon electrode. The substances were electrochemically oxidized at potential range 0.55–0.75 V. The oxidation was reversible and exhibited diffusion‐controlled process. The mechanism of the oxidation process is discussed. According to the linear relation between peak current and concentration, differential pulse voltammetry (DPV) and square wave voltammetry (SWV) methods for quantitative determination of chlorpromazine and propericiazine in 0.1 M HClO₄, and thioridazine in pH 2 phosphate buffer, was applied. Both the repeatability and reproducibility of the methods were also determined for all studied substances. The developed procedures were successfully applied to the determination of chlorpromazine and thioridazine in pharmaceutical dosage forms.