Development and validation of a simple and rapid capillary zone electrophoresis method for determination of nnrti nevirapine in pharmaceutical formulations
Abstract:Um método simples e rápido por eletroforese capilar foi desenvolvido e validado para a quantificação do inibidor não nucleosídeo da transcritase reversa (NNRTI) nevirapina, em medicamentos. A análise foi otimizada utilizando tampão fosfato de sódio 10 mmol L -1 , pH 2,5, voltagem aplicada de +25 kV, injeção hidrodinâmica a 0,5 psi por 5 s e detecção UV em 200 nm. Diazepam (50,0 µg mL -1 ) foi usado como padrão interno. Sob estas condições, nevirapina foi analisada em aproximadamente menos de 2,5 min. A curva a… Show more
“…Analytical methods are reported in the literature for the determination of NVP in tablets and suspensions. They employ techniques such as capillary electrophoresis [10] [11], electroanalysis [12]- [23], spectrophotometry [24]- [33], high performance liquid chromatography (HPLC) [24] [28] [34]- [63], liquid chromatography coupled with mass spectrometry LC/MS/MS [64]- [77], gas chromatography coupled with mass spectrometry (CG-MS) [78] and high performance thin layer chromatography (HPTLC) [58] [79]. The International Pharmacopoeia, USP, British and European Pharmacopoeia have adopted the HPLC method for the quantitative analysis of nevirapine in formulations [80] [81] [82] [83].…”
The development of the spectrofluorimetric method can be considered a promising alternative that is relatively less expensive and sufficiently reliable. In the current literature, no method for the analysis of nevirapine by spectrofluorimetric has been reported. The proposed method is based on the transformation of naturally non-fluorescent nevirapine into a fluorescent derivative after chemical synthesis. Maximum excitation and emission wavelengths are 290 nm and 357 nm respectively. The analytical performance of the method demonstrates linearity in the concentration range 1.5 × 10 −2 and 13.5 × 10 −2 μg/mL with a correlation coefficient (r) greater than 0.999. The detection (LOD) and quantification (LOQ) limits found are 1.97 × 10 −3 μg/mL and 5.48 × 10 −3 μg/mL respectively. Recovery is achieved with 99.9% and 100.3% trueness, intra-day precision with a coefficient of variation of repeatability (CVr) of 0.99% and inter-day precision with a coefficient of variation of precision (CVR) of 1.7%. The method has been successfully applied in the analysis of 10 batches of nevirapine tablets and suspensions.
“…Analytical methods are reported in the literature for the determination of NVP in tablets and suspensions. They employ techniques such as capillary electrophoresis [10] [11], electroanalysis [12]- [23], spectrophotometry [24]- [33], high performance liquid chromatography (HPLC) [24] [28] [34]- [63], liquid chromatography coupled with mass spectrometry LC/MS/MS [64]- [77], gas chromatography coupled with mass spectrometry (CG-MS) [78] and high performance thin layer chromatography (HPTLC) [58] [79]. The International Pharmacopoeia, USP, British and European Pharmacopoeia have adopted the HPLC method for the quantitative analysis of nevirapine in formulations [80] [81] [82] [83].…”
The development of the spectrofluorimetric method can be considered a promising alternative that is relatively less expensive and sufficiently reliable. In the current literature, no method for the analysis of nevirapine by spectrofluorimetric has been reported. The proposed method is based on the transformation of naturally non-fluorescent nevirapine into a fluorescent derivative after chemical synthesis. Maximum excitation and emission wavelengths are 290 nm and 357 nm respectively. The analytical performance of the method demonstrates linearity in the concentration range 1.5 × 10 −2 and 13.5 × 10 −2 μg/mL with a correlation coefficient (r) greater than 0.999. The detection (LOD) and quantification (LOQ) limits found are 1.97 × 10 −3 μg/mL and 5.48 × 10 −3 μg/mL respectively. Recovery is achieved with 99.9% and 100.3% trueness, intra-day precision with a coefficient of variation of repeatability (CVr) of 0.99% and inter-day precision with a coefficient of variation of precision (CVR) of 1.7%. The method has been successfully applied in the analysis of 10 batches of nevirapine tablets and suspensions.
“…For the measurement of EFV, different analytical tests have been established, including chromatographic [1,[4][5][6][7][8][9][10][11], spectrophotometric methods [2,12], and electrophoresis [13,14]. These assays, on the other hand, are expensive and necessitate lengthy and arduous experimental procedures, solvent extraction, sample pre-treatment, optimized instruments, and a qualified analyst [3,15].…”
In this study, a new hybrid sensor was developed using titanium oxide nanoparticles (TiO2-NPs) and nafion as an anchor agent on a glassy carbon electrode (GCE/TiO2-NPs-nafion) to detect efavirenz (EFV), an anti-HIV medication. TiO2-NPs was synthesized using Eucalyptus globulus leaf extract and characterized using ultraviolet–visible spectroscopy (UV–VIS), scanning electron microscopy (SEM), X-ray diffraction (XRD), and energy-dispersive spectroscopy (EDS). The electrochemical and sensing properties of the developed sensor for EFV were assessed using cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The current response of GCE/TiO2-NPs-nafion electrode towards the oxidation of EFV was greater compared to the bare GCE and GCE/TiO2-NPs electrodes. A linear dynamic range of 4.5 to 18.7 µM with 0.01 µM limit of detection was recorded on the electrode using differential pulse voltammetry (DPV). The electrochemical sensor demonstrated good selectivity and practicality for detecting EFV in pharmaceuticals (EFV drugs) with excellent recovery rates, ranging from 92.0–103.9%. The reactive sites of EFV have been analyzed using quantum chemical calculations based on density functional theory (DFT). Monte Carlo (MC) simulations revealed a strong electrostatic interaction on the substrate-adsorbate (GCE/TiO2-NPs-nafion-EFV) system. Results show good agreement between the MC computed adsorption energies and the experimental CV results for EFV. The stronger adsorption energy of nafion onto the GCE/TiO2-NPs substrate contributed to the catalytic role in the signal amplification for sensing of EFV. Our results provide an effective way to explore the design of new 2D materials for sensing of EFV, which is highly significant in medicinal and materials chemistry.
Bi2O3 nanoparticles were synthesized by solution combustion method and utilized for fabrication of an electrochemical sensor [carbon paste electrode modified with Bi2O3 (CPE‐Bi2O3)] for nevirapine (NVP). Electrode materials were characterized by XRD, FTIR, TG‐DTA, AFM and SEM‐EDS methods. CPE‐Bi2O3 was electroreduced (Er) in KOH in the potential range of −1.3–0 V to obtain CPE‐ErBi2O3. CPE‐ErBi2O3 exhibited electrocatalytic activity towards the oxidation of NVP. Under optimized conditions, linearity between the peak current and NVP concentration was observed in the range of 0.05–50 µM. Further, the sensor was used for the assay of NVP in tablets and biological samples.
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