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1.
Anal Bioanal Chem ; 412(1): 113-127, 2020 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-31897565

RESUMO

Two solid-phase extraction methods were systematically studied to determine 32 pharmaceuticals and personal care products in water and sediments by ultrahigh-performance liquid chromatography-tandem mass spectrometry. One involves HLB cartridges activated with sodium dodecyl sulfate before the passage of the sample to form an ion pair with cationic analytes, and the other uses mixed HLB-cation exchange cartridges. The accuracy of the sodium dodecyl sulfate method was good for most compounds (recoveries of 61-120% with relative standard deviation less than 23%). However, the recoveries for atorvastatin, codeine, paracetamol, flufenamic acid, and salicylic acid were approximately 50% and for omeprazole and triclocarban were even lower (from 0 to 12%). The detection limits were 1.65-25 ng L-1 in water and 0.33-4.00 ng g-1 (dry weight) in sediment. The recoveries for the mixed-mode cartridge (Strata-X-CW) method ranged from 57% to 120% with relative standard deviation less than 21%, with the exception of codeine [25% (water)], metformin [11% (sediment)], paracetamol [48% (sediment)], and salicylic acid [32% (sediment)]. The detection limits were 1.65-38.35 ng L-1 in water and 0.33-10 ng g-1 (dry weight) in sediment. Both methods followed the same pattern when applied to water. For sediments, the recoveries, which offer good performance, were not very high, although 60% of the compounds had recoveries greater 80%. The methods were applied to the analysis of surface water and sediments from the Albufera Natural Park (Spain). Twenty-seven of 32 analytes were detected in the samples analyzed.


Assuntos
Cromatografia Líquida/métodos , Cosméticos/análise , Sedimentos Geológicos/química , Preparações Farmacêuticas/isolamento & purificação , Espectrometria de Massas em Tandem/métodos , Poluentes Químicos da Água/análise , Limite de Detecção , Reprodutibilidade dos Testes , Extração em Fase Sólida/métodos
2.
Chemosphere ; 238: 124658, 2020 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-31548174

RESUMO

Adsorption is a common process used to remove pharmaceuticals, personal care products and endocrine disrupting chemicals (PPCPs/EDCs) from water. However, as PPCPs/EDCs cover a wide range of molecules and chemical structures, prediction of the adsorption capacity is very challenging. In this study, a novel model was developed to predict adsorption isotherms of PPCPs/EDCs onto various types of adsorbents using a combination of Polanyi potential theory, molecular connectivity indices (MCIs) and molecular characteristics. Polanyi theory provided the basic mathematical form for the correlation. MCIs, hydrophobicity and H-bond count were used to normalize the Polanyi equation based on the molecular structure and interactions among the chemicals, the adsorbents, and the solution. In total, adsorption data were collected from 158 reports for 55 PPCPs/EDCs onto 306 different adsorbent materials. The correlation was first trained with 46 PPCPs/EDCs adsorbed onto 162 carbonaceous adsorbents (CAs), with 44.8% SDEV. Then the model was employed to predict 46 PPCPs/EDCs onto 118 other CAs and 9 new PPCPs/EDCs onto 23 CAs in ultrapure water, with error from 42 to 48% SDEV. When applying to non-carbonaceous adsorbents, the models can still predict the adsorption of PPCPs/EDCs with 90.09% SDEV. For the first time, a model, the PD - MCI - hydrophobic - H bond model, was developed to predict adsorption of a wide group of complicated PPCPs/EDCs onto a big variety of carbonaceous and non-carbonaceous adsorbents. The proposed model approach may provide a simple means for predicting adsorption capacities of PPCPs/EDCs onto various adsorbents.


Assuntos
Cosméticos/isolamento & purificação , Disruptores Endócrinos/isolamento & purificação , Preparações Farmacêuticas/isolamento & purificação , Poluentes Químicos da Água/isolamento & purificação , Purificação da Água/métodos , Adsorção , Disruptores Endócrinos/análise , Interações Hidrofóbicas e Hidrofílicas , Água/química , Poluentes Químicos da Água/análise
3.
J Chromatogr A ; 1608: 460411, 2019 Dec 20.
Artigo em Inglês | MEDLINE | ID: mdl-31405572

RESUMO

In the current study, for the first time, the sugaring-out effect was assessed in a conventional electromembrane extraction (EME) system. Utilizing the sugars in the donor solution as green additives can result in production of a pioneering and influential EME mode. Sugaring-out assisted electromembrane extraction was combined with high-performance liquid chromatography (HPLC) to enhance the extraction of four basic model drugs (pseudoephedrine, lidocaine, propranolol, and ketoconazole). In this mode of EME, not only the transfer of analytes through the supported liquid membrane (SLM) was improved, but also the whole extraction system became more stable than the conventional one in the same voltage. The type and concentration of sugars were optimized in addition to the common experimental parameters influencing the EME, and figures of merit were also studied. Under the optimum conditions, repeatability (RSD%) was obtained in the range of 2.8-6.9% in the water, while RSD value was obtained in the range of 8.2-11.8% (n = 3) for conventional EME with the same state. The linearity range was also in the interval of 5.0-1000.0 ng mL-1 and limits of quantification and detection were in the ranges of 5.0-10.0 ng mL-1 and 1.5-3.0 ng mL-1, respectively, in the introduced EME. Extraction recoveries in the range of 41.2 and 80.8% were obtained resulting in enrichment factors in the range of 96-189. In light of such factor, new suggested EME mode was assessed in the real biological samples including human plasma and urine in order to prove the sugaring-out efficiency in EME systems.


Assuntos
Análise Química do Sangue/métodos , Preparações Farmacêuticas/isolamento & purificação , Açúcares/química , Urinálise/métodos , Cromatografia Líquida de Alta Pressão , Eletrônica , Humanos , Membranas Artificiais , Preparações Farmacêuticas/sangue , Preparações Farmacêuticas/urina
4.
J Chromatogr A ; 1607: 460375, 2019 Dec 06.
Artigo em Inglês | MEDLINE | ID: mdl-31353071

RESUMO

Four amino acid chiral ionic liquids were evaluated in dual systems with hydroxypropyl-ß-cyclodextrin to investigate the enantioseparation by CE of a group of seven drugs as model compounds (duloxetine, verapamil, terbutaline, econazole, sulconazole, metoprolol, and nadolol). The use of two of these chiral ionic liquids (tetramethylammonium L-Lysine ([TMA][L-Lys]) and tetramethylammonium L-glutamic acid ([TMA][L-Glu])) as modifiers in CE is reported for the first time in this work whereas tetrabutylammonium L-lysine ([TBA][L-Lys]) and tetrabutylammonium L-glutamic acid ([TBA][L-Glu]) were employed previously in CE although very scarcely. The effect of the nature and the concentration of each ionic liquid added to the separation buffer containing the neutral cyclodextrin on the enantiomeric resolution and the migration time obtained for each drug, was investigated. A synergistic effect was observed when combining each chiral ionic liquid with hydroxypropyl-ß-cyclodextrin in the case of the five compounds for which the cyclodextrin showed enantiomeric discrimination power when used as sole chiral selector (duloxetine, verapamil, terbutaline, econazole, sulconazole). Buffer concentration and pH, temperature and separation voltage were varied in order to optimize the enantiomeric separation of these five compounds using dual systems giving rise to resolutions ranging from 1.1 to 6.6.


Assuntos
2-Hidroxipropil-beta-Ciclodextrina/química , Aminoácidos/química , Eletroforese Capilar/métodos , Líquidos Iônicos/química , Preparações Farmacêuticas/isolamento & purificação , Tampões (Química) , Ácido Glutâmico/química , Concentração de Íons de Hidrogênio , Estereoisomerismo , Temperatura Ambiente
5.
Int J Biol Macromol ; 136: 469-475, 2019 Sep 01.
Artigo em Inglês | MEDLINE | ID: mdl-31216449

RESUMO

Chitosan-glyoxal/Polyvinylpyrrolidone/MoS2 (CSG/PVP/MoS2) nanocomposites were synthesized via hydrothermal-ultrasonic method. The CSG/PVP/MoS2 nano catalyst was characterized by XRD, UV-visible spectroscopy, FTIR, SEM and X-ray photoelectron spectroscopy, and diclofenac was used for the adsorption and photo-degradation test. SEM revealed the CSG/PVP/MoS2 nanocomposite has coarse and semi-flake structure and UV-vis absorbance spectra indicated its strong UV light response. Additionally, the CSG/PVP/MoS2 presents enhanced adsorption-photocatalytic activities in comparison to CSG/PVP, and the degradation was reaching 94.5%. Kinetic study results demonstrated that the diclofenac photo-degradation could be explained by pseudo-first-order model. The material may have great potential in wastewater treatment applications. The synthesized nanomaterials were tested for their antibacterial properties against microorganisms Staphylococcus epidermidis and Pseudomonas aeruginosa. The antimicrobial property CSG/PVP/MoS2 nanocomposite was observed with a maximum of zone inhibition.


Assuntos
Quitosana/química , Dissulfetos/química , Glioxal/química , Molibdênio/química , Preparações Farmacêuticas/química , Preparações Farmacêuticas/isolamento & purificação , Fotólise , Povidona/química , Adsorção , Antibacterianos/química , Antibacterianos/farmacologia , Catálise , Cinética , Nanocompostos/química , Pseudomonas aeruginosa/efeitos dos fármacos , Staphylococcus aureus/efeitos dos fármacos , Poluentes Químicos da Água/química , Poluentes Químicos da Água/isolamento & purificação , Purificação da Água
6.
ScientificWorldJournal ; 2019: 8962923, 2019.
Artigo em Inglês | MEDLINE | ID: mdl-31205453

RESUMO

This paper includes synthesis and characterization of mixed ligand complexes derived from mefenamic acid and metformin using transition metal ions such as Co(II) and Cu(II). These complexes have been characterized by magnetic susceptibility, molar conductance, TG analyses, and spectral techniques such as FTIR and UV spectra. The theoretical study of the ligands and their complexes using semiempirical (PM6) method was used to measure IR and UV spectroscopy, HOMO-LUMO categories of the ligands. These synthesized complexes are also studied for their biological activities. The studies made on these complexes proposed a six octahedral geometry.


Assuntos
Complexos de Coordenação/química , Complexos de Coordenação/isolamento & purificação , Modelos Teóricos , Preparações Farmacêuticas/química , Preparações Farmacêuticas/isolamento & purificação , Fenômenos Químicos , Complexos de Coordenação/farmacologia , Ligantes , Estrutura Molecular , Análise Espectral , Relação Estrutura-Atividade , Termogravimetria
7.
J Chromatogr A ; 1602: 107-116, 2019 Sep 27.
Artigo em Inglês | MEDLINE | ID: mdl-31182304

RESUMO

Polystyrene is one of the best candidates as the extracting medium due to its high stability in different media and acceptable extraction capability. However, the hydrophobic nature and low wettability of polystyrene limits its application to non-polar analytes. To resolve this limitation, in this project, amine groups were chemically attached to the surface of magnetic polystyrene. The resulting hydrophilic magnetic particles were expected to be capable of extracting both polar and non-polar analytes. Non-steroidal anti-inflammatory drugs (NSAIDs) were chosen for testing the applicability of modified magnetic polystyrene according to the importance of their analysis and also their wide polarity range. Major parameters associated with the extraction procedure were optimized using central composite design (CCD) method and pH 3, extraction time of 15 min, desorption volume of 350 µL and desorption time of 4 min were chosen as optimized values. Under these conditions, figures of merit were calculated including: linear dynamic range (0.5-1000 µg L-1), linear equation and limits of detection (0.1-3 µg L-1). To investigate the method precision, inter-day, intra-day and synthesis-to-synthesis relative standard deviation (RSD) were studied (<12%). All studies were conducted using blank urine samples spiked with aspirin, salicylic acid, ibuprofen, diclofenac and mefenamic acid. Naproxen was chosen as the internal standard and high-performance liquid chromatography-UV-Vis (HPLC-UV) was employed for the subsequent determination after extraction. To evaluate the applicability of the method for real sample analysis, urine samples from patients under treatment were analyzed and acceptable results were obtained. The aminated magnetic polystyrene revealed superior extraction efficiency, much higher than polystyrene before functionalization. In addition, hospital wastewater sample was tested and acceptable extraction efficiencies were obtained.


Assuntos
Aminas/química , Magnetismo , Preparações Farmacêuticas/isolamento & purificação , Preparações Farmacêuticas/urina , Poliestirenos/química , Anti-Inflamatórios não Esteroides/química , Anti-Inflamatórios não Esteroides/urina , Diclofenaco/química , Diclofenaco/urina , Humanos , Ibuprofeno/química , Ibuprofeno/urina , Limite de Detecção , Reprodutibilidade dos Testes , Extração em Fase Sólida/métodos , Espectroscopia de Infravermelho com Transformada de Fourier , Águas Residuárias/química
8.
J Chromatogr A ; 1603: 23-32, 2019 Oct 11.
Artigo em Inglês | MEDLINE | ID: mdl-31230878

RESUMO

The analyses of drugs and metabolites in complex matrices have been widely studied in recent years. However, due to high levels endogenous compounds and matrix complexity, these analyses require a sample pre-treatment step. To this aim, two lab-made extractive phases were integrated to probe electrospray ionization mass spectrometry (PESI-MS) technique for direct analysis of illicit drugs in biological fluids and phorbol esters in Jatropha curcas extract. The polypyrrole (PPy) phase was electropolymerized onto a platinum wire surface by cyclic voltammetry. The molecularly imprinted polymer (MIP) was synthesized and adhered onto a stainless-steel needle with epoxy resin. The PPy-PESI-MS method showed to be linear in a concentration range from 1 to 500 µg L-1, with accuracy values between -2.1 and 14%, and precision values between 0.8 and 10.8%. The MIP-PESI-MS method showed to be linear in a concentration range from 0.9 to 30 mg L-1, with accuracy values between -1.6 and -15.3%, and precision values between 4.1 and 13.5%.


Assuntos
Impressão Molecular/métodos , Preparações Farmacêuticas/análise , Preparações Farmacêuticas/isolamento & purificação , Polímeros/química , Pirróis/química , Microextração em Fase Sólida/métodos , Espectrometria de Massas por Ionização por Electrospray/métodos , Cocaína/análise , Cocaína/isolamento & purificação , Voluntários Saudáveis , Humanos , Jatropha/química , Dietilamida do Ácido Lisérgico/análise , Dietilamida do Ácido Lisérgico/isolamento & purificação , Metanfetamina/análise , Metanfetamina/isolamento & purificação , N-Metil-3,4-Metilenodioxianfetamina/análise , N-Metil-3,4-Metilenodioxianfetamina/isolamento & purificação , Ésteres de Forbol/análise , Ésteres de Forbol/isolamento & purificação , Extratos Vegetais/análise , Extratos Vegetais/isolamento & purificação , Saliva/metabolismo , Aço Inoxidável/química , Urinálise
9.
Methods Mol Biol ; 1985: 201-237, 2019.
Artigo em Inglês | MEDLINE | ID: mdl-31069737

RESUMO

Since their introduction by Daniel W. Armstrong in 1994, antibiotic-based chiral stationary phases have proven their applicability for the chiral resolution of various types of racemates. The unique structure of macrocyclic glycopeptides and their large variety of interactive sites (e.g., hydrophobic pockets, hydroxy, amino and carboxyl groups, halogen atoms, aromatic moieties) are the reasons for their wide-ranging selectivity. The commercially available Chirobiotic™ phases, which display complementary characteristics, are capable of separating a broad variety of enantiomeric compounds with good efficiency, good column loadability, high reproducibility, and long-term stability. These are the major reasons for the frequent use of macrocyclic antibiotic-based stationary phases in HPLC enantioseparations.This overview chapter provides a brief summary of general aspects of antibiotic-based chiral stationary phases including their preparation and their application to direct enantioseparations of various racemates focusing on the literature published since 2004.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Glicopeptídeos/química , Antibacterianos/química , Compostos Macrocíclicos/química , Preparações Farmacêuticas/química , Preparações Farmacêuticas/isolamento & purificação , Estereoisomerismo
10.
Methods Mol Biol ; 1985: 357-364, 2019.
Artigo em Inglês | MEDLINE | ID: mdl-31069744

RESUMO

The enantioseparation of acidic and neutral compounds can be successfully achieved in capillary electrophoresis (CE) using dual-cyclodextrin (CD) systems. This chapter describes how to separate the enantiomers of acidic or neutral substances using dual-CD systems made up of a negatively charged CD derivative, i.e., sulfobutyl-ß-CD or carboxymethyl-ß-CD, in combination with a neutral one, namely heptakis(2,3,6-tri-O-methyl)-ß-CD. An acidic compound (carprofen) and a weakly acidic drug (pentobarbital) were selected as model compounds.


Assuntos
Ciclodextrinas/química , Eletroforese Capilar/métodos , Eletrólitos/química , Preparações Farmacêuticas/química , Preparações Farmacêuticas/isolamento & purificação , Estereoisomerismo
11.
Methods Mol Biol ; 1985: 373-381, 2019.
Artigo em Inglês | MEDLINE | ID: mdl-31069746

RESUMO

The enantioseparation of acidic and basic compounds can be successfully achieved in nonaqueous capillary electrophoresis (NACE) using single-isomer charged ß-cyclodextrin (ß-CD) derivatives of opposite charge to that of the analytes. This chapter describes how to separate the enantiomers of three basic substances selected as model compounds, i.e., alprenolol, bupranolol, and terbutaline, using the negatively charged heptakis(2,3-di-O-acetyl-6-O-sulfo)-ß-CD (HDAS-ß-CD). The enantiomers of three acidic drugs (tiaprofenic acid, suprofen, and flurbiprofen) are resolved using a monosubstituted amino ß-CD derivative, namely 6-monodeoxy-6-mono(3-hydroxy)propylamino-ß-CD (PA-ß-CD).


Assuntos
Ciclodextrinas/química , Eletroforese Capilar/métodos , Preparações Farmacêuticas/química , Preparações Farmacêuticas/isolamento & purificação , Estereoisomerismo
12.
Methods Mol Biol ; 1985: 407-416, 2019.
Artigo em Inglês | MEDLINE | ID: mdl-31069749

RESUMO

Particular attention has been paid to capillary electrophoresis as versatile and environmentally friendly approach for enantioseparations of a wide spectrum of compounds. Cyclodextrin-modified micellar electrokinetic chromatography (CD-MEKC) is a method of choice to provide effective separation toward hydrophobic and uncharged stereoisomers. The chiral discrimination of the solutes relies upon the partitioning between a given CD in the aqueous phase and micelles formed from a surfactant. Synergistic combinations of chiral selectors, surfactant, and modifier contribute to successful enantioseparations of the enantiomers. In this chapter, an application of CD-MEKC for the enantioseparation of selected imidazole drugs employing a dual CDs system is described.


Assuntos
Cromatografia Capilar Eletrocinética Micelar/métodos , Ciclodextrinas/química , Imidazóis/química , Preparações Farmacêuticas/química , Preparações Farmacêuticas/isolamento & purificação , Estereoisomerismo
13.
Biomed Chromatogr ; 33(10): e4602, 2019 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-31116448

RESUMO

The present work describes novel methods using densitometry and indirect or off-line high performance thin-layer chromatography-mass spectrometry (HPTLC-MS) for the simultaneous detection and quantification of asenapine, propranolol and telmisartan and their phase II glucuronide metabolites. After chromatographic separation of the drugs and their metabolites the analytes were scraped, extracted in methanol and concentrated prior to mass spectrometric analysis. Different combinations of toluene and methanol-ethanol-n-butanol-iso-propanol were tested for analyte separation and the best results were obtained using toluene-methanol-ammonia (6.9:3.0:0.1, v/v/v) as the elution solvent. All of the drug-metabolite pairs were separated with a homologous retardation factor difference of ≥22. The conventional densitometric approach was also studied and the method performances were compared. Both of the approaches were validated following the International Conference on Harmonization guidelines, and applied to spiked human plasma samples. The major advantage of the TLC-MS approach is that it can provide much lower limits of detection (1.98-5.83 pg/band) and limit of quantitation (5.97-17.63 pg/band) with good precision (˂3.0% coefficient of variation) compared with TLC-densitometry. The proposed indirect HPTLC-MS method is simple yet effective and has tremendous potential in the separation and quantitation of drugs and their metabolites from biological samples, especially for clinical studies.


Assuntos
Cromatografia em Camada Delgada/métodos , Densitometria/métodos , Glucuronídeos , Preparações Farmacêuticas , Espectrometria de Massas por Ionização por Electrospray/métodos , Administração Oral , Cromatografia Líquida de Alta Pressão , Glucuronídeos/sangue , Glucuronídeos/isolamento & purificação , Glucuronídeos/metabolismo , Glucuronídeos/farmacocinética , Compostos Heterocíclicos de 4 ou mais Anéis , Humanos , Limite de Detecção , Modelos Lineares , Preparações Farmacêuticas/sangue , Preparações Farmacêuticas/isolamento & purificação , Preparações Farmacêuticas/metabolismo , Reprodutibilidade dos Testes
14.
Molecules ; 24(7)2019 Mar 27.
Artigo em Inglês | MEDLINE | ID: mdl-30934659

RESUMO

In this study, a novel sort of sample preparation sorbent was developed, by preparing thin layer graphene oxide tablets (GO-Tabs) utilizing a mixture of graphene oxide and polyethylene glycol on a polyethylene substrate. The GO-Tabs were used for extraction and concentration of omeprazole (OME) in human saliva samples. The determination of OME was carried out using liquid chromatography-tandem mass spectrometry (LC⁻MS/MS) under gradient LC conditions and in the positive ion mode (ESI+) with mass transitions of m/z 346.3→198.0 for OME and m/z 369.98→252.0 for the internal standard. Standard calibration for the saliva samples was in the range of 2.0⁻2000 nmol L-1. Limits of detection and quantification were 0.05 and 2.0 nmol L-1, respectively. Method validation showed good method accuracy and precision; the inter-day precision values ranged from 5.7 to 8.3 (%RSD), and the accuracy of determinations varied from -11.8% to 13.3% (% deviation from nominal values). The extraction recovery was 60%, and GO-Tabs could be re-used for more than ten extractions without deterioration in recovery. In this study, the determination of OME in real human saliva samples using GO-Tab extraction was validated.


Assuntos
Grafite/química , Omeprazol/farmacocinética , Óxidos/química , Preparações Farmacêuticas/química , Saliva , Comprimidos/química , Cromatografia Líquida , Tomografia com Microscopia Eletrônica , Humanos , Omeprazol/química , Preparações Farmacêuticas/isolamento & purificação , Polimerização , Reprodutibilidade dos Testes , Solventes , Espectrometria de Massas em Tandem
15.
Methods Mol Biol ; 1972: 127-136, 2019.
Artigo em Inglês | MEDLINE | ID: mdl-30847788

RESUMO

The present work describes a capillary electrophoretic (CE) generic strategy used for chiral enantioseparation of Fluconazole (as an example of acidic drugs) and donepezil (as an example of basic drugs). Several modified cyclodextrins (CDs) were applied for enantioseparation of racemates such as highly sulfated α, γ CDs, hydroxyl propyl-ß-CD, and sulfobutyl ether-ß-CD. The starting screening conditions consist of 50 mM phosphate-triethanolamine buffer at pH 2.5, an applied voltage of 15 kV, and a temperature of 25 °C. The design of experiment (DOE) was based on a full factorial design of the crucial two factors (pH and %CD) at three levels, to make a total of nine (32) experiments with high, intermediate, and low values for both factors. Evaluation of the proposed strategy pointed out that best resolution was obtained at pH 2.5 for the investigated racemates using low percentages of HS-γ-CD, while SBE-ß-CD was the most successful chiral selector offering acceptable resolution, with best separation at low pH values and at higher %CD within 10 min runtime. Regression study showed that the linear model shows a significant lack of fit for all chiral selectors, anticipating that higher orders of the factors are most likely to be present in the equation with possible interactions.


Assuntos
Ácidos/química , Eletroforese Capilar/métodos , Preparações Farmacêuticas/química , Preparações Farmacêuticas/isolamento & purificação , Concentração de Íons de Hidrogênio , Modelos Teóricos , Estereoisomerismo
16.
Molecules ; 24(5)2019 Feb 26.
Artigo em Inglês | MEDLINE | ID: mdl-30813595

RESUMO

A new functionalized polymer monolithic capillary with a macrocyclic antibiotic, namely colistin sulfate, as chiral selector was prepared via the copolymerization of binary monomer mixtures consisting of glycidyl methacrylate (GMA) and ethylene glycol dimethacrylate (EGDMA) in porogenic solvents namely 1-propanol and 1,4-butanediol, in the presence of azobisiso-butyronitrile (AIBN) as initiator and colistin sulfate. The prepared capillaries were investigated for the enantioselective nano-LC separation of a group of racemic pharmaceuticals, namely, α- and ß-blockers, anti-inflammatory drugs, antifungal drugs, norepinephrine-dopamine reuptake inhibitors, catecholamines, sedative hypnotics, antihistaminics, anticancer drugs, and antiarrhythmic drugs. Acceptable separation was achieved for many drugs using reversed phase chromatographic conditions with no separation achieved under normal phase conditions. Colistin sulfate appears to be useful addition to the available macrocyclic antibiotic chiral phases used in liquid chromatography.


Assuntos
Eletrocromatografia Capilar/métodos , Colistina/química , Preparações Farmacêuticas/síntese química , Compostos de Epóxi/química , Metacrilatos/química , Nitrilos/química , Preparações Farmacêuticas/química , Preparações Farmacêuticas/isolamento & purificação , Polímeros/química , Solventes , Estereoisomerismo
17.
Chem Asian J ; 14(9): 1487-1495, 2019 May 02.
Artigo em Inglês | MEDLINE | ID: mdl-30896087

RESUMO

A composite material that comprised metal-organic nanotubes (MONTs) and a sponge, Cu-MONTs-sponge, was synthesized by using a rapid and convenient surfactant-assisted dip-coating method and used as a high-performance adsorbent for the solid-phase extraction of pharmaceuticals and personal care products (PPCP) from environmental water samples. By adjusting the surfactant concentration, a composite material that contained metal-organic nanotubes and a macroporous 3D porous sponge was constructed. This modified sponge achieved outstanding reproducibility as an adsorbent, with the adsorption of trace or ultratrace amounts of contaminants. Moreover, this composite material was conveniently recycled and its extraction efficiency only decreased by 6.3-12.1 % after 30 adsorption/desorption cycles. The resulting composite exhibited excellent adsorption capacity for PPCPs, which was attributed to its unique porous structure, natural hydrophobicity, and electrostatic interactions between the metal-organic nanotubes and analyte molecules. This Cu-MONTs-sponge material is an ideal adsorbent for the extraction of trace amounts of PPCPs from environmental water samples.


Assuntos
Cosméticos/análise , Estruturas Metalorgânicas/química , Nanotubos/química , Preparações Farmacêuticas/análise , Poluentes Químicos da Água/análise , Adsorção , Cosméticos/isolamento & purificação , Interações Hidrofóbicas e Hidrofílicas , Preparações Farmacêuticas/isolamento & purificação , Porosidade , Reprodutibilidade dos Testes , Extração em Fase Sólida , Eletricidade Estática , Poluentes Químicos da Água/química
18.
Chemosphere ; 226: 210-219, 2019 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-30927673

RESUMO

The presence of PPCPs (Pharmaceuticals and Personal Care Products) in water sources and drinking water has concerned researchers in recent times. This study was carried out to evaluate the occurrence of 6 PPCPs (namely paracetamol, diclofenac, naproxen, ibuprofen, benzophenone-3 and methylparaben) in the Lobo reservoir, their degradation products, and how efficiently they were removed by 22 ecological filters, considering individual and mixture of compounds. There were 3 spiking events of PPCPs (2 µg L-1) in the ecological filter influents conducted with a lag period of 15 days between spikes. Water samples were collected from the influent and effluent of the filters at 3, 6 and 24 h after each spiking event. All target PPCPs were identified in the Lobo reservoir water in the range of µg L-1. The personal care products were detected with 100% frequency in the samples, and in higher concentrations compared to the pharmaceuticals. Degradation products of diclofenac and benzophenone-3 were identified in the water samples. Results of this investigation show that ecological filtration was an effective process (70-99%) to remove 2 µg L-1 of the selected PPCPs, and demonstrated that the filters were resilient to individual compounds and to their mixtures.


Assuntos
Filtração/métodos , Preparações Farmacêuticas/isolamento & purificação , Poluentes Químicos da Água/isolamento & purificação , Purificação da Água/métodos , Benzofenonas/análise , Brasil , Cosméticos/análise , Diclofenaco/análise , Preparações Farmacêuticas/análise , Eliminação de Resíduos Líquidos/métodos , Poluentes Químicos da Água/análise
19.
J Chromatogr A ; 1593: 24-33, 2019 May 24.
Artigo em Inglês | MEDLINE | ID: mdl-30712822

RESUMO

Polar-embedded stationary phases are superior to conventional alkyl stationary phases in terms of water-wettability, silanol activity and polar selectivity. A novel method was proposed for efficient preparation of amide-embedded stationary phases bearing extended aliphatic chain and large aromatic ring. The present approach, which simply required isocyanate and desired carboxylic acid, rather than the normal combination of amine/acyl chloride/proton scavenger, produced aromatic pyrenyl amide-embedded (PYE-Amide) and aliphatic docosanyl amide-embedded (C22-Amide) stationary phases. The as-synthesized packing materials were characterized and evaluated in comparison with conventional octadecyl stationary phases in terms of bonding density, aromatic and hydrophobic natures, charge-transfer capability, and selectivity towards isomers of various unsaturated compounds. A high affinity of the unsaturated ligand for the unsaturated solutes, especially the electron-deficient ones, was observed. The PYE-Amide stationary phase exhibited unique aromaticity-dependent shape selectivity, which was beneficial to the resolution of certain geometric isomers of polycyclic arenes. The applicability of such stationary phases was demonstrated by effective separations of estrogens and sulfonamide drugs.


Assuntos
Amidas/química , Cromatografia de Fase Reversa/instrumentação , Cromatografia de Fase Reversa/métodos , Interações Hidrofóbicas e Hidrofílicas , Modelos Químicos , Preparações Farmacêuticas/análise , Preparações Farmacêuticas/química , Preparações Farmacêuticas/isolamento & purificação
20.
Artigo em Inglês | MEDLINE | ID: mdl-30709041

RESUMO

We present herein the preparation of novel polymer inclusion membranes (PIMs) containing insoluble ß-CD polymer as a carrier, polyvinyl chloride as a base polymer, and dibuthylphtalate (DBP) as a plasticizer in varying proportions. The prepared PIMs can be obtained by a simple, fast, and high-yield preparation process. Physicochemical characterizations of such membranes occurred in a homogeneous structure. In addition, Fourier-transform infrared Spectroscopy (FT-IR) analysis found that DBP was inserted between these polymeric chains by non-covalent interactions. This led to a spacing of PVC/poly(ß-cyclodextrin) chains inducing a better access of guest molecules to PIM cyclodextrins. To achieve the elimination of ibuprofen and progesterone, two examples of emerging environmental contaminants that can lead to possible alterations to aquatic environments and affect human health, the effect of three operating parameters was studied (pH, the proportion of ß-cyclodextrin polymer, and wastewater agitation). The proportion of ß-cyclodextrin polymer and wastewater agitation had a favorable influence on drug extraction at 10 ppm. The PIMs containing ß-cyclodextrin polymer was unstable in basic conditions and was more effective at acidic pH. These initial results demonstrate the high potential for drug extraction of this polymer.


Assuntos
Celulose/química , Ciclodextrinas/química , Preparações Farmacêuticas/isolamento & purificação , Polímeros/química , Águas Residuárias/química , Poluentes Químicos da Água/isolamento & purificação , Humanos , Solubilidade , Espectroscopia de Infravermelho com Transformada de Fourier/métodos
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