Determination Of Niclosamide Research Articles

Optimization of vortex-assisted hydrophobic magnetic deep eutectic solvent-based dispersive liquid phase microextraction for quantification of niclosamide in real samples.

In this manuscript, a green and fast vortex-assisted hydrophobic magnetic deep eutectic solvent-based dispersive liquid phase microextraction (VA-HMDES-DLPME) method was developed for the selective extraction and determination of niclosamide in read samples, including rice, medicine tablets, and water samples. Here, hydrophobic magnetic deep eutectic solvents were used as the extracting solvent without requiring any centrifugation step. In the light of preliminary experiments, important parameters, such as volume of extraction solvent, pH, acetonitrile volume and vortex time, affecting the extraction efficiency of niclosamide were optimized using a Box-Behnken design. The linear dynamic range (0.25-120 µg/L), the limit of detection (0.08 µg/L), the limit of quantitation (0.25 µg/L), preconcentration factor (180), and enrichment factor (130) of the method were determined using optimized data. In particular, the validation parameters of the optimized VA-HMDES-DLPME, including robustness, matrix effect accuracy, and precision, were investigated. In addition to this, intra- and inter-day precisions were determined as≤3.5 % and≤4.1%, respectively. Finally, the optimized method was successfully used for the extraction of niclosamide in the selected samples prior to spectrophotometric analysis.

Using of Salicylaldehyde Reagent in Spectrophotometric Determination of Niclosamide Via Schiff Base Reaction

The present method includes spectrophotometric determination of niclosamide (NICS) via Schiff base reaction in an alcoholic medium (ethanol) after reducing the nitro group in NICS by added zinc powder in an acidic medium to produce a primary amine group which can be coupled with the salicylaldehyde (SSA) reagent to give a yellow solution whose absorption is followed at the wavelength of 405 nm. Beer's law limitation for the proposed method was in the range of concentrations of 4.0-30 μg. ml-1. The molar absorbance value was 8.701 x 104 l mol.-1 cm.-1 and Sandell's sensitivity value was 0.0376 μg. cm-2. The effect of the reaction components was studied separately by changing one of the components and keeping the other constant, and the optimal conditions were chosen for all these studied components. The proposed method has been successfully applied for the determination of NICS in a pharmaceutical formulation (Yumesan tablets). The recovery percentage of the medicinal compound under study (niclosamide) from the tablet pharmaceutical preparation (Yumesan) via applying the suggested method was not less than 96.36%, and the values of each of the low detection limit (LOD), the low quantitation limit (LOQ), the relative error percentage (RE%), and the relative standard deviation percentage (RSD%), their values were calculated as they are listed 0.9778 μg. ml-1, 3.259 μg. ml-1, -3.61% and not more than 3.67% respectively.

Determination of Niclosamide and its Metabolites in Liver and Muscles of Common Carp (Cyprinus carpio) Fingerlings

Background: Niclosamide is a medication used to treat tapeworm infestation in animals and humans. It is also lampricide and molluscicide, and can be used in in agriculture as a pesticide. In the treatment of parasitic diseases in fish, niclosamide can be used as bath or mixed with the feed. Its most important use in common carp (Cyprinus carpio) is for the treatment of Bothriocephalus acheilognathi, which is a very common parasite in this fish species. The aim of this study was to determine the concentrations of niclosamide (NIC) and its metabolite 2-chloro 4-nitro aniline (CNA) and 5-chloro salycilic acid (CSA) in the liver and muscles of common carp fingerlings.Materials, Methods & Results: The fish for the experiment were obtained from Kapetanski Rit fish pond, and were acclimated to test conditions at 20.5 ± 1°C. Common carps with an average mass of 60 ± 10 g were treated with niclosamide in concentration of 2 g/kg of feed during five consecutive days. The experiment was performed in two treatments: one control and niclosamide, in three replications. Each group contained of 30 fish, in 120 L polyethylene tanks. At the end of the treatment, the levels of niclosamide residues were determined using a high performance liquid chromatography (HPLC) analysis during over 13 days. The mean values of niclosamide and CNA concentrations in the muscles ranged from 27.7 µg/kg starting from the first day to <0.5 µg/kg on the 11th day and 14.2 µg/kg from the first day to <1 µg/kg on the 9th day. The CSA metabolite in muscles were <1 µg/kg during throughout the entire study. The niclosamide concentration in the liver were found to be 51.5 (30.2-61.8) µg/kg the first day and decreased proportionally to <0.5 µg/kg on the13th day. CNA level in the liver of treated Common Carps amounted to 170.1 (157-181) µg/kg on the first day and continuously declined until the 13th day when recorded values were <1 µg/kg. The CSA concentrations in the liver reached a maximum level of 11.5 (10.1-12.8) µg/kg on the 7th day and fell to <1 µg/kg on the 13th day.Discussion: Niclosamide use in fish is questionable, primarily due to the possible toxic effects on some aquatic organisms. In Serbia, niclosamide preparation for use in aquaculture, has been produced by Veterinarski zavod Subotica since 1984 when it was registred for the first time. Niclosamid degradation mechanism showed that the metabolism of niclosamide resulted in two main metabolites CNA and CSA. Withdrawal of niclosamide and its residues in the liver and muscle in the present investigation lasted from 9 to 13 days. This decrease in residues concentrations is expected and depends primarily on several factors such as the length and concentration of drug with which the fish is treated, biotransformation, excretion and decomposition of used drug. Niclosamide and CNA were proportionally decreased during the withdrawal time, while the CSA value increased to the seventh day although the fish during this period no longer consumed food with niclosamide, after which the value then decreased until the end of its elimination. This is also not unexpected because it is known that liver and gallbladder is a major organ for collection, storage and elimination of chemical residues. Although the treated fish received 2 mg of the niclosamide per g of feed for five consecutive days results obtained in this study indicate that the maximal residues concentrations were much lower than doses of niclosamide that each fish absorbed into the body. Data obtained during this study provided information about the concentration and withdrawal times of niclosamide and its residues CNA and CSA in the liver and muscles of common carp treated orally.

Determination of Niclosamide in Aquatic Animal Tissue by a Novel Extraction Procedure and High-Performance Liquid Chromatography–Heated Electrospray Ionization-Tandem Mass Spectrometry

Niclosamide is a mollusicide used for aquaculture on a large scale in China. However, it has high toxicity to aquatic animals and may cause damage to DNA. A modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) extraction procedure with high-performance liquid chromatography–heated electrospray ionization-tandem mass spectrometry method was developed for its determination. Samples were extracted with ammoniated acetonitrile, and anhydrous magnesium sulfate was added to remove moisture and precipitate proteins. The extracts were further purified with octadecylsilane. The recoveries of niclosamide in fortified muscle tissue at concentrations of 0.5 to 20 µg/kg were between 76.40% and 95.60% with relative standard deviations less than 9.54%. The limits of detection and quantification were 0.2 µg/kg and 0.5 µg/kg, respectively. The developed method was used to study the adsorption of niclosamide in channel catfish after administration.

Kinetic study and mechanism of Niclosamide degradation

A spectrophotometric kinetic study of Niclosamide alkaline degradation as a function of drug concentration, alkaline concentration and temperature has been established utilizing double divisor-ratio spectra spectrophotometric method. The developed method allowed determination of Niclosamide in presence of its alkaline degradation products; namely; 2-chloro-4-nitro aniline (DEG I) and 5-chloro salicylic acid (DEG II) with characterization of its degradation mechanism. It was found that degradation kinetic of Niclosamide followed pseudo-first order under the established experimental conditions with a degradation rate constant (k) of 0.0829mol/h and half life (t1/2) of 8.35h. The overall degradation rate constant as a function of the temperature under the given conditions obeyed Arrhenius equation where the activation energy was calculated to be 3.41kcal/mol.

Selective Differential Spectrophotometric Methods for Determination of Niclosamide and Drotaverine Hydrochloride

ABSTRACT Differential (ΔA), second derivative (ΔD2) and third derivative (ΔD3) differential ultraviolet spectrophotometric methods have been presented for the quantitation of niclosamide and drotaverine hydrochloride in pure forms and in their pharmaceutical formulations. For niclosamide, the method is based on measuring ΔΔ A, Δ ΔD2, A ΔD3 of niclosamide in alkaline solutions against their neutral ethanolic solutions as blanks. For drotaverine hydrochloride, the acidic solutions of the drug are measured against their alkaline solutions as blanks. The proposed methods are sensitive, highly specific and advangageous over the conventional UV assays, since the interference of the excipients, impurities, degradation products or other accompanying drugs is nullified. Accuracy of the analysis with the proposed procedures is significantly greater than the classical spectrophotometric methods.

Spectrophotometric Determination of Niclosamide Using P-Benzoquinone

A simple spectrophotometric method for the determination of niclosamide in pure and dosage forms has been developed. The proposed method is based on the reduction of the nitro group in niclosamide to the amino group by heating in a water bath a mixture of niclosamide solution in 95% ethanol, zinc powder and dilute hydrochloric acid for 15 minutes. The cold and clear filtrate reacts with p-benzoguinone, where a compound of pink colour is obtained which absorbs maximally at 506 nm. The stoichiometry of the proposed method and the possible pathway of the reaction is presented. The method determines from 12.5–125 μg/ml of niclosamide with mean percentage recovery of 100.07 ± 0.707. The suggested method was applied to Niclosan and Yomesan tablets and its validity was ascertained by standard addition technique.

Rapid and Accurate Method for Determination of Niclosamide Released from Molluscicidal Formulations

Abstract A rapid, simple, and reproducible method was developed for quantitative determination of niclosamide ethanolamine salt (NES) — the most widely used molluscicide against snail vectors of schistosomiasis — in both distilled and natural canal waters. The biocide is extracted completely from water samples by passing through Sep-Pak C18 cartridge and eluting the cartridge with methanol. The eluate is then analyzed directly for NES by UV/vis spectrophotometry at 330 nm. This method was found sensitive enough to detect 0.1–5 ppm, and it is highly reproducible (standard deviation, 0.006–0.012). The standard curve obeyed Beer’s law. The method also successfully measured the release rate of NES from controlled-release elastomeric formulations. The release study suggests that NES loading and certain rubber additives are not the key factors that govern the release of the biocide.