Yanhua Ma

In situ loading of gold nanoparticles on Fe3O4@SiO2 magnetic nanocomposites and their high catalytic activity

In this work, a facile approach was successfully developed for in situ catalyzing Au nanoparticles loaded on Fe3O4@SiO2 magnetic nanospheres via Sn(2+) linkage and reduction. After the Fe3O4@SiO2 MNPs were first prepared via a sol-gel process, only one step was needed to synthesize the Fe3O4@SiO2-Au magnetic nanocomposites (Fe3O4@SiO2-Au MNCs), so that both the synthesis step and the reaction cost were remarkably decreased. Significantly, the as-synthesized Fe3O4@SiO2-Au MNCs showed high performance in the catalytic reduction of 4-nitrophenol to 4-aminophenol and could be reused for several cycles with convenient magnetic separability. This approach provided a useful platform based on Fe3O4@SiO2 MNPs for the fabrication of Au or other noble metal magnetic nanocatalysts, which would be very useful in various catalytic reductions.

Micelle to solvent stacking of two alkaloids in nonaqueous capillary electrophoresis.

This paper for the first time describes the development of micelle to solvent stacking (MSS) to nonaqueous capillary electrophoresis (NACE). In this proposed MSS-NACE, sodium dodecyl sulfate (SDS) micelles transport, release, and focus analytes from the sample solution to the running buffer using methanol as their solvent. After the focusing step, the focused analytes were separated via NACE. The focusing mechanism and influencing factors were discussed using berberine (BBR) and jatrorrhizine (JTZ) as model compounds. And the optimum condition was obtained as following: 50 mM ammonium acetate, 6% (v/v) acetic acid and 10 mM SDS in redistilled water as sample matrix, 50 mM ammonium acetate and 6% (v/v) acetic acid in pure methanol as the running buffer, -20 kV focusing voltage with 30 min focusing time. Under these conditions, this method afforded limits of detection (S/N=3) of 0.002 μg/mL and 0.003 μg/mL for BBR and JTZ, respectively. In contrast to conventional NACE, the concentration sensitivity was improved 128-153-fold.

A sensitive colorimetric method for the determination of nitrite in water supplies, meat and dairy products using ionic liquid-modified methyl red as a colour reagent

This paper describes a colorimetric approach to determine trace amounts of nitrite in water supplies, meat and dairy products using 1-butyl-3-methylimidazolium-modified methyl red ([BMIM]MR) as a colour reagent. The technique capitalises on the catalytic effect of nitrite on the oxidative degradation of [BMIM]MR by potassium bromate in acidic media. The absorbances were proportional to nitrite concentrations in the range of 8.70×10(-2) to 4.17 μM with a detection limit of 1.64×10(-2) μM. Compared with the method using methyl red as a colour reagent, 60 times improvement of sensitivity was obtained. Activation energy and the apparent rate constant for the catalytic reaction are 61.11 kJ mol(-1) and 1.18×10(4) s(-1), respectively. The proposed method was successfully applied for the analysis of nitrite in Yellow River water, chicken, and milk with recoveries ranging from 96% to 105%.

A novel cross-H-channel interface for flow injection-capillary electrophoresis to reduce sample requirement and improve sensitivity

In this study, a cross-H-channel interface was constructed for coupling flow injection with capillary electrophoresis (FI-CE) to reduce sample requirement and sensitivity loss in the typical FI-CE. Based on this cross-H-channel interface, a new FI-CE system was established, in which sample introduction was performed by directly injecting sample solution along a thin capillary (50 μm, i.d.) to the interface from an injection syringe. The sample requirement was reduced distinctly and usual sample dilution in the sample transport process was obviously decreased, thereby spontaneously enhancing the sensitivity. Moreover, because of the unique construction of the cross-H-channel interface, field amplified sample stacking (FASS) and high-speed CE were skillfully combined to further improve the sensitivity and to shorten separation time. The versatility of this new FI-CE was demonstrated by determination of ephedrine (E) and pseudoephedrine (PE) in human urine. Up to 45 repeated injections per hour and clearly baseline separation of E and PE in less than 1 min were achieved, giving limits of detection (LODs) of 0.23 and 0.21 μg mL(-1) for E and PE, respectively, and yielding relative standard deviation (RSD) values of the migration time and the peak height (n=5) of 2.6% and 3.1% for E, 2.3% and 3.3% for PE, respectively. In contrast to typical FI-CE, approximately 8-250-fold decreases in sample volume requirement, 7-fold shortening in separation time and 50-fold improvements in sensitivity were obtained.

Chiral separation of β-blockers by MEEKC using neutral microemulsion: Analysis of separation mechanism and further elucidation of resolution equation

Based on the investigation of the effect of microemulsion charge on the chiral separation, a new chiral separation method with MEEKC employing neutral microemulsion was established. The method used a microemulsion containing 3.0% (w/v) neutral surfactant Tween 20 and 0.8% (w/v, 30 mM) dibutyl l‐tartrate in 40 mM sodium tetraborate buffer to separate the enantiomers of β‐blockers. The effect of major parameters on the chiral separation was investigated. The applied voltage had little effect on the resolution, but the chiral separation could be improved by suppressing the EOF. Nine racemic β‐blockers obtained relatively good enantioseparation after appropriate concentrations of tetradecyl trimethyl ammonium bromide were added into the microemulsion to suppress the EOF. These results were explained based on the analysis of the separation mechanism of the method and deduced separation equations. The resolution equation of the method was further elucidated. It was found that the fourth term in the resolution equation, an additional term compared to the conventional resolution equation for column chromatography, represents the ratio of the relative movement distance between the analyte and microemulsion droplets relative to the effective capillary length. It can be regarded as a correction for the effective capillary length. These findings are significant for the development of the theory of MEEKC and the development of new chiral MEEKC method.

Recent developments in chiral analysis of β-blocker drugs by capillary electromigration techniques.

The latest developments in chiral analysis of β‐blocker drugs by capillary electromigration techniques are reviewed in this article. Following the previous review by Aturki et al. [Electrophoresis 2011, 32, 2602–2628], this review includes the papers published during the period from January 2011 to December 2013. During this time, some novel chiral selectors were reported and applied to improve the enantioseparation of β‐blocker drugs and structurally related compounds. These chiral selectors include CDs and their derivatives, macrocyclic antibiotics, tartrate complexs, the monolithic molecularly imprinted polymer, and the polymeric surfactants. In addition, this article summarizes the methodological improvements for enhancing sensitivity in chiral analysis of β‐blockers and structurally related compounds by CE. The involved authors described the use of online sample preconcentration techniques to increase the detection sensitivity in the enantiomeric analysis of a broad range of samples.

Preparation and characterization of magnetic gold shells using different sizes of gold nanoseeds and their corresponding effects on catalysis

The effect of gold nanoseeds with different sizes on the gold shell was investigated. Gold nanoparticles of two different sizes (∼3 nm and ∼15 nm) were prepared and attached to the surface of amine functionalized silica coated iron oxide nanoparticles. The gold nanoparticles assembled on the surface were used as seeds for further gold shell formation. It was observed that the amount of Au attached to iron oxide nanoparticles is higher for bigger gold nanoseeds as compared to smaller gold nanoseeds. Similarly, after the formation of gold shell, a higher amount of Au was found for larger gold nanoparticles. However, both transmission electron microscopy (TEM) and scanning electron microscopy (SEM) results show that a complete, uniform, and compact gold shell was formed in the case of using small gold nanoseeds, but for larger gold nanoseeds the shell formed was discontinuous and was not uniform, while most of the gold nanoparticles were found to be aggregated on the surface. The nanocomposites showed high efficiency in catalysis for the reduction of 4-nirophenol, among which Nanocomp-2, with a thin stable gold shell showed excellent catalytic activity and reusability. All of the nanocomposites have high magnetization values and can be easily separated from the reaction mixture using a magnet and can be reused.

Sensitive enantioanalysis of β‐blockers via field‐amplified sample injection combined with water removal in microemulsion electrokinetic chromatography

In this study, an on‐line sample preconcentration technique, field‐amplified sample injection combined with water removal by electroosmotic flow (EOF) pump, was applied to realize a highly sensitive chiral analysis of β‐blocker enantiomers by MEEKC. The introduction of a water plug in capillary before the electrokinetic injection provided the effective preconcentration of chiral compounds. And then the water was moving out of the column from the injection end under the effect of the EOF, which avoided dilution of the stacked β‐blocker enantiomers concentration suffering from the presence of water in separation buffer. Moreover, the addition of H3PO4 and methanol in the sample solution greatly improved the enhancement efficiency further. Under optimized conditions, more than 2700‐fold enhancement in sensitivity was obtained for each enantiomer of bupranolol (BU), alprenolol (AL), and propranolol (PRO) via electrokinetic injection. LODs were 0.10, 0.10, 0.12, 0.11, 0.02, and 0.02 ng/mL for S‐BU, R‐BU, S‐AL, R‐AL, S‐PRO, and R‐PRO, respectively. Eventually, the proposed method was successfully applied to the determination of BU, AL, and PRO in serum samples with good recoveries ranging from 93.4 to 98.2%.