Determination of residual fluoroquinolones in honey by liquid chromatography using metal chelate affinity chromatography

A new analytical method for the simultaneous determination of seven fluoroquinolones, namely, norfloxacin, ciprofloxacin, danofloxacin, enrofloxacin, orbifloxacin, sarafloxacin, and difloxacin, especially in dark-colored honey, has been developed. Fluoroquinolone antibiotics were extracted from samples with MacIlvaine buffer solution (pH 4.0) containing EDTA disodium salt dihydrate. The extracts were treated with both a polymeric cartridge and a metal chelate affinity column preloaded with ferric ion (Fe3+). LC separation with fluorescence detection was performed at 40 degrees C using an Inertsil ODS-4 analytical column (150 x 4.6 mm, 3 microm). The mobile phase was composed of 20 mM/L citrate buffer solution (pH 3.1)-acetonitrile mixture (70 + 30, v/v) containing 1 mM/L sodium dodecyl sulfate. Lomefloxacin was used as an internal standard. The developed method was validated according to the criteria of European Commission Decision 2002/657/EC. Decision limits and detection capabilities were below 2.9 and 4.4 microg/kg, respectively.     

High-performance liquid chromatography with photodiode array detection for determination of nobiletin content in the brain and serum of mice administrated the natural compound

We recently demonstrated that nobiletin, a citrus flavonoid, exhibits anti-dementia action in animals. However, no determination methods for the content of nobiletin with beneficial action in the brain of nobiletin-administered animals have been developed, nor has its pharmacokinetics been revealed completely. Here, we established the high-performance liquid chromatography/photodiode array detection method for nobiletin determination using Bond Elut C18 SPE cartridges for extraction, where the calibration curve was linear over 0.025-10 ng, with coefficient of variation of less than 6.76%. This method enabled us to determine pharmacokinetic parameters of nobiletin given intraperitoneally or per os in the brain of mice.     

9-Azanoradamantane N-oxyl (Nor-AZADO): a highly active organocatalyst for alcohol oxidation

A highly active organocatalyst for alcohol oxidation has been developed. 9-Azanoradamantane N-oxyl (Nor-AZADO 4), constituting an unhindered, stable nitroxyl radical, exhibits superior catalytic activity to 2,2,6,6-tetramethylpiperidine-1-oxyl (TEMPO) and AZADOs in the oxidation of alcohols to their corresponding carbonyl compounds.     

Synthesis of bis(N-heterocyclic carbene) palladium complexes derived from (S,S)-1,2-bis(1-hydroxypropyl)benzene

New o-xylylene-linked bis(benzimidazolium) salts were synthesized in six-steps from C₂-symmetric chiral 1,4-diol, 1,2-bis(1-hydroxypropyl)benzene, as a starting material. The silver complex of bis(benzimidazol-2-ylidene) was obtained on treatment of bis(benzimidazolium) salt with silver oxide. The reaction of the silver bis-NHC with [PdCl₂(PhCN)₂] afforded the bis-NHC complex of palladium. The X-ray diffraction studies on Pd complexes revealed that these complexes have distorted square planar geometry around the Pd center coordinating the NHC ligand in mutually cis-position. The arene ring of o-xylylene unit hanged over the Pd center and thus these complexes showed C₁-symmetric structures. The variable temperature NMR spectroscopy revealed that these Pd complexes showed fluxional behavior between C₁- and C₂-symmetric structures in solution state.     

Growth rate predictions of single- and multi-mode Richtmyer�CMeshkov instability with reshock

The single- and multi-mode Richtmyer–Meshkov instabilities (RMI) with reshock are numerically analyzed in two- and three-dimensional domains. Four different types of air/SF ₆ interface shapes are investigated in a shock tube configuration, and the predicted post-reshock growth rates are compared with available empirical models of Mikaelian’s (Physica D 36(3):343–347, 1989) and Charakhch’an’s (J Appl Mech Tech Phys 41(1):23–31, 2000). The simulation of 3D multi-mode RMI shows good agreement with a past experimental study, but other interface types (2D single-mode, 2D multi-mode and 3D single-mode) result in different growth rates after reshock. Parametric studies are therefore performed to investigate the sensitivities of the post-reshock growth rates to model the empirical parameters. For single-mode RMI configurations, the interface shape is found to be only a weak function of the post-reshock growth rate, as also predicted by previous reshock models. The post-reshock growth rate shows a linear correlation to the velocity jump due to reshock; however, it is only about a half of the prediction of Charakhch’an’s model even though the growth before reshock compares well with pre-reshock models. The 3D single-mode post-reshock RMI growth rate is nearly 1.6 times larger than the 2D single-mode RMI. The parametric studies of multi-mode RMI show two distinctly different growth rates depending on the mixing conditions at reshock. If the interface remains sharp at the time of reshock, the post-reshock growth rate is as large as the single-mode cases. However, if the interface is mixed due to non-linear interactions of bubbles and spikes, the growth rates becomes slow and independent of the interface shapes. Overall, this study provides new insights into the flow features of reshocked RMI for different initial perturbation types.     

γ-poly(glutamic acid) as an initiator of cationic polymerization of N-vinylcarbazole and N-vinyl-2-pyrrolidone

The cationic polymerization of vinyl monomers initiated by biosynthesized γ-poly(glutamic acid) (γ-PGA) powder surface was carried out in a heterogeneous system. It was found that the polymerization of N-vinylcarbazole (NVC) and N-vinyl-2-pyrrolidone (NVPD) is initiated by γ-PGA powder. The grafting of polymers onto γ-PGA surface was scarcely observed. The apparent activation energy of the polymerization of NVC and NVPD was estimated to be 20.2 and 24.8 kJ/mol, respectively. The polymerization was totally inhibited by the addition of triethylamine and pyridine, but not hydroquinone. The polymerization rate in nitrobenzene was larger than that in toluene. These results indicated the cationic nature of the polymerization. γ-PGA treated with KOH did not show the initiating activity of the polymerization. Therefore, carboxyl groups on γ-PGA powder surface play an important role in the initiation of the polymerization. It may be suggested that the polymerization is initiated by proton addition to monomer from carboxyl groups on γ-PGA powder surface and the propagation proceeds with carboxylate anion on the surface as counter ion. © 1993 John Wiley & Sons, Inc.     

Liquid-liquid extraction of silver ion with benzothiacrown ether derivatives

The extraction behavior of mono-, poly-, anal bis-(benzothiacrown ether)s is studied for alkali, alkaline-earth, heavy, and transition metal ions in the presence of picrate. These ethers show high selectivity for silver ion. Silver extractions from binary and quaternary mixtures of silver with heavy or transition metal ions were successful, except for mixtures with mercury(II) ion. Silver was extracted from a copper ore with ca. 80% recovery.     

Determination of methylglyoxal in mouse blood by liquid chromatography with fluorescence detection

A highly sensitive and rapid liquid chromatographic method for the determination of methylglyoxal in mouse blood is described, based on the precolumn conversion of methylglyoxal to a highly fluorescent 3-methyl-6,7-methylenedioxyquinoxaline by reaction with 1,2-diamino- 4,5-methylenedioxybenzene. The method is applied to the determination of methylglyoxal (0.1- 10⁴ pmol) in 5 μ1 of blood.     

A multi-objective lead time control problem in multi-stage assembly systems using genetic algorithms

In this paper, we develop a multi-objective model to optimally control the lead time of a multi-stage assembly system, using genetic algorithms. The multi-stage assembly system is modelled as an open queueing network. It is assumed that the product order arrives according to a Poisson process. In each service station, there is either one or infinite number of servers (machines) with exponentially distributed processing time, in which the service rate (capacity) is controllable. The optimal service control is decided at the beginning of the time horizon. The transport times between the service stations are independent random variables with generalized Erlang distributions. The problem is formulated as a multi-objective optimal control problem that involves four conflicting objective functions. The objective functions are the total operating costs of the system per period (to be minimized), the average lead time (min), the variance of the lead time (min) and the probability that the manufacturing lead time does not exceed a certain threshold (max). Finally, we apply a genetic algorithm with double strings using continuous relaxation based on reference solution updating (GADSCRRSU) to solve this multi-objective problem, using goal attainment formulation. The results are also compared against the results of a discrete-time approximation technique to show the efficiency of the proposed genetic algorithm approach.     

Direct mono-phosphorylation of 1,3-diols. A synthesis of FTY720-phosphate

A novel method for selective and direct phosphorylation of various 1,3-diols using silver(I) oxide, tetrabenzyl pyrophosphate (TBPP), and tetrahexylammonium iodide affording mono-phosphates was developed. We applied the present method to the synthesis of FTY720-phosphate.