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1.
Arch Pharm (Weinheim) ; : e2400256, 2024 Jun 18.
Artículo en Inglés | MEDLINE | ID: mdl-38889397

RESUMEN

Green and white chemistry are vital to revolutionizing the chemical industry through their unparalleled potential to enhance sustainability and efficiency. In this study, nine sustainability tools of both green and white metrics, including green analytical procedure index (GAPI), ComplexGAPI, analytical greenness, analytical greenness metric for sample preparation, Analytical Eco-Scale (ESA), analytical method greenness score, high-performance liquid chromatography- environmental assessment tool (HPLC-EAT), analytical method volume intensity, and blue applicability grade index (BAGI), have been developed for appraising environmental friendliness for both innovative and straightforward mean centering of ratio spectra (MCR) and reversed-phase high-performance liquid chromatography (RP-HPLC) strategies utilized for concurrent analysis and separation of cyclopentolate (CYC) and C12 and C14 homologs of benzalkonium chloride (BNZ) in pure and ophthalmic solution. The mobile phase, formed of buffer phosphate and acetonitrile (35:65, v/v), was adjusted to pH 6.3, and 215-nm UV detection was used. The experimental flow rate was 2.0 mL min-1, and the analytical column was L11 Inertsil Ph-3 (150 mm × 4.6 mm, 5 µm). All sequences were run at 25°C in the column oven. The MCR approach effectively resolved the drug's spectral overlapping. CYC and BNZ employed this approach at 227.5 and 220.4 nm, respectively. As part of the HPLC analysis, an isocratic method was employed with phosphate buffer and acetonitrile in the mobile phase at 35:65. A correlation coefficient greater than 0.999 was observed between the calibration curves for the HPLC and MCR methods in the ranges of 20-320 µg mL-1 and 5-30 µg mL-1 for all drugs. The technique yields excellent primary recovery rates, ranging from 97.2% to 100.5%. The recommended approach has been validated according to International Council for Harmonization guidelines.

2.
Arch Pharm (Weinheim) ; : e2400025, 2024 Apr 21.
Artículo en Inglés | MEDLINE | ID: mdl-38644337

RESUMEN

A novel environmentally friendly reversed-phase high-performance liquid chromatography (RP-HPLC) method has been effectively validated for simultaneously measuring a prospective conjunction of tizanidine (TIZ) and etoricoxib (ETC), the combined medicine, in rat plasma. The technique employs diclofenac potassium as the internal standard, guaranteeing dependable and precise outcomes. This study aimed to assess the impact of the suggested combination therapy on treating inflammation resulting from rheumatoid arthritis (RA) in a rat model. The procedure was performed using an Agilent series 1200 model HPLC apparatus. The chromatographic conditions consist of isocratic elution mode, C18 column with dimensions of 150 mm × 4.6 mm × 5 µm, flow rate of 1.5 mL/min, wavelength of 230 nm, temperature of 50°C, and injection volume of 10 µL. The elution was performed using a mobile phase consisting of a phosphate buffer with a pH of 3.5 and acetonitrile in a ratio of 80:20 v/v. Calibration curves were conducted for TIZ and ETC within the 1-50 µg/mL range, demonstrating linear trends with R2 values over 0.999. The effectiveness and eco-friendliness of the proposed method were evaluated using eight separate environmentally conscious metrics. The addition of TIZ and ETC to arthritic rodents amplified these effects significantly. Furthermore, TIZ and ETC significantly reduced serum levels in arthritic rodents, and safety investigations revealed normal complete blood count, liver, and renal functions. TIZ and ETC appear to have antiarthritic, anti-inflammatory, and safe combinations, making them viable future treatment options for RA that are also safe and efficacious. Following validation by United States Food and Drug Administration (US-FDA) rules, all goods met the criteria.

3.
Ann Pharm Fr ; 82(3): 420-432, 2024 May.
Artículo en Inglés | MEDLINE | ID: mdl-37739216

RESUMEN

OBJECTIVES: Allergic rhinitis and chronic idiopathic urticaria are common conditions triggered by environmental irritants, stress, and certain foods. The FDA has recently announced that the efficacy and safety of Ebastine (EBS) have been thoroughly evaluated and confirmed. This study considered using various tools to assess their greenness. We used AGREEprep, analytical eco-scale (ESA), and analytical method volume intensity (AMVI) to evaluate the greenness of the validated stability-indicating method and a forced degradation study. This allowed for easy determination and quantitation of EBS in wastewater and dosage form. METHODS: The method was established on Symmetry RP-C18 (150mm×4.6mm,5µm) using mobile phase, which can be prepared by mixing buffer solution of pH 3 with acetonitrile in a ratio of (37.5: 62.5, v/v) in addition to dissolving 0.72 gm of sodium lauryl sulfate in the final solution. The separation process was executed at a flow rate of 1.5mL/min and 5µL injection volume with UV detection at 254nm. Linearity was conducted for EBS in the 5-50µg/mL range. Different validation parameters were investigated, including accuracy, precision, robustness, and specificity. RESULTS: The limits of both detection and quantification were 0.84µg/mL and 2.57µg/mL for EBS. The recovery percentages of EBS were found to be 101.01% and 101.02% for wastewater and pharmaceutical formulations, respectively. CONCLUSION: According to International Council for Harmonisation (ICH) guidelines, a forced degradation study of EBS was evaluated, including acid, base hydrolysis, and oxidative hydrolysis using hydrogen peroxide and photolytic and thermal degradation. The highest degradation was achieved by acid hydrolysis. The safety and efficacy of EBS were evaluated via a safety comparative profile study.

4.
Molecules ; 23(12)2018 Dec 11.
Artículo en Inglés | MEDLINE | ID: mdl-30544987

RESUMEN

The paper describes the synthesis and biological evaluation of some new benzimidazole derivatives as potent clinical drugs that are useful in the treatment of some microbial infections and tumor inhibition. The starting compound 2-(bromomethyl)-1H-benzimidazole (1) was prepared, and hence underwent interesting functionalization reactions to afford several series of benzimidazole-5-(aryldiazenyl)thiazole derivatives: 3a⁻c, 7a⁻c, and 8a⁻c. The antibacterial activities of the synthesized compounds were evaluated by calculation of the inhibition zone diameter (mm) and the determination of minimum inhibitory concentration (µg/mL) against selected pathogenic bacteria Staphylococcus aureus (Gram-positive bacteria) and Escherichia coli (Gram-negative bacteria).Noticeable efficiency was found based on in vitro screening for their antioxidant activity and cytotoxicity effect against the human liver cancer cell line (HepG2) and human hepatocyte carcinoma cells at relatively high concentrations.


Asunto(s)
Antibacterianos/química , Antibacterianos/farmacología , Antineoplásicos/farmacología , Antibacterianos/síntesis química , Antineoplásicos/síntesis química , Antineoplásicos/química , Antioxidantes/química , Antioxidantes/farmacología , Bencimidazoles/química , Evaluación Preclínica de Medicamentos/métodos , Escherichia coli/efectos de los fármacos , Células Hep G2 , Humanos , Pruebas de Sensibilidad Microbiana , Staphylococcus aureus/efectos de los fármacos , Tiazoles/química
5.
Can J Urol ; 21(2): 7246-7, 2014 Apr.
Artículo en Inglés | MEDLINE | ID: mdl-24775580

RESUMEN

Artificial urinary sphincter (AUS) erosion often involve the urethral cuff and is managed by complete or partial device removal. Abdominal wall erosion of AUS tubing has not been previously reported and its management is unknown. We report tube erosion (TE) of AUS successfully managed without device explant. An 81-year-old male with AUS for post-prostatectomy incontinence presented with TE at the site of inguinal incision without signs or symptoms of infection. The exposed tube was reduced and wound was closed after copious antibiotic solution irrigation. No complications were noted at 2 month follow up. AUS-TE can be successfully managed conservatively with antiseptic wound site irrigation and reinsertion in absence of infection.


Asunto(s)
Pared Abdominal/cirugía , Antibacterianos/uso terapéutico , Falla de Equipo , Irrigación Terapéutica/métodos , Incontinencia Urinaria/terapia , Esfínter Urinario Artificial/efectos adversos , Anciano de 80 o más Años , Humanos , Masculino , Prostatectomía/efectos adversos , Infección de la Herida Quirúrgica/prevención & control , Resultado del Tratamiento , Incontinencia Urinaria/etiología
6.
Anal Sci ; 40(4): 755-763, 2024 Apr.
Artículo en Inglés | MEDLINE | ID: mdl-38379121

RESUMEN

The primary aim of the present investigation was to evaluate the efficiency of pure zeolite and activated dithizone zeolite for arsenic(V) removal from aqueous solutions. The analytical eco-scale and analytical greenness for sample preparation results confirm that the proposed method is environmentally friendly. Zeolite adsorbents were characterized and tested for their ability to adsorb arsenic(V) from wastewater. Our study delved into arsenic(V) sorption behavior on pristine and activated zeolites. Through steady-state experiments using pure zeolite and activated dithizone zeolite, we examined the sorption of arsenic from aqueous solutions. We optimized operational parameters, including pH, adsorbent dosage, contact time, and arsenic(V) concentration. Our findings revealed that the Langmuir and Freundlich adsorption isothermal models were highly influential in fitting the experimental data, resulting in statistically significant outcomes. This study highlights the potential of zeolites as outstanding adsorbents for removing arsenic(V) from aqueous solutions. The calculated maximum adsorption capacity (qmax) of pure zeolite and activated dithizone zeolite was 18.2 and 21.1(mg/g), respectively, with R2 = 0.999. According to Freundlich's linear model, the experimental isothermal data indicated that activated dithizone zeolite has a higher value of kf constant and a lower value of the 1/n constant than that obtained for pure zeolite. These results imply favorable adsorption of arsenic(V) on activated dithizone zeolite.

7.
Future Med Chem ; 16(7): 647-663, 2024 04.
Artículo en Inglés | MEDLINE | ID: mdl-38385167

RESUMEN

Aim: This study focuses on advancing green chemistry in anticancer drug discovery, particularly through the synthesis of azine derivatives with a naphthalene core using CS-SO3H as a catalyst. Methods: Novel benzaldazine and ketazine derivatives were synthesized using (E)-(naphthalen-1-ylmethylene)hydrazine and various carbonyl compounds. The methods employed included thermal and grinding techniques, utilizing CS-SO3H as an eco-friendly and cost-effective catalyst. Results: The approach resulted in high yields, short reaction times and demonstrated catalyst reusability. Cytotoxicity tests highlighted compounds 3b, 11 and 13 as potent against the HEPG2-1. Conclusion: This study successfully aligns with the objectives of eco-conscious drug development in organic chemistry. Molecular docking and in silico studies further indicate the potential of these ligands as antitumor medicines, with favorable oral bioavailability properties.


Asunto(s)
Antineoplásicos , Quitosano , Simulación del Acoplamiento Molecular , Antineoplásicos/química , Naftalenos/farmacología , Catálisis
8.
J Contam Hydrol ; 264: 104364, 2024 May.
Artículo en Inglés | MEDLINE | ID: mdl-38749070

RESUMEN

The increase in antibiotic residues poses a serious threat to ecological and aquatic environments, necessitating the development of cost-effective, convenient, and recyclable adsorbents. In our study, we used cellulose-based layered double hydroxide (LDH) as an efficient adsorbent and nanocarrier for both sulfamethoxazole (SMX) and cefixime (CFX) residues due to their biodegradability and biocompatibility. Chemical processes are measured according to green chemistry metrics to identify which features adhere to the principles. A GREEnness Assessment (ESA), Analytical GREEnness Preparation (AGREEprep), and Analytical Eco-Scale Assessments (ESA) were used to assess the suitability of the proposed analytical method. We extensively analyzed the synthesized CoFe LDH/cellulose before and after the adsorption processes using XRD, FTIR, and SEM. We investigated the factors affecting the adsorption process, such as pH, adsorbent dose, concentrations of SMX and CFX and time. We studied six nonlinear adsorption isotherm models at pH 5 using CoFe LDH, which showed maximum adsorption capacities (qmax) of 272.13 mg/g for SMX and 208.00 mg/g for CFX. Kinetic studies were also conducted. The 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyl-2H-tetrazolium bromide (MTT) assay was performed on Vero cells in direct contact with LDH nanocomposites to evaluate the cytotoxicity and side effects of cellulose-based CoFe LDH. The cellulose-based CoFe LDH nanocomposite demonstrated excellent cytocompatibility and less cytotoxic effects on the tested cell line. These results validate the potential use of these unique LDH-based cellulose cytocompatible biomaterials for water treatment applications. The cost of the prepared adsorbents was investigated.


Asunto(s)
Cefixima , Celulosa , Sulfametoxazol , Contaminantes Químicos del Agua , Celulosa/química , Sulfametoxazol/química , Sulfametoxazol/toxicidad , Adsorción , Contaminantes Químicos del Agua/química , Contaminantes Químicos del Agua/toxicidad , Animales , Cefixima/química , Antibacterianos/química , Antibacterianos/toxicidad , Células Vero , Hidróxidos/química , Chlorocebus aethiops , Nanocompuestos/química , Nanocompuestos/toxicidad , Tecnología Química Verde/métodos
9.
J Chromatogr Sci ; 61(8): 705-716, 2023 Oct 03.
Artículo en Inglés | MEDLINE | ID: mdl-35876214

RESUMEN

In patients with Type 2 diabetes, a combination of Alogliptin and Pioglitazone medications, together with diet and physical activity, are used to improve glycemic control. Eco-friendly, cost-effective, and precise stability-indicating RP-HPLC method was developed and validated for the identification and quantification of Alogliptin and Pioglitazone in their tablet dosage form, as well as implementation to in vitro dissolution studies and uniformity of dosage unit. Isocratic separation is conducted at ambient temperature on the InertSustain C18 Analytical Column (150 × 4.6 mm, 5 µm) using mobile phase comprising 50 mM of ammonium dihydrogen phosphate and 5.0 mM of heptane sulfonic acid:acetonitrile (45:55, v/v) at a flow rate of 1.3 mL/minute. Calibration curves are conducted in the linearity range of 1-40 µg/mL of Alogliptin and 2.5-75 µg/mL of Pioglitazone with a correlation value >0.9995 and satisfactory recovery findings between 99 and 100%. The degraded samples are analyzed under relevant stress conditions as acidity, alkalinity, thermal and oxidation. The active components in finished products were subjected to a content uniformity test, which showed that they achieved the declared claim's acceptance standards (85-115%). Comparative in vitro dissolution studies are performed for generic products Inhibazone 12.5/30 mg FCT and Inhibazone 25/15 mg FCT against innovator products Oseni 12.5/30 mg FCT and Oseni 25/15 mg FCT at suitable FDA dissolution medium and different USP dissolution media and the results are similar. The metrics of the designed method were assessed according to ICH requirements, and all metrics, such as system suitability, linearity, recovery, robustness, LOD, LOQ, specificity and precision, were found to be within required tolerances and no overlapping was found for degradation peaks. Thence, the method can be used in quality control for the analysis of raw material, bulk, finish and stability.


Asunto(s)
Diabetes Mellitus Tipo 2 , Hipoglucemiantes , Humanos , Estabilidad de Medicamentos , Hipoglucemiantes/análisis , Pioglitazona , Solubilidad , Comprimidos
10.
J AOAC Int ; 106(5): 1165-1179, 2023 Sep 01.
Artículo en Inglés | MEDLINE | ID: mdl-37341634

RESUMEN

BACKGROUND: Antihypertensives bisoprolol fumarate (BIS) and perindopril arginine (PER) were simultaneously determined in their pure, bulk, and combined tablet dosage form. OBJECTIVE: This study develops a novel, reproducible, and accurate Reversed phase high-performance liquid chromatography (RP-HPLC) and Reversed phase ultra-performance liquid chromatography (RP-UPLC) with photodiode array detection techniques, which were then applied to in vitro dissolution studies. METHODS: The first RP-HPLC method relied on isocratic elution using a mobile phase of methanol-0.05 M phosphate buffer pH 2.6 (1 + 1, by volume), and separation was performed using a Thermo Hypersil C8 column (150 mm × 4.6 mm, 5 µm). Ion-pair UPLC was the second method. An acceptable resolution was achieved using an RP-C18 chromatographic column, Agilent Eclipse (100 × 2.1 mm, 1.7 µm), with a mobile phase containing 0.005 M sodium 1-heptane sulfonate-triethylamine (64 + 1 + 35, by volume), adjusted with phosphoric acid to a pH of 2.0. RP-HPLC used a 1.0 mL/min flow rate, while UPLC used 0.5 mL/min, and the two methods used detection at 210 nm. RESULTS: Calibration curves of BIS and PER were linear for RP-HPLC and RP-UPLC methods at 0.5-15 and 0.5-40 µg/mL, respectively. BIS and PER had RP-UPLC LODs of 0.22 and 0.10 µg/mL, respectively, and LOQs of 0.68 and 0.31 µg/mL, respectively. As a result, the approach has been effectively applied to in vitro dissolution testing for drugs in generic and reference products, showing that the two products are comparable. The Six Sigma approach was implemented to compare the recommended and United States Pharmacopeia (USP) procedures, which both exhibited process capability index (Cpk) >1.33. A content uniformity test demonstrated that the drugs in their dosage form met the acceptance limit (85-115%). The degradation products were reliably distinguished from pure drugs for a range of retention times. CONCLUSION: In their commercial drug product, the proposed method could be used in QC laboratories for concurrent testing, content uniformity, and in vitro dissolution investigations of BIS and PER. The methods were successfully validated per International Council for Harmonisation (ICH) guidelines. HIGHLIGHTS: This study is innovative since it is the first to establish and validate specific and reproducible UPLC and HPLC methods for the concurrent quantitation of the studied drugs in their binary mixture and application to lean Six Sigma, content uniformity, and comparative dissolution approaches.


Asunto(s)
Bisoprolol , Perindopril , Arginina , Bisoprolol/análisis , Perindopril/análisis , Solubilidad , Gestión de la Calidad Total
11.
Sci Rep ; 13(1): 17613, 2023 10 17.
Artículo en Inglés | MEDLINE | ID: mdl-37848502

RESUMEN

Investigation of a unique and fast method for the determination and separation of a mixture of three drugs viz., ciprofloxacin (CIP), Ibuprofen (IBU), and diclofenac sodium (DIC) in actual samples of human plasma. Also, the technique was used to look at their pharmacokinetics study. Hydrocortisone was chosen as the internal standard (IS). The drugs were chromatographically separated using an Acquity ultra-performance liquid chromatography UPLC ® BEH C18 1.7 µm (2.1 × 150 mm) column with a mobile phase composed of acetonitrile: water (65:35, v/v) adjusted to pH 3 with diluted acetic acid. Plasma proteins were precipitated with acetonitrile. The separated drugs ranged from 0.3 to 10, 0.2-11, and 1-25 µg/mL for CIP, IBU, and DIC, respectively. Calibration curves were discovered to achieve linearity with acceptable correlation coefficients (0.99%). Examination of quality assurance samples showed exceptional precision and accuracy. Following the successful application of this improved technique to plasma samples, the pharmacokinetic characteristics of each selected drug were evaluated using (UPLC) with UV detection at 210 nm. Two green metrics were applied, the Analytical Eco-scale and the Analytical GREEnness Calculator (AGREE). Separation was achieved in only 4-min analysis time. The method's validation agreed with the requirements of the FDA, and the results were sufficient.


Asunto(s)
Diclofenaco , Ibuprofeno , Humanos , Cromatografía Líquida de Alta Presión/métodos , Ciprofloxacina , Espectrometría de Masas en Tándem/métodos , Reproducibilidad de los Resultados , Acetonitrilos
12.
BMC Chem ; 17(1): 136, 2023 Oct 10.
Artículo en Inglés | MEDLINE | ID: mdl-37817268

RESUMEN

Economical, highly robust, selective, precise, and eco-friendly RP-UPLC and spectrophotometric methods were developed and validated for the concurrent estimation of selected pharmaceutical drugs represented in ceftazidime (CFZ) and pyridine (PYD) in their solutions using Agilent Zorbax SB-C18 RRHD (50 × 2.1 mm, 1.8 µm) column at flow rate 0.3 mL/min with wavelength 254 nm. Box-Behnken design (BBD) established Response surface methodology (RSM) to achieve the optimum chromatographic condition with minimal trials conducted. Three independent variables specifically acetonitrile ratio 60-70%, pH 3-7, and temperature 25-35 °C were implemented to evaluate the influences of these variables on the responses as resolution and retention time. Desirability and overlay plots were carried out to adjust the optimal condition that achieved the shortest retention time of less than 2 min and desired resolution of more than 1.5 using a mobile phase consisting of acetonitrile: purified water (70:30, v/v) at pH 5.0 adjusted by 0.1% orthophosphoric acid with the column oven temperature 30 °C and column void volume 0.46 mL. Mean centering of ratio spectra (MCR) and ratio subtraction (RS) methods were effectively applied to resolve drugs' spectral superposition at 220 nm, 255.4 nm, 260.3 nm, and 254.6 nm for CFZ and PYD, respectively. Linearity range was accomplished for UPLC, MCR, and RS methods over the concentration range of 2-100, 1-50,3-30 and 5-30 µg/mL for CFZ and PYD, respectively with correlation coefficient > 0.999 and good recovery results within 98-102%. Six Sigma methodology was achieved using the process capability index (Cpk) to compare the suggested and USP methods showing that both are highly capable with Cpk > 1.33. The proposed method was successfully validated depending on ICH guidelines and ANOVA results and applied for the accelerated stability study.

13.
J AOAC Int ; 105(3): 703-716, 2022 Apr 27.
Artículo en Inglés | MEDLINE | ID: mdl-35015880

RESUMEN

BACKGROUND: A combination of paracetamol, pseudoephedrine, chlorpheniramine, and sodium benzoate in (Cold-Flu) 1,2,3 Syrup dosage form is specified for the treatment of common cold and flu symptoms. OBJECTIVE: The functional role of this study is to develop a novel, reliable, and selective stability-indicating reversed-phase ultra-performance liquid chromatography (RP-UPLC) method for simultaneous identification of a quaternary mixture of paracetamol, pseudoephedrine, chlorpheniramine, and sodium benzoate in (Cold-Flu) 1,2,3 Syrup dosage form. METHOD: The specific method is accomplished using an Acquity UPLC HSS T3 C18 column (2.1 mm × 100 mm), 1.8 µm particle size with pore size 100 Å, utilizing a mixture of purified water-methanol-trifluoroacetic acid (72.5:27.5:1.5, v/v) as the mobile phase at a flow rate of 0.3 mL/min. The column void volume is 1.15 min. UPLC detection is adjusted at 205 nm using a photodiode array detector. RESULTS: Calibration curves are obtained in the linearity ranges: 25-500 µg/mL for paracetamol, 10-50 µg/mL for pseudoephedrine, 0.5-5 µg/mL for chlorpheniramine, and 3-30 µg/mL for sodium benzoate with a correlation coefficient > 0.9992. The mean recovery of the developed method is tested and shows good recovery results between 99-101%; selectivity and forced degradation studies are investigated as per the International Council for Harmonisation Guidelines and no interference is detected due to degradation peaks. CONCLUSION: The proposed stability-indicating UPLC method for simultaneous determination of the three drugs, paracetamol, pseudoephedrine, and chlorpheniramine, with a preservative sodium benzoate in (Cold-Flu) 1,2,3 Syrup dosage form is successfully accomplished, developed, and validated, and can be easily used in the analysis of drugs in pure or dosage form. HIGHLIGHTS: The novelty of the current research work lies in the development of the UPLC method for simultaneous determination of a quaternary mixture of paracetamol, pseudoephedrine, chlorpheniramine, and sodium benzoate in (Cold-Flu) 1,2,3 Syrup dosage form.


Asunto(s)
Clorfeniramina , Resfriado Común , Acetaminofén/análisis , Clorfeniramina/análisis , Cromatografía Líquida de Alta Presión/métodos , Humanos , Seudoefedrina/análisis , Benzoato de Sodio/análisis
14.
Int J Biol Macromol ; 205: 385-395, 2022 Apr 30.
Artículo en Inglés | MEDLINE | ID: mdl-35183600

RESUMEN

The current study explores the effect of the extracted novel Mushroom polysaccharides and its formulation onto Alginate (Alg.)/kappa carrageenan microcapsules to exert immunotherapeutic effect upon activating gut resident natural killer cells (NK) against colon cancer. The extracted polysaccharides of Agaricus bisporus MH751906 was microcapsulated in Alg/κ-carrageenan microcapsules as an oral delivery system for colon cancer. The microcapsule is characterized by SEM, FTIR, Raman and TGA; and showed a superior acidic stability, controlled release, and thermal stability at high temperature with higher hydrogel swelling rate in colon-mimicking pH. Upon activation of human NK cells with microcapsules (ANK cells), a significant increase in CD16+CD56+ NK cell populations were recorded. These activated NK cells showed 74.09% cytotoxic effects against human colon cancer Caco-2 cells where majority of cancer cell populations arrested at G0/G1 phase leading to apoptosis. The apoptotic molecular mechanism induced by ANK cells on Caco-2 treated cells is through down regulations of both BCL2 and TGF surviving genes and up regulation in IkappaB-α gene expression. Therefore, this novel polysaccharides-alginate/κ-carrageenan microcapsules can be used as an oral targeted delivery system for colon cancer immunotherapy.


Asunto(s)
Agaricus , Neoplasias del Colon , Agaricus/química , Alginatos/química , Células CACO-2 , Cápsulas , Carragenina/química , Neoplasias del Colon/tratamiento farmacológico , Humanos , Inmunoterapia , Células Asesinas Naturales , Polisacáridos/química
15.
ACS Omega ; 7(31): 27239-27248, 2022 Aug 09.
Artículo en Inglés | MEDLINE | ID: mdl-35967052

RESUMEN

Water polluted by phenolic compounds is a global threat to health and the environment; accordingly, we prepared a green novel sorbent biological system from a chitosan (CS), gelatin (GT), and Chlorella vulgaris freshwater microalgae (m-Alg) composite impregnated with zinc oxide nanoparticles (ZnO-NPs) for the remediation of bisphenol-A (BPA) from water. C. vulgaris was selected to be one of the constituents of the prepared composite because of its high capability in phytoremediation. The morphology and the structure of CS/GT*m-Alg/ZnO beads were characterized by SEM, FTIR, XRD, and TGA. Different monitoring experimental conditions, such as contact time, pH, BPA concentration, and sorbent dosage, were optimized. The optimum conditions for the adsorption process showed outstanding removal efficiency toward BPA at pH 4.0, contact time 40.0 min, and 40.0 mg L-1 BPA initial concentration. Langmuir, Freundlich, and Temkin isotherm models have been studied for adsorption equilibrium, and the best fit is described by the Langmuir adsorption isotherm. The adsorption kinetics has been studied using pseudo-first-order (PFO), pseudo-second-order (PSO), Elovich, and intraparticle diffusion (IPD) models. The pseudo-second-order kinetic model shows the optimum experimental fit. The monolayer adsorption capacity of the prepared CS/GT*m-Alg/ZnO for BPA was determined to be 38.24 mg g-1. The prepared CS/GT*m-Alg/ZnO beads show advantageous properties, such as their high surface area, high adsorption capacity, reusability, and cost-effectiveness.

16.
Animals (Basel) ; 9(7)2019 Jul 22.
Artículo en Inglés | MEDLINE | ID: mdl-31336620

RESUMEN

The present study was conducted to examine that impact of dietary xylanase (Xyl) and arabinofuranosidase (Abf) supplementation on the performance, protein and fat digestibility, the lipid peroxidation, the plasma biochemical traits, and the immune response of broilers. A total of 480, un-sexed, and one-day-old broilers (Ross 308) were randomly divided into three treatments with eight replicates, where chicks in the first treatment were fed basal diets and served as the control, chicks in the second treatment were fed diets formulated with reductions of 90 kcal/kg, and chicks in the third treatment were fed the same formulated diets used in the second group as well as the Xyl and Abf combination (Rovabio® Advance). Feed intake was decreased by the low energy diet, leading to an enhancement in feed efficiency enzyme supplementation in the low energy diet (p < 0.015). Both protein and fat digestibility were improved (p < 0.047) due to enzyme supplementation. Moreover, enzyme supplementation increased muscle total lipids content and decreased muscle thiobarbituric acid retroactive substance content. Furthermore, diets supplemented with Xyl and Abf exhibited an increase in antibody titers against the Newcastle disease virus (p < 0.026). In addition, enzyme supplementation increased gene expression related to growth and gene expression related to fatty acid synthesis. It could be concluded that dietary Xyl and Abf supplementation had beneficial impacts on growth, nutrient digestibility, lipid peroxidation, immune response, and gene expressions related to growth and fatty acid synthesis in broiler chickens fed low-energy diets.

17.
J Agric Food Chem ; 55(2): 204-10, 2007 Jan 24.
Artículo en Inglés | MEDLINE | ID: mdl-17227043

RESUMEN

Monitoring of water resources for pesticide residues is often needed to ensure that pesticide use does not adversely impact the quality of public water supplies or the environment. In many rural areas and throughout much of the developing world, monitoring is often constrained by lack of testing facilities; thus, collection of samples and shipment to centralized laboratories for analysis is required. The portability, ease of use, and potential to enhance analyte stability make solid-phase extraction (SPE) an attractive technique for handling water samples prior to their shipment. We describe performance of an SPE method targeting a structurally diverse mixture of 25 current-use pesticides and two common degradates in samples of raw and filtered drinking water collected in Greater Cairo, Egypt. SPE was completed in a field laboratory in Egypt, and cartridges were shipped to the United States for elution and high-performance liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry analysis. Quantitative and reproducible recovery of 23 of 27 compounds (average = 96%; percent relative standard deviation = 21%) from matrix spikes (1 microg L-1 per component) prepared in the field and from deionized water fortified similarly in the analytical laboratory was obtained. Concurrent analysis of unspiked samples identified four parent compounds and one degradate in drinking water samples. No significant differences were observed between raw and filtered samples. Residue levels in all cases were below drinking water and "harm to aquatic-life" thresholds, indicating that human and ecological risks of pesticide contamination were relatively small; however, the study was limited in scale and scope. Further monitoring is needed to define spatial and temporal variation in residue concentrations. The study has demonstrated the feasibility of performing studies of this type using SPE to extract and preserve samples in the field. The approach should be broadly applicable in many settings.


Asunto(s)
Cromatografía Líquida de Alta Presión/métodos , Espectrometría de Masas/métodos , Plaguicidas/análisis , Abastecimiento de Agua/análisis , Agua/química , Egipto , Residuos de Plaguicidas/análisis , Medición de Riesgo
18.
Artículo en Inglés | MEDLINE | ID: mdl-25965516

RESUMEN

New vanadium(IV) and chromium(III) complexes of metformin (MFN) were synthesized upon the chemical interaction between vanadyl(II) sulfate monohydrate or chromium(III) chloride hexahydrate with metformin diabetic drug in the media of a pure grade of methanol solvent. The [(VO)2(MFN)2(SO4)2]2H2O and [Cr(MFN)3]·Cl3·6H2O complexes were discussed using microanalytical measurements, molar conductance, spectroscopic (infrared, ESR, XRD, and UV-vis), effective magnetic moment, scanning electron microscopy (SEM), and thermal analyses (TG/DTG). The elemental analysis shows that VO(II) and Cr(III) complexes were associated with 1:1 and 1:3M ratios, respectively. The infrared spectroscopic results data received from the comparison between free MFN free ligand and their vanadyl(II) and chromium(III) complexes were proven that metformin reacted with respected metal ions as a bidentate ligand through its two imino groups. The kinetic thermodynamic parameters were estimated from the DTG curves. The microstructure changes of the VO(II) and Cr(III) complexes have been probed using positron annihilation lifetime (PAL) and positron annihilation Doppler broadening (PADB) techniques. The PAL and PADB line-shape parameters were found to be dependent on the structure, electronic configuration and molecular weight of metal complexes. Antimicrobial activity of the metformin free ligand and its vanadyl(II) and chromium(III) complexes were evaluated against the gram negative and gram positive bacteria strains and different fungal strains. Moderate antimicrobial activity recorded by disk diffusion inhibition growth zone method in vanadyl(II) and chromium(III) complexes compared to metformin free ligand.


Asunto(s)
Antiinfecciosos/química , Cromo/química , Complejos de Coordinación/química , Metformina/análogos & derivados , Vanadio/química , Antiinfecciosos/síntesis química , Antiinfecciosos/farmacología , Infecciones Bacterianas/tratamiento farmacológico , Cromo/farmacología , Complejos de Coordinación/síntesis química , Complejos de Coordinación/farmacología , Hongos/efectos de los fármacos , Humanos , Metformina/síntesis química , Metformina/farmacología , Pruebas de Sensibilidad Microbiana , Micosis/tratamiento farmacológico , Vanadio/farmacología
19.
Dalton Trans ; 44(31): 14110-21, 2015 Aug 21.
Artículo en Inglés | MEDLINE | ID: mdl-26172408

RESUMEN

A series of copper(ii) complexes, viz. [Tp(MeMe)Cu(Cl)(H2O)] (), [Tp(MeMe)Cu(OAc)(H2O)] (), [Tp(MeMe)Cu(NO3)] () and [Tp(MeMe)Cu(ClO4)] () containing tris(3,5-dimethylpyrazolyl)borate (KTp(MeMe)), have been synthesized and fully characterized. The substitution reaction of with thiourea was studied under pseudo-first-order conditions as a function of concentration, temperature and pressure in methanol and acetonitrile as solvents. Two reaction steps that both depended on the nucleophile concentration were observed for both solvents. Substitution of coordinated methanol is about 40 times faster than the substitution of chloride. In acetonitrile, the rate constant for the displacement of coordinated acetonitrile was more than 20 times faster than the substitution of chloride. The reported activation parameters indicate that both reaction steps follow a dissociative mechanism in both solvents. On going from methanol to acetonitrile, the rate constant for the displacement of the solvent becomes more than 200 times faster due to the more labile acetonitrile, but the substitution mechanism remained to have a dissociative character. The antioxidant activities of were evaluated for superoxide dismutase (SOD), glutathione-s-transferase (GST0 and glutathione reduced (GSH-Rd) activity. and were found to show (p < 0.05) the highest antioxidant activity in comparison to and , which can be ascribed to the geometric configuration as well as the nature of the co-ligand. showed catechol oxidase activity with turnover numbers of 20 min(-1) and a coordination affinity for 3,5-DTBC of K1, = 31 mM(-1). K1 is rather large and seems to be typical for faster biomimetic models, and also for the enzyme itself (25 mM(-1)). The reaction rate depended linearly on the complex concentration, indicating a first-order dependence on the catalyst concentration.


Asunto(s)
Antioxidantes/metabolismo , Materiales Biomiméticos/química , Boratos/química , Cobre/química , Compuestos Organometálicos/química , Oxidorreductasas/metabolismo , Pirazoles/química , Catálisis , Catecol Oxidasa/metabolismo , Cinética , Ligandos , Oxidación-Reducción , Análisis Espectral , Termodinámica
20.
Eur J Med Chem ; 44(9): 3519-23, 2009 Sep.
Artículo en Inglés | MEDLINE | ID: mdl-19398146

RESUMEN

Cyclocondensation of cyanoacetamide, cyanothioacetamide and 3-aminopyrazols with sodium salt of 3-hydroxy-1-(2-naphthyl)prop-2-en-1-one gives pyridin-2-one, pyridin-2(1H)-thione, and pyrazolo[1,5-a]pyrimidine derivatives. These derivatives showed potent anti-tumor cytotoxic activity in vitro using different human cancer cell lines.


Asunto(s)
Antineoplásicos/síntesis química , Antineoplásicos/farmacología , Pirazoles/síntesis química , Pirazoles/farmacología , Piridinas/síntesis química , Piridinas/farmacología , Pirimidinas/síntesis química , Pirimidinas/farmacología , Antineoplásicos/química , Línea Celular Tumoral , Supervivencia Celular/efectos de los fármacos , Ensayos de Selección de Medicamentos Antitumorales , Humanos , Estructura Molecular , Pirazoles/química , Piridinas/química , Pirimidinas/química , Relación Estructura-Actividad
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