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1.
Int J Pharm ; 655: 124058, 2024 Apr 25.
Artículo en Inglés | MEDLINE | ID: mdl-38552754

RESUMEN

Polypharmacy is a common issue, especially among elderly patients resulting in administration errors and patient inconvenience. Hypertension is a prevalent health condition that frequently leads to polypharmacy, as its treatment typically requires the co-administration of more than one different Active Pharmaceutical Ingredients (API's). To address these issues, floating hollow torus-shaped dosage forms were developed, aiming at providing prolonged gastric retention and sustained drug release. The dosage forms (polypills) containing three anti-hypertensive API's (diltiazem (DIL), propranolol (PRP) and hydrochlorothiazide (HCTZ)) were created via Fused Deposition Modelling 3D printing. A multitude of the dosage forms were loaded into a capsule and the resulting formulation achieved prolonged retention times over a 12-hour period in vitro, by leveraging both the buoyancy of the dosage forms, and the "cheerios effect" that facilitates the aggregation and retention of the dosage forms via a combination of surface tension and shape of the objects. Physicochemical characterization methods and imaging techniques were employed to investigate the properties and the internal and external structure of the dosage forms. Furthermore, an ex vivo porcine stomach model revealed substantial aggregation, adhesion and retention of the 3D printed dosage forms in porcine stomach. In vitro dissolution testing demonstrated almost complete first-order release of PRP and DIL (93.52 % and 99.9 %, respectively) and partial release of HCTZ (65.22 %) in the 12 h timeframe. Finally, a convolution-based single-stage approach was employed in order to predict the pharmacokinetic (PK) parameters of the API's of the formulation and the resemblance of their PK behavior with previously reported data.


Asunto(s)
Antihipertensivos , Diltiazem , Humanos , Anciano , Preparaciones de Acción Retardada/química , Comprimidos/química , Liberación de Fármacos , Hidroclorotiazida , Impresión Tridimensional , Tecnología Farmacéutica/métodos
2.
J Chromatogr A ; 1717: 464674, 2024 Feb 22.
Artículo en Inglés | MEDLINE | ID: mdl-38290172

RESUMEN

In this research, a sol-gel Carbowax 20M-zwitterionic ionic liquid composite sorbent-based capsule phase microextraction (CPME) device was developed in combination with liquid chromatography-post column derivatization for the first ever reported determination of a somatostatin analogue - lanreotide in human urine. The sol-gel Carbowax 20M-zwitterionic ionic liquid composite sorbent was encapsulated in the lumen of a polypropylene capillary tube and characterized by FT-IR spectroscopy and SEM with energy dispersive X-ray spectroscopy (EDS). The main steps of the CPME workflow were optimized to obtain high extraction efficiency for the target analyte. After the separation of the analyte on a C8 stationary phase, the peptide was derivatized online with o-phthalaldehyde before the fluorescence detection. The main experimental parameters of CPME and the post-column procedures were systematically investigated and optimized. The method was validated in terms of selectivity, linearity, accuracy, precision, limits of detection (LOD), and limits of quantification (LOQ). The relative bias ranged between 88.8 and 115.6 % for the peptide, while the RSD values for repeatability and intermediate precision were less than 14.3 %. The achieved limit of detection (LOD) was 0.2 µΜ while the limit of quantitation (LOQ) was established as 0.9 µΜ. Finally, the sol-gel Carbowax 20M-zwitterionic ionic liquid composite sorbent-based microextraction capsules were found to be reusable for at least 20 extractions. The developed method presented adequate overall performance, and it could be applied in the analysis of selected peptide in human urine samples.


Asunto(s)
Líquidos Iónicos , Microextracción en Fase Líquida , Somatostatina/análogos & derivados , Humanos , Cromatografía Líquida de Alta Presión/métodos , Polietilenglicoles , Líquidos Iónicos/química , Espectroscopía Infrarroja por Transformada de Fourier , Microextracción en Fase Sólida/métodos , Péptidos Cíclicos , Límite de Detección
3.
Molecules ; 28(20)2023 Oct 14.
Artículo en Inglés | MEDLINE | ID: mdl-37894565

RESUMEN

Homotaurine (HOM) is considered a promising drug for the treatment of Alzheimer's and other neurodegenerative diseases. In the present work, a new high-performance liquid chromatography with fluorescence detection (HPLC-FLD) (λex. = 340 nm and λem. = 455 nm) method was developed and validated for the study of substance permeability in the central nervous system (CNS). Analysis was performed on a RP-C18 column with a binary gradient elution system consisting of methanol-potassium phosphate buffer solution (pH = 7.0, 0.02 M) as mobile phase. Samples of homotaurine and histidine (internal standard) were initially derivatized with ortho-phthalaldehyde (OPA) (0.01 M), N-acetylcysteine (0.01 M) and borate buffer (pH = 10.5; 0.05 M). To ensure the stability and efficiency of the reaction, the presence of different nucleophilic reagents, namely (a) 2-mercaptoethanol (2-ME), (b) N-acetylcysteine (NAC), (c) tiopronin (Thiola), (d) 3-mercaptopropionic acid (3-MPA) and (e) captopril, was investigated. The method was validated (R2 = 0.9999, intra-day repeatability %RSD < 3.22%, inter-day precision %RSD = 1.83%, limits of detection 5.75 ng/mL and limits of quantification 17.43 ng/mL, recovery of five different concentrations 99.75-101.58%) and successfully applied to investigate the in vitro permeability of homotaurine using Franz diffusion cells. The apparent permeability (Papp) of HOM was compared with that of memantine, which is considered a potential therapeutic drug for various CNSs. Our study demonstrates that homotaurine exhibits superior permeability through the simulated blood-brain barrier compared to memantine, offering promising insights for enhanced drug delivery strategies targeting neurological conditions.


Asunto(s)
Acetilcisteína , Memantina , Acetilcisteína/química , Cromatografía Líquida de Alta Presión/métodos , o-Ftalaldehído/química , Indicadores y Reactivos , Tiopronina , Reproducibilidad de los Resultados
4.
Bioanalysis ; 15(15): 937-954, 2023 Aug.
Artículo en Inglés | MEDLINE | ID: mdl-37638635

RESUMEN

Microextraction techniques have attracted the attention of many researchers working in the field of bioanalysis due to their unique advantages, mainly in downsizing the scale of sample preparation steps. In parallel, analytical derivatization offers a powerful combination in terms of additional sensitivity, selectivity and compatibility with modern separation techniques. The aim of this review is to discuss the most recent advances in bioanalytical sample preparation based on the combination of microextraction and analytical derivatization. Both innovative fundamental reports and analyte-targeted applications are included and discussed. Dispersive liquid-liquid extraction and solid-phase microextraction are the most common techniques that typically combined with derivatization, while the development of novel and greener protocols is receiving substantial consideration in the field of analytical chemistry.


Asunto(s)
Química Analítica , Extracción Líquido-Líquido , Humanos , Investigadores , Microextracción en Fase Sólida , Manejo de Especímenes
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