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1.
Appl Microbiol Biotechnol ; 108(1): 198, 2024 Feb 07.
Artigo em Inglês | MEDLINE | ID: mdl-38324052

RESUMO

The increasing antibiotic resistance towards a panel of microorganisms is one of the public health concerns. For this reason, the search for alternatives to the widely used antibiotic has been undertaken. In the era of sustainable chemistry, deep eutectic solvents (DESs) have emerged as promising antimicrobial agents. These solvents possess several advantages such as low volatility, low flammability, ease of preparation, and typically low cost of production. These properties make DES suitable for various applications, including extraction of biomolecules and preparation of cosmetics. Natural DESs (NADESs) are special category of DESs prepared from natural sources, which matched the recent trends of leaning back to nature, and decreasing dependence on synthetic precursors. NADES can be prepared by heating and stirring, freeze-drying, evaporation, grinding, and ultrasound-assisted and microwave-assisted synthesis. Utilizing NADESs as an alternative to traditional antibiotics, which become ineffective over time due to bacterial resistance, holds great promise for these reasons. This review aims to discuss the antimicrobial properties of multiple NADESs, including antibacterial and antifungal activities. To the best of our knowledge, this review is the first literature survey of the antimicrobial activities of NADESs. KEY POINTS: • Natural deep eutectic solvents are promising antimicrobial alternative to antibiotics • NADES holds high potential for their activity against bacterial resistance • NADES have also substantial antifungal activities.


Assuntos
Antifúngicos , Solventes Eutéticos Profundos , Antibacterianos , Solventes , Liofilização
2.
Altern Ther Health Med ; 30(8): 43-51, 2024 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-39110055

RESUMO

Background: Viral diseases are a worldwide concern as some of them are associated with unexpectedly high mortality rates. Common viruses include e.g., Influenza virus, HIV, hepatitis viruses, and recently COVID-19. Many viral diseases are still incurable by conventional antiviral drugs. Moreover, the emergence of resistant viral strains has reinforced the search for other alternatives. In ancient times, herbal therapy was commonly used where medicinal formulations were created from various plants. In recent times, in vitro, in vivo, animal studies, and clinical trials have revealed the antiviral properties of these plants, sparking hope for the treatment of serious viral diseases. The present review aims to summarize studies that focus on medicinal plants available in Egypt with antiviral properties. Methods: The articles published in English between 1988 and 2022 and available in PubMed and Scopus databases with the relevant keywords were included. Results: Thirty-two plants in Egypt have met the criteria and possess in vitro or in vivo antiviral activity via different mechanisms. Only five of them; Camellia sinensis, Marine algae, Zizyphus spina-christi L., Trachyspermum Ammi, and Aloe Vera have been proven to be effective in vivo. For COVID-19, thirteen plants have shown efficacy against SARS-Cov-2 via different mechanisms including Camellia sinensis, Cinnamomum Verum, Punica granatum, Glycyrrhiza glabra, Zingiber officinale, Curcuma longa, Marine algae, Phlomis aurea oil, Solanum nigrum, Trachyspermum Ammi, Arum palaestinum, Aloe Vera, and Cyperus rotundus. Conclusion: This review summarizes the current scientific evidence on 32 medicinal plant species cultivated in Egypt that have demonstrated antiviral properties against various DNA and RNA viruses through in vitro and in vivo studies, highlighting their potential as prospective sources for the development of novel antiviral therapies. Further clinical research is still warranted to validate the effectiveness and safety of these plants as complementary treatment options for viral infections.


Assuntos
Antivirais , Fitoterapia , Plantas Medicinais , Plantas Medicinais/química , Humanos , Antivirais/farmacologia , Antivirais/uso terapêutico , Egito , Fitoterapia/métodos , Animais , Tratamento Farmacológico da COVID-19 , Extratos Vegetais/farmacologia , Extratos Vegetais/uso terapêutico , SARS-CoV-2/efeitos dos fármacos , Viroses/tratamento farmacológico
3.
J Fluoresc ; 33(4): 1337-1346, 2023 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-36648625

RESUMO

A simple, fast, and ecofriendly spectrofluorometric method was developed and validated for determination of mono sodium glutamate (MSG). The method depended on the reaction between MSG and iron (III) salicylate based on ligand exchange mechanism. Addition of MSG turned-on the fluorescent response of iron (III) salicylate at λem 411 nm. Reaction conditions including reagent concentration, pH, and time were optimized. The method was validated regarding the ICH guidelines. The method determined MSG within the linearity range of 25-250 µM with a coefficient of determination of 0.9967 and a calculated limit of detection of 1.73 µM. Furthermore, the developed method was successfully applied for the determination of MSG in food preparation (instant noodles). The results were compared to those obtained by a published HPLC method using t-test and F-test at 95% confidence interval; no statistically significant difference was found. Based on the analytical Eco-scale and the green analytical procedure index (GAPI), the developed method was assessed to be greener than the published HPLC method. The developed method offered advantages over other spectrophotometric reported methods and was convenient for routine determination of MSG in foodstuffs.


Assuntos
Corantes , Glutamato de Sódio , Indicadores e Reagentes , Cromatografia Líquida de Alta Pressão , Espectrometria de Fluorescência
4.
Postgrad Med J ; 99(1175): 962-975, 2023 Aug 22.
Artigo em Inglês | MEDLINE | ID: mdl-36892422

RESUMO

Google Trends has been extensively used in different sectors from finance to tourism, the economy, fashion, the fun industry, the oil trade, and healthcare. This scoping review aims to summarize the role of Google Trends as a monitoring and a predicting tool in the COVID-19 pandemic. Inclusion criteria for this scoping review were original English-language peer-reviewed research articles on the COVID-19 pandemic conducted in 2020 using Google Trends as a search tool. Articles that were in a language other than English, were only in abstract form, or did not discuss the role of Google Trends during the COVID-19 pandemic were excluded. According to these criteria, a total of 81 studies were included to cover the period of the first year after the emergence of the crisis. Google Trends can potentially help health authorities to plan and control pandemics earlier and to decrease the risk of infection among people.


Assuntos
COVID-19 , Humanos , COVID-19/epidemiologia , Pandemias , Ferramenta de Busca , Revisão por Pares
5.
Virol J ; 19(1): 152, 2022 09 22.
Artigo em Inglês | MEDLINE | ID: mdl-36138463

RESUMO

The coronavirus pandemic is a worldwide hazard that poses a threat to millions of individuals throughout the world. This pandemic is caused by the severe acute respiratory syndrome-coronavirus 2 (SARS-CoV-2), which was initially identified in Wuhan, China's Hubei provincial capital, and has since spread throughout the world. According to the World Health Organization's Weekly Epidemiological Update, there were more than 250 million documented cases of coronavirus infections globally, with five million fatalities. Early detection of coronavirus does not only reduce the spread of the virus, but it also increases the chance of curing the infection. Spectroscopic techniques have been widely used in the early detection and diagnosis of COVID-19 using Raman, Infrared, mass spectrometry and fluorescence spectroscopy. In this review, the reported spectroscopic methods for COVID-19 detection were discussed with emphasis on the practical aspects, limitations and applications.


Assuntos
COVID-19 , COVID-19/diagnóstico , Teste para COVID-19 , Diagnóstico Precoce , Saúde Global , Humanos , Pandemias , SARS-CoV-2
6.
J Sep Sci ; 45(1): 185-209, 2022 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-34472701

RESUMO

Liquid-liquid extraction is a widely used technique of sample preparation in biomedical analysis. In spite of the high pre-concentration capacities of liquid-liquid extraction, it suffers from a number of limitations including time and effort consumption, large organic solvent utilization, and poor performance in highly polar analytes. Homogeneous liquid-liquid extraction is an alternative sample preparation technique that overcomes some drawbacks of conventional liquid-liquid extraction, and allows employing greener organic solvents in sample treatment. In homogeneous liquid-liquid extraction, a homogeneous phase is formed between the aqueous sample and the water-miscible extractant, followed by chemically or physically induced phase separation. To form the homogeneous phase, aqueous samples are mixed with water-miscible organic solvents, water-immiscible solvents/cosolvents, surfactants, or smart polymers. Then, phase separation is induced chemically (adding salt, sugar, or buffer) or physically (changing temperature or pH). This mode is rapid, sustainable, and cost-effective in comparison with other sample preparation techniques. Moreover, homogeneous liquid-liquid extraction is more suitable for the extraction of delicate macromolecules such as enzymes, hormones, and proteins and it is more compatible with liquid chromatography with tandem mass spectrometry, which is a vital technique in metabolomics and proteomics. In this review, the principle, types, applications, automation, and technical aspects of homogeneous liquid-liquid extraction are discussed.


Assuntos
Hormônios/isolamento & purificação , Extração Líquido-Líquido/métodos , Proteínas/isolamento & purificação , Animais , Cromatografia Líquida de Alta Pressão , Hormônios/química , Humanos , Extração Líquido-Líquido/instrumentação , Proteínas/química , Solventes/química , Espectrometria de Massas em Tandem
7.
J Sep Sci ; 45(18): 3529-3541, 2022 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-35894696

RESUMO

A simple stability-indicating reversed-phase high-performance liquid chromatography method has been developed for determination of elobixibat in presence of its potential impurities and degradation products. The chromatographic separation was carried on a Thermo scientific Base Deactivated Silica BDS Hypersil-C18 (150 × 4.6 mm; 5 µm) column using a mobile phase of acetonitrile and phosphate buffer (25 mM, pH 2.5) in a ratio of (70:30, v/v). The experimental conditions were accurately investigated, and the method was validated according to ICH guidelines Q2 (R1). The drug was subjected to various stress conditions including acidic, basic, oxidative, and photolytic conditions. The method successfully separates the drug from the three reported impurities and different degradants. The method was also successfully applied for the determination of elobixibat in laboratory prepared tablets (5.0 mg). Analysis shows no interference from excipients and degradation products. The method was also applied for performing in vitro dissolution testing of elobixibat laboratory prepared tablets. Since elobixibat is recently introduced into the market, there are no previous stability studies and no reported analytical methods for its determination. Thus, this study presents a validated and selective method that can be effectively employed in routine quality control studies.


Assuntos
Excipientes , Dióxido de Silício , Acetonitrilas , Cromatografia Líquida de Alta Pressão/métodos , Dipeptídeos , Estabilidade de Medicamentos , Fosfatos , Reprodutibilidade dos Testes , Solubilidade , Comprimidos , Tiazepinas
8.
Biomed Chromatogr ; 36(6): e5365, 2022 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-35274347

RESUMO

Favipiravir is a potential antiviral medication that has been recently licensed for Covid-19 treatment. In this work, a gadolinium-based magnetic ionic liquid was prepared and used as an extractant in dispersive liquid-liquid microextraction (DLLME) of favipiravir in human plasma. The high enriching ability of DLLME allowed the determination of favipiravir in real samples using HPLC/UV with sufficient sensitivity. The effects of several variables on extraction efficiency were investigated, including type of extractant, amount of extractant, type of disperser and disperser volume. The maximum enrichment was attained using 50 mg of the Gd-magnetic ionic liquid (MIL) and 150 µl of tetrahydrofuran. The Gd-based MIL could form a supramolecular assembly in the presence of tetrahydrofuran, which enhanced the extraction efficiency of favipiravir. The developed method was validated according to US Food and Drug Administration bioanalytical method validation guidelines. The coefficient of determination was 0.9999, for a linear concentration range of 25 to 1.0 × 105  ng/ml. The percentage recovery (accuracy) varied from 99.83 to 104.2%, with RSD values (precision) ranging from 4.07 to 11.84%. The total extraction time was about 12 min and the HPLC analysis time was 5 min. The method was simple, selective and sensitive for the determination of favipiravir in real human plasma.


Assuntos
Tratamento Farmacológico da COVID-19 , Líquidos Iônicos , Microextração em Fase Líquida , Amidas , Cromatografia Líquida de Alta Pressão/métodos , Furanos , Gadolínio , Humanos , Microextração em Fase Líquida/métodos , Fenômenos Magnéticos , Pirazinas
9.
Anal Chem ; 93(5): 2802-2810, 2021 02 09.
Artigo em Inglês | MEDLINE | ID: mdl-33496173

RESUMO

The influence of the addition of various non-ionic surfactants to poly(ethylene glycol) diacrylate-based monolith formulations was studied. Eight non-ionic surfactants having different chemistries were chosen for this study. These surfactants were Brij L4, Span 80, IGEPAL CO-520, Tergitol 15S9, 2,4,7,9-tetramethyl-5-decyne-4,7-diol ethoxylate, Tween 40, Triton X-405, and Tetronic 701. The chemical structures of these surfactants have a variety of functional groups and cover a wide range of molecular weights (360-3600 g/mol), viscosities (60-1500 cP), and hydrophilic-lipophilic balances (1.0-17.6). The formed polymers were characterized by scanning electron microscopy, surface area measurement by the Brunauer-Emmet-Teller method, elemental analysis, and Fourier transform infrared. Four formulations, involving the use of surfactants, resulted in permeable materials when prepared in 150 µm ID silica capillaries. The chromatographic performance of the resulting columns in reversed-phase mode was evaluated and compared using a mixture of alkyl benzenes as test analytes. The highest efficiency and methylene selectivity were observed when Tween 40 was included in the formulation, using decane/decanol/dodecanol as coporogens. This porogenic mixture was successfully used for preparation of monolithic columns from a selection of methacrylate- and styrene-based monomers, including butylmethacrylate, hydroxyethymethacrylate, laurylmethacrylate, glycidyl methacrylate, bisphenol diacrylate, benzylmethacrylate, and N,N-dimethylacrylamide, as well as for divinylbenzene. These results show the applicability of this porogenic mixture for a variety of monolithic formulations, providing an approach for developing a universal porogen system.

10.
J Fluoresc ; 31(3): 675-684, 2021 May.
Artigo em Inglês | MEDLINE | ID: mdl-33566265

RESUMO

In this study, a novel and simple fluorescent carbon quantum dots (CQDs) based nano-sensor for colchicine determination has been prepared. The nitrogen doped CQDs probe was prepared using uric acid as a carbon/nitrogen source via a one-step pyrolysis. The sensor is based on inner filter effect (IFE) where colchicine acts as a powerful absorber that affects the excitation of the fluorescer (CQDs). This overlap results in a quantitative attenuation of the fluorescence of CQDs with increasing colchicine concentration in the range of 2-25 µM. The developed sensor has the advantages of simplicity, less time-consuming, convenience and satisfactory selectivity for colchicine determination in pharmaceutical dosage forms.

11.
Anal Bioanal Chem ; 413(1): 205-214, 2021 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-33095289

RESUMO

A hydrophobic gadolinium-based magnetic ionic liquid (MIL) was investigated for the first time as an extraction solvent in dispersive liquid-liquid microextraction (DLLME). The tested MIL was composed of trihexyl(tetradecyl)phosphonium cations and paramagnetic gadolinium chloride anions. The prepared MIL showed low water miscibility, reasonable viscosity, markedly high magnetic susceptibility, adequate chemical stability, low UV background, and compatibility with reversed-phase HPLC solvents. These features resulted in a more efficient extraction than the corresponding iron or manganese analogues. Accordingly, the overall method sensitivity and reproducibility were improved, and the analysis time was reduced. The applicability of the proposed MIL was examined through the microextraction of four sartan antihypertensive drugs from aqueous samples followed by reversed-phase HPLC with UV detection at 240 nm. The DLLME procedures were optimized for disperser solvent type, MIL mass, disperser solvent volume, as well as acid, base, and salt addition. The limits of quantitation (LOQs) obtained with the analysis of 1.2-mL samples after DLLME and HPLC were 80, 30, 40, and 160 ng/mL for azilsartan medoxomil, irbesartan, telmisartan, and valsartan, respectively. Correlation coefficients were greater than 0.9988 and RSD values were in the range of 2.48-4.07%. Under the optimized microextraction conditions and using a 5-mL sample volume, enrichment factors were raised from about 40 for all sartans using a 1.2-mL sample to 175, 176, 169, and 103 for azilsartan medoxomil, irbesartan, valsartan, and telmisartan, respectively. The relative extraction recoveries for the studied sartans in river water varied from 82.5 to 101.48% at a spiked concentration of 0.5 µg/mL for telmisartan and irbesartan and 1 µg/mL for azilsartan medoxomil and valsartan. Graphical abstract.


Assuntos
Gadolínio/química , Líquidos Iônicos/química , Microextração em Fase Líquida/métodos , Magnetismo , Cromatografia Líquida de Alta Pressão , Humanos , Interações Hidrofóbicas e Hidrofílicas , Líquidos Iônicos/toxicidade , Limite de Detecção , Reprodutibilidade dos Testes , Solventes/química , Espectrofotometria Ultravioleta , Água/química
12.
J Sep Sci ; 44(16): 3117-3125, 2021 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-34101992

RESUMO

Miniaturization of liquid-liquid extraction is a growing field of sample preparation to reduce solvent consumption, protect the environment, and preserve operators' health. In this work, four different modes of liquid-liquid microextraction have been compared including dispersive liquid-liquid microextraction, binary and ternary salting-out, and sugaring-out induced liquid-liquid microextraction. The extraction efficiency was evaluated by the enrichment factors of 14 different drugs from three pharmacological classes. Compared with the other modes, sugaring-out induced liquid-liquid microextraction was found to be the most efficient and, thus, it was applied for sample preparation of the antivirals in human plasma. Method optimization was performed using response surface methodology for the sugar type and amount (in mg), the sample pH, the equilibration time (in min), and the extractant volume (in µL). The method was then validated and found linear in the concentration range of 0.10-10 µg/mL for daclatasvir, 0.05-10 µg/mL for velpatasvir, and 0.20-10 µg/mL for ledipasvir, with correlation coefficients in the range 0.996-0.999. These results shows that sugaring-out induced liquid-liquid microextraction could be a more efficient microextraction mode for preparation of biological samples. Compared with other types of microextraction, sugaring-out induced liquid-liquid microextraction is greener, simpler, and cost-effective, with less tendency to affect the sample pH.


Assuntos
Frutose/química , Glucose/química , Microextração em Fase Líquida/métodos , Extração Líquido-Líquido/métodos , Sacarose/química , Acetonitrilas/análise , Antivirais/análise , Cromatografia , Humanos , Concentração de Íons de Hidrogênio , Limite de Detecção , Modelos Lineares , Análise de Regressão , Reprodutibilidade dos Testes , Cloreto de Sódio , Solventes
13.
J Sep Sci ; 43(1): 56-69, 2020 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-31589375

RESUMO

Porogens are key components required for the preparation of porous polymer monoliths for application in separation science. Porogens determine the stability, selectivity, and permeability of polymer monoliths. This review summarizes the role of porogens in the preparation of porous polymer monoliths with a focus on clear understanding of effect of porogens on morphological properties, porosity, surface area, mechanical stability, and permeability of monoliths, particularly targeting the field of separation science. This review also includes the use of different types of porogens with the focus on various approaches used to set criteria for their systematic selection, including porogen-free techniques recently used for synthesis of porous monoliths. It discusses the current state-of-the-art applications of porogens in column preparation as well as where the future developments in this field may be directed.

14.
Luminescence ; 34(3): 375-381, 2019 May.
Artigo em Inglês | MEDLINE | ID: mdl-30884083

RESUMO

Sodium alendronate is the first in a pharmacological class known as bisphosphonates, used for treatment of various bone diseases. Assay of bisphosphonates by a spectroscopic technique is very challenging due to the fact that they lack chromophores and none of them are fluorescent. In this work, a simple method is presented for determination of alendronate in bulk and in pharmaceutical tablets using spectrofluorometry by exploiting the ability of alendronate to displace salicylate from the iron(III)-salicylate chelate, forming a non-fluorescent colorless iron(III)-alendronate complex. The liberated salicylate is fluorescent and is equivalent to the mount of alendronate added. The response was linear over the concentration range 20-90 µM and the proposed method was validated according to the guidelines of the International Conference on Harmonization. The correlation coefficient was found to be 0.995 and the limit of detection was 7.5 µM. The method was successfully applied for determination of alendronate in the commercially available Osteonate® tablets. The average percent recovery ± percent relative standard deviation was found to be 102.118 ± 2.033 which is congruent with the label claim of the dosage form. The results were also compared to a reported method using t-test and F-test at 95% confidence level; no significant differences were observed. The presented method is simple, fast, easy, cost-effective and suitable for routine pharmaceutical analysis.


Assuntos
Alendronato/análise , Conservadores da Densidade Óssea/análise , Espectrometria de Fluorescência/métodos , Fluorescência , Comprimidos/análise
15.
Spectrochim Acta A Mol Biomol Spectrosc ; 322: 124825, 2024 Dec 05.
Artigo em Inglês | MEDLINE | ID: mdl-39033610

RESUMO

The COVID-19 pandemic has highlighted the urgent need for effective antiviral agents. One such promising drug is nirmatrelvir (NIRMA), which has demonstrated the ability to inhibit viral replication and reduce hospitalization and mortality rates. In the field of analytical chemistry, carbon quantum dots (CQDs) derived from fruit peel waste have gained attention for their eco-friendly and cost-effective properties. In this study, CQDs were synthesized from the peel biomass waste of yellow lupin and utilized for the spectrofluorometric determination of NIRMA in pharmaceutical tablets. The proposed method offers simplicity and speed compared to existing methods. The synthesis process involved washing and grinding the peel waste, followed by heating in propylene glycol and purification using a dialysis membrane. The resulting CQD solution showed fluorescence at an emission wavelength of 411 nm upon excitation at 325 nm. The validation of the method, including linearity, range, limit of detection and quantification, accuracy, precision, and robustness, was conducted following ICH guidelines. The fluorescence intensities exhibited a linear relationship with increasing NIRMA concentration in the range of 15-150 µg/mL. The limit of detection found to be 4.0 µg/mL, with %relative standard deviations ≤ 1.46. This spectrofluorometric method represents a novel approach for the determination of NIRMA using CQDs derived from yellow lupin peel waste.


Assuntos
Carbono , Química Verde , Lupinus , Pontos Quânticos , Espectrometria de Fluorescência , Pontos Quânticos/química , Carbono/química , Espectrometria de Fluorescência/métodos , Química Verde/métodos , Lupinus/química , Limite de Detecção , Antivirais/análise , Antivirais/química , Reprodutibilidade dos Testes , Comprimidos
16.
J Pharm Biomed Anal ; 248: 116270, 2024 Sep 15.
Artigo em Inglês | MEDLINE | ID: mdl-38870836

RESUMO

The misuse of pregabalin has become a significant issue over the last decade. Consequently, there is a growing demand for a sensitive and selective method for its determination. In this study, an eco-friendly cobalt-doped carbon quantum dots (CQDs) have been fabricated and applied as nanoprobes for the fluorometric determination of pregabalin. The CQDs were synthesized through mixed doping with non-metallic atoms such as nitrogen and sulfur, and a metal ion, cobaltous ion, via a microwave-assisted method in just 1.5 min. The synthesized Co-NS-CQDs exhibited advantageous characteristics, including rapid response times, compatibility with various pH levels, exceptional detection limits, high sensitivity, and excellent selectivity. The Co-NS-CQDs exhibited a high quantum yield (55 %) relative to NS-CQDs (38 %), with blue emissive light at 438 nm. The assessment of pregabalin was based on its enhancement effect on the native fluorescence intensity of CQDs. The proposed method had a good linearity over the range of 25-250 µg/mL, with a limit of detection of 4.17 µg/mL and a limit of quantitation of 12.63 µg/mL, respectively. The prepared NS-CQDs have been successfully applied for the pregabalin determination in pharmaceutical capsules, with excellent % recovery (98-102 %). The greenness of the developed method has been investigated using different greenness metrics, in comparison with the reported RP HPLC method. The greenness characteristics of the method originated from the synthesis of CQDs, utilizing sustainable, readily available, and cost-effective starting materials.


Assuntos
Cápsulas , Carbono , Cobalto , Limite de Detecção , Pregabalina , Pontos Quânticos , Espectrometria de Fluorescência , Pregabalina/análise , Pregabalina/química , Pontos Quânticos/química , Cobalto/química , Cobalto/análise , Carbono/química , Espectrometria de Fluorescência/métodos , Química Verde/métodos
17.
J Pharm Biomed Anal ; 242: 116021, 2024 May 15.
Artigo em Inglês | MEDLINE | ID: mdl-38354540

RESUMO

Multicomponent drugs are medications that combine two or more active pharmaceutical ingredients in a single dosage form. These dosage forms improve the patient compliance, reduce the risk of drug interactions, and simplify dosing regimens. However, quality control of these multicomponent dosage forms can be challenging, especially if the final product contains four or more ingredients that are active (comprise stabilizers, preservatives, excipients, and other components). This problem can be more pronounced if the excipients can interfere with the analysis. In this work, a stability indicating assay method was developed and validated (according to the ICH International Guidelines) for the simultaneous determination of hydroquinone (HQ), tretinoin (TRT), hydrocortisone (HCA), butylated hydroxytoluene (BHT), methyl paraben (MP) and propyl paraben (PP) in commercially available pharmaceutical creams. The proposed method is based on gradient elution using X-Bridge C18 (150 × 4.6 mm, 5 µm) column with a flow rate of 1 mL/min. The linear ranges (µg/mL) were 240-560 for HQ, 24-56 for MP, 132-308 for HCA, 6-14 for PP, 12-28 for BHT, 6.6-15 for TRT. During the validation process, the intra- and interday precision and trueness (evaluated as recovery) were found to be below 2.0% and between 100-102%, respectively. System suitability tests (SST) allow validating the herein proposed procedure specifically for pharmaceutical and industrial applications. SST test shows that the reported procedure fulfill with the Guidelines, allowing excellent separation of the analytes with very sensitive, accurate (precise and true) and reproducible quantitation of each analytes. The method was successfully applied in forced degradation studies of the six analytes. Specifically, acid degradation slightly affected HCA and BHT (91% recovery), while alkaline degradation drastically reduced HCA recovery (5.5%) and moderately affected BHT (85%). Photodegradation primarily influenced TRT quantity, and oxidative degradation intensified the BHT peak (130%).


Assuntos
Parabenos , Tretinoína , Humanos , Parabenos/análise , Tretinoína/análise , Hidrocortisona/análise , Hidroxitolueno Butilado , Excipientes , Cromatografia Líquida de Alta Pressão/métodos , Hidroquinonas/análise
18.
J Chromatogr A ; 1732: 465192, 2024 Sep 13.
Artigo em Inglês | MEDLINE | ID: mdl-39079363

RESUMO

Metal-organic frameworks (MOFs) are a fascinating family of crystalline porous materials made up of metal clusters and organic linkers. In comparison with other porous materials, MOFs have unique characteristics including high surface area, homogeneous open cavities, and permanent high porosity with variable shapes and sizes. For these reasons, MOFs have recently been explored as sorbents in sample preparation by solid-phase extraction (SPE). However, SPE requires large amounts of sorbents and suffers from limited contact surfaces with analytes, which compromises extraction recovery and efficiency. Dispersive SPE (D-SPE) overcomes these limitations by dispersing the sorbents into the sample, which in turn increases contact with the analytes. Miniaturization of the microextraction procedure, particularly the amount of sorbent reduces the amount consumed of the organic solvent and shorten the time required to attain the equilibrium state. This may explain the reported high efficiency and applicability of MOFs in dispersive micro SPE (D-µ-SPE). This method retains all the advantages of solid phase extraction while also being simpler, faster, cheaper, and, in some cases, more effective in comparison with D-SPE. Besides, D-µ-SPE requires smaller amounts of the sorbents which reduces the overall cost, and the amount of waste generated from the analytical process. In this review, we discuss the applications of MOFs in D-µ-SPE of various analytes including pharmaceuticals, pesticides, organic dyes from miscellaneous matrices including water samples, biological samples and food samples.


Assuntos
Estruturas Metalorgânicas , Microextração em Fase Sólida , Estruturas Metalorgânicas/química , Microextração em Fase Sólida/métodos , Extração em Fase Sólida/métodos , Adsorção , Poluentes Químicos da Água/isolamento & purificação , Poluentes Químicos da Água/análise , Poluentes Químicos da Água/química , Porosidade
19.
BMC Chem ; 18(1): 74, 2024 Apr 13.
Artigo em Inglês | MEDLINE | ID: mdl-38615027

RESUMO

This study presents a stability indicating high-performance liquid chromatography HPLC method for the determination of cenobamate (CNB) in presence of its main impurity (CNB H-impurity) and degradation products. The chromatographic separation was carried out on a Thermo BDS Hypersil-C18 column (150 × 4.6 mm; 5 µm) with a mobile phase consisting of a 50:50 (%v/v) ratio of methanol and purified water. The flow rate was maintained at 1.0 mL. min- 1. CNB was detected at 210 nm using a PDA detector. The column temperature was held at 40 °C.The retention time of the drug was found to be 3.2 min. Furthermore, the study investigates the degradation behavior of CNB under various stress conditions, including acidic, basic, oxidative, and light-induced degradation. The results indicate that CNB is particularly susceptible to basic degradation. Consequently, a comprehensive study of the basic degradation kinetics was conducted. The method was also successfully applied for the determination of CNB in its dosage form. The results also show that there is no co-elution from degradation products or excipients as indicated by the mass balance and peak purity values confirming the specificity of the proposed method and its applicability for routine analysis of CNB.

20.
RSC Adv ; 14(12): 8188-8194, 2024 Mar 06.
Artigo em Inglês | MEDLINE | ID: mdl-38469198

RESUMO

A novel, simple, affordable, and reliable colorimetric paper-based analytical device (PAD) was developed for the point-of-use quality testing of ethanol-based hand sanitizers, mainly against adulteration by water. The principle was based on the novel solvatochromism of methylparaben (MPB)-Fe3+ complex, where water is essential for complex formation and ethanol is necessary for MPB solubility. The intensity of the formed violet color, measured at 528 nm, showed a good correlation (R2 = 0.996) with the percentage water in the reaction media over a range from 40% to 100% (0-60% ethanol), with excellent accuracy and precision as indicated by the percent recovery within 100.00% ± 2% and %RSD of <2%. A PAD was prepared by the sequential immobilization of Fe3+ ions and MPB on chitosan-modified filter paper. The developed PAD was successfully applied for the quality testing of ethanol-based hand sanitizers using an established color index, where clearly distinct colors were observed as a function of the percentage ethanol (0-100%). The developed test strips could achieve on-site lab-quality results without expensive or sophisticated instruments using a few milligrams of FeCl3 and MPB in addition to regular filter paper. Accordingly, it can be used as a test strip for the quality checking of ethanol-based hand sanitizers by end users.

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