RESUMEN
Bilayer pseudo-stationary phase micellar liquid chromatography (MLC) was developed for simultaneous isocratic isolation of hydrochlorothiazide, as a basic-polar (hydrophilic) cardiovascular drug, as well as triamterene and losartan potassium, as acidic-nonpolar (hydrophobic) cardiovascular drugs. Utilizing a deep eutectic solvent (DES), as a novel green mobile phase additive in combination with acetonitrile (ACN) and acetic acid (ACA), drastically improved the chromatographic behavior of the drugs. Concentration of sodium dodecyl sulphate (SDS), as well as volume percentages of ACN, DES, and ACA were optimized by using a central composite design. The optimal composition of the mobile phase (0.12â¯molâ¯L-1 SDS, 5% ACN, 4% DES, and 2% ACA) was chosen through the desirability function. The chromatographic peaks of both hydrophilic and hydrophobic drugs, respectively, emerged at high and low retention time values in the shortest total analysis time of 20â¯min (at a flow rate of 2â¯mLâ¯min-1). Analytical characterization of the developed approach was investigated through Food and Drug Administration (FDA) guidelines. Applicability of the method was evaluated by analysing of human plasma samples which were directly injected into the system.
Asunto(s)
Fármacos Cardiovasculares/aislamiento & purificación , Hidroclorotiazida/aislamiento & purificación , Losartán/aislamiento & purificación , Proyectos de Investigación , Triantereno/aislamiento & purificación , Fármacos Cardiovasculares/sangre , Fármacos Cardiovasculares/química , Cromatografía Líquida de Alta Presión , Humanos , Hidroclorotiazida/sangre , Hidroclorotiazida/química , Interacciones Hidrofóbicas e Hidrofílicas , Losartán/sangre , Losartán/química , Micelas , Programas Informáticos , Triantereno/sangre , Triantereno/química , Estados Unidos , United States Food and Drug AdministrationRESUMEN
This paper reports the applicability of two-phase and three-phase hollow fiber based liquid-phase microextraction (HF-LPME) for the extraction of hydrochlorothiazide (HYD) and triamterene (TRM) from human urine. The HYD in two-phase HF-LPME is extracted from 24 mL of the aqueous sample into an organic phase with microliter volume located inside the pores and lumen of a polypropylene hollow fiber as acceptor phase, but the TRM in three-phase HF-LPME is extracted from aqueous donor phase to organic phase and then back-extracted to the aqueous acceptor phase, which can be directly injected into HPLC for analysis. Under optimized conditions preconcentration factors of HYD and TRM were obtained as 128 and 239, respectively. The calibration curves were linear (R(2) ≥ 0.995) in the concentration range of 1.0-100 µg/L for HYD and 2.0-100 µg/L for TRM. The limits of detection for HYD and TRM were 0.5 µg/L. The intra-day and inter-day RSD based on four replicates were obtained as ≤5.8 and ≤9.3%, respectively. The methods were successfully applied for determining the concentration of the drugs in urine samples. Copyright © 2015 John Wiley & Sons, Ltd.
Asunto(s)
Diuréticos/aislamiento & purificación , Hidroclorotiazida/aislamiento & purificación , Microextracción en Fase Líquida/métodos , Triantereno/aislamiento & purificación , Diuréticos/orina , Humanos , Hidroclorotiazida/orina , Triantereno/orinaRESUMEN
Through precipitation polymerization, three monodisperse molecularly imprinted polymers (MIPs) containing imprints of 2,4-diamino-6-methyl-1,3,5-triazine (DM), cyromazine (CY) or trimethoprim (TM), were synthesized using methacrylic acid as functional monomer, divinylbenzene as cross-linker, and a mixture of acetonitrile-toluene (90/10, v/v) as porogen. The morphology and selectivity of the MIPs were characterized and compared systematically. The MIPs had the best specific binding in pure acetonitrile, and the data of adsorption experiment were fitted well with Langmuir and Freundlich model. In addition, DM-MIPs showed the excellent binding and multi-recognition capability for CY, melamine (ME), triamterene (TA) and TM, and the binding capacity were 7.18, 7.56, 5.66 and 5.45µmol/g, respectively. Due to the pseudo template and the ability of multi-recognition, DM-MIPs as sorbent material could avoid the effect of template leakage on quantitative analysis. Therefore, DM-MIPs were used as a solid-phase extraction material to enrich ME, CY, TA and TM from different bio-matrix samples for high performance liquid chromatography analysis. Under the optimized conditions, the recoveries of three spiked levels in different bio-matrix samples were ranged from 80.9% to 91.5% with RSD≤4.2 (n=3).
Asunto(s)
Microesferas , Polimerizacion , Triantereno/aislamiento & purificación , Triazinas/aislamiento & purificación , Trimetoprim/aislamiento & purificación , Humanos , Límite de Detección , Microscopía Electrónica de Rastreo , Triantereno/orina , Triazinas/orina , Trimetoprim/orinaRESUMEN
A tandem solid-phase extraction method (SPE) of connecting two different cartridges (C(18) and MCX) in series was developed as the extraction procedure in this article, which provided better extraction yields (>86%) for all analytes and more appropriate sample purification from endogenous interference materials compared with a single cartridge. Analyte separation was achieved on a C(18) reversed-phase column at the wavelength of 265 nm by high-performance liquid chromatography (HPLC). The method was validated in terms of extraction yield, precision and accuracy. These assays gave mean accuracy values higher than 89% with RSD values that were always less than 3.8%. The method has been successfully applied to plasma samples from rats after oral administration of target compounds.