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1.
J Chromatogr A ; 1311: 176-82, 2013 Oct 11.
Article in English | MEDLINE | ID: mdl-24011418

ABSTRACT

A novel approach based on surface molecularly imprinted technique is demonstrated for the synthesis of surface molecularly imprinted silica nanoparticles (MI-SiNPs) in aqueous media, using l-tryptophan (l-Trp) as template molecule. The MI-SiNPs were fully characterized by transmission electron microscopy (TEM), thermo gravimetric analysis (TGA) and atomic force microscopy (AFM), and the results showed MI-SiNPs thus prepared were uniform in particle size (∼87nm) with a distinct core-shell structure with shell thickness of ∼7nm. The terminal carboxyl groups endowed the MI-SiNPs with good water-compatibility, and so good suspension stability for MI-SiNPs in water-rich buffer solutions can be easily achieved without the addition of any other reagents. When MI-SiNPs were used as pseudostationary phases (PSPs) in electrokinetic chromatography (EKC) for the enantioseparation of Trp, a resolution of 2.73 can be achieved in less than 10min with symmetric peaks. These excellent separation features are mainly attributed to the fast mass transfer and good accessibility of the interaction sites locating at the surface of the MI-SiNPs. The effects of some important separation factors, e.g., pH and concentration of buffer solution, content of MI-SiNPs added, content of organic modifier in buffer solution, on the enantioseparation of Trp were studied, and an optimum separation condition of 30% (v/v) acetonitrile in 20mmolL(-1) phosphate buffer (pH 7.0), with 0.50mgmL(-1) MI-SiNPs added was ultimately selected.


Subject(s)
Molecular Imprinting/methods , Silicon Dioxide/chemistry , Tryptophan/isolation & purification , Acetonitriles/chemistry , Buffers , Nanoparticles/chemistry , Particle Size , Stereoisomerism , Water/chemistry
2.
Electrophoresis ; 33(13): 2012-8, 2012 Jul.
Article in English | MEDLINE | ID: mdl-22806467

ABSTRACT

A novel and simple method for the preparation of silica nanoparticles having surface-functionalized diamino moiety (dASNPs) was reported in our paper and characterized using scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectrometry, and thermogravimetry techniques. To test this method practically, in this contribution we describe the enhanced separation of four plant auxins - indole-3-acetic acid (IAA), indole-3-butyric acid (IBA), 2,4-dichlorophenoxyacetic acid (dCPAA), and 2-(1-naphthyl) acetic acid (NAA) - by capillary electrochromatography using diamino moiety functionalized silica nanoparticles as pseudostationary phase (PSP) in the running buffer. The effect of pH, buffer concentration, and diamino moiety functionalized silica nanoparticles concentration on the selectivity of separation was investigated. A combination of the nanoparticles and running buffer reversed the electroosmotic direction making possible the rapid and efficient separation of the auxins from the auxins migrated in the same direction with the EOF under optimum experimental conditions. A good resolution of four auxins was obtained within 5.5 min under optimum experimental conditions. The precision (RSD, n = 5) was in the range of 0.72-0.91% and 1.89-2.23% for migration time and peak area response, respectively. The detection limits were 0.48, 0.44, 0.46, and 0.42 µM for NAA, IBA, IAA, and dCPAA, respectively. Furthermore, the method was successfully tested for the determination of IAA in the grapes.


Subject(s)
Capillary Electrochromatography/methods , Indoleacetic Acids/isolation & purification , Nanoparticles/chemistry , Silicon Dioxide/chemistry , Vitis/chemistry , 2,4-Dichlorophenoxyacetic Acid/analysis , 2,4-Dichlorophenoxyacetic Acid/isolation & purification , Electroosmosis , Hydrogen-Ion Concentration , Indoleacetic Acids/analysis , Linear Models , Naphthols/analysis , Naphthols/isolation & purification , Reproducibility of Results , Sensitivity and Specificity
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