Analytical Sciences
Online ISSN : 1348-2246
Print ISSN : 0910-6340
ISSN-L : 0910-6340
Volume 32 , Issue 12
Showing 1-21 articles out of 21 articles from the selected issue
Original Papers
  • Yaxin FAN, Xiaojie WU, Miao ZHAO, Beining GUO, Guoying CAO, Jicheng YU ...
    Type: Original Papers
    2016 Volume 32 Issue 12 Pages 1269-1276
    Published: December 10, 2016
    Released: December 10, 2016
    JOURNALS FREE ACCESS
    Rapid, accurate and sensitive ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) methods were developed and validated for the simultaneous quantitation of amoxicillin and clavulanic acid in human plasma and urine samples. Amoxicillin and clavulanic acid in both plasma and urine were extracted using a solid-phase extraction method. The compounds were separated on an Acquity UPLC HSS T3 column (2.1 × 100 mm, 1.8 μm). Ampicillin was used as the internal standard (IS) in plasma, while amoxicillin-d4 and sulbactam were used as ISs in urine. The lower limit of quantitation was 0.0500 and 0.0250 μg/mL for amoxicillin and clavulanic acid in plasma, and 0.0500 μg/mL for both analytes in urine. The established methods were validated in terms of selectivity, precision, accuracy, linearity, matrix effect, recovery, carryover, interaction, dilution integrity and stability, and successfully applied to a pharmacokinetic study of amoxicillin sodium and clavulanate potassium (10:1) injection in healthy volunteers.
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  • Xiao-Tong MA, Xi-Wen HE, Wen-You LI, Yu-Kui ZHANG
    Type: Original Papers
    2016 Volume 32 Issue 12 Pages 1277-1282
    Published: December 10, 2016
    Released: December 10, 2016
    JOURNALS FREE ACCESS
    Glycosylation plays an important part in many biological processes. However, many glycoproteins are either of low abundance or covered by other components in biological samples. Hence, developing new methods to measure the glycoproteins with both high efficiency and low detection limit is important. In this work, a self-assembled 4-mercaptophenylboronic acid film was coated on a quartz crystal microbalance chip. By optimizing the reaction time and the concentration of 4-mercaptophenylboronic acid, a sensor that specifically responded to glycoproteins was created. Then, several parameters for the prepared sensor were investigated and the working curve for representative glycoprotein–transferrin was established. The linearity range was from 50 to 400 ng/mL and the detection limit was 21.0 ng/mL. The sensor was used to detect transferrin in artificial urine samples. This sensor has a low detection limit of glycoproteins requiring only a small amount of samples, and thus has potential applications in both pharmaceutical and medical areas.
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  • Takashi NAKAZAWA, Saori IZUMO, Naoki FURUTA
    Type: Original Papers
    2016 Volume 32 Issue 12 Pages 1283-1289
    Published: December 10, 2016
    Released: December 10, 2016
    JOURNALS FREE ACCESS
    To accelerate the vaporization, atomization, and ionization efficiencies in laser ablation inductively coupled plasma mass spectrometry, we merged HCl gas with laser-ablated particles before introduction into the plasma, to convert their surface constituents from oxides to lower-melting chlorides. When particles were merged with HCl gas generated from a HCl solution at 200°C, the measured concentrations of elements in the particles were 135% higher on average than the concentrations in particles merged with ultrapure water vapor. Particle corrosion and surface roughness were observed by scanning electron microscopy, and oxide conversion to chlorides was confirmed by X-ray photoelectron spectroscopy. Under the optimum conditions, the recoveries of measured elements improved by 23% on average, and the recoveries of elements with high-melting oxides (Sr, Zr, and Th) improved by as much as 36%. These results indicate that vaporization, atomization, and ionization in the ICP improved when HCl gas was merged with the ablated particles.
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  • Xiaodan ZENG, Mingshuo MA, Baocun ZHU, Lin ZHU
    Type: Original Papers
    2016 Volume 32 Issue 12 Pages 1291-1294
    Published: December 10, 2016
    Released: December 10, 2016
    JOURNALS FREE ACCESS
    A fluorescent probe 1 has been successfully developed to determine human serum albumin (HSA). Probe 1 expresses a dramatic fluorescence enhancement to HSA without interference from other amino acids. Under the optimal conditions, the calibration graphs are linear over the range of 0 – 13.3 μg/mL with the limit of determination of 0.61 μg/mL. Thus, this probe shows high sensitivity and selectivity to HSA.
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  • Malay DOLAI, Rabiul ALAM, Atul KATARKAR, Keya CHAUDHURI, Mahammad ALI
    Type: Original Papers
    2016 Volume 32 Issue 12 Pages 1295-1300
    Published: December 10, 2016
    Released: December 10, 2016
    JOURNALS FREE ACCESS
    A newly designed oxime based probe, 2,4-dihydroxyacetophenone-oxime (DHAO), was found to recognize H2AsO4 selectively with ∼3 fold "turn-on" fluorescence enhancement and LOD of 29 μM, K = (2.10 ± 0.54) × 104 M–1 in purely aqueous medium. The structures of the DHAO and its adduct with H2AsO4 were optimized by DFT calculations. Intracellular imaging of As(V) in HepG2 cells demonstrate the possibilities of in vitro/in vivo applications for selective monitoring of such species.
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  • Yanbei ZHU, Akihide ITOH
    Type: Original Papers
    2016 Volume 32 Issue 12 Pages 1301-1305
    Published: December 10, 2016
    Released: December 10, 2016
    JOURNALS FREE ACCESS
    A method for direct and precise determination of Cd in seawater by ICP-QMS/QMS was developed, where a high matrix introducing unit permitted the direct introduction of seawater without clogging the cones while the matrix effect of seawater was canceled by standard addition. NH3 gas was selected as the reaction gas for removing the MoO interferences with the measurement of Cd isotopes, effectively improving the signal to background ratio. The lower limit of detection obtained at 114Cd was 0.0002 ng mL–1, which is enough for the determination of Cd in natural seawater. The validity of the present method was confirmed by the analysis of two certified reference materials, i.e. NASS-5 and NASS-6, whose observed values of Cd concentration agreed with the certified values. The analytical figures of merit of the present method were comparable to or better than those reported for direct analysis of seawater.
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  • Naoki SASAKI, Mariko TATANOU, Tomoko SUZUKI, Yasutaka ANRAKU, Akihiro ...
    Type: Original Papers
    2016 Volume 32 Issue 12 Pages 1307-1314
    Published: December 10, 2016
    Released: December 10, 2016
    JOURNALS FREE ACCESS
    Nanoparticles have been widely utilized to deliver drugs from blood vessels to target tissues. A crucial issue concerning nanoparticle-based drug delivery is to discuss the relationship between experimentally-obtained permeability and physical parameters. Although nanoparticles can permeate vascular pores, because the size and shape of the pores are essentially non-uniform, conventional animal testing and recent cell-based microfluidic devices are unable to precisely evaluate the effects of physical parameters (e.g. pore size and nanoparticle size) on permeation. In this study, we present a membrane-integrated microfluidic device to study permeation of nanoparticles through straight micropores. Porous membranes possessing uniform straight pores were utilized. The effects of pore size and pressure difference across the pores on nanoparticle permeation were examined. The experimentally determined permeability coefficient of 1.0 μm-pore membrane against 100 nm-diameter nanoparticles agreed well with the theoretical value obtained for convectional permeation. Our method can be utilized to clarify the relationship between the experimentally-obtained permeability and physical parameters, and will help rational design of nanomedicines.
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  • Burcu BEKDESER, Mustafa ÖZYÜREK, Esin AKYÜZ, Resat APAK
    Type: Original Papers
    2016 Volume 32 Issue 12 Pages 1315-1320
    Published: December 10, 2016
    Released: December 10, 2016
    JOURNALS FREE ACCESS
    In this study, a novel fluorometric method for the determination of peroxynitrite anion (ONOO) scavenging (PAS) activity of amino acids and biothiols, which can mostly trap peroxynitrite in vivo, is described. This assay is based on the conversion of a gentisic acid probe to its non-fluorescent oxidation products with ONOO. The attenuation of the fluorescence intensity (FI) of the probe upon peroxynitrite attack is diminished with antioxidants, the difference in FI being related to the PAS activity of the antioxidants. The IC50 (50% inhibitive concentration) values of biothiols, amino acids and tissue homogenates were estimated, in comparison with the reference Pyrogallol Red (PR) bleaching method. PR is the most suitable and frequently used dye to determine PAS activity, but is relatively insensitive. The developed fluorometric assay is highly sensitive to allow determinations of the PAS activity of amino acids.
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  • Shelja TIWARI, Niharika SHARMA, Reena SAXENA
    Type: Original Papers
    2016 Volume 32 Issue 12 Pages 1321-1325
    Published: December 10, 2016
    Released: December 10, 2016
    JOURNALS FREE ACCESS
    An online preconcentration system based on solid-phase extraction was developed for speciation and determinations of Cr in industrial water samples using flame atomic absorption spectrometry. A minicolumn packed with Amberlite XAD-16 loaded with salicylic acid was used to preconcentrate chromium species. All flow and chemical parameters that influence sorption were studied. The preconcentration factor and detection limit for the preconcentration time of 120 s were 79 and 0.10 μg L–1, respectively. The concentration of Cr(VI) species was calculated by the difference of the total Cr and Cr(III). The relative standard deviation (RSD) (five replicate of measurements) for 50 and 100 μg L–1 Cr(III) solution was 1.2 and 1.0% respectively. The accuracy of the method was verified by analyzing a standard reference material (NIST SRM 1640a, trace elements in natural water). The proposed preconcentration method was successfully applied to the determination of Cr species in industrial water samples with satisfactory results.
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  • Toshio TAKAYANAGI, Natsumi SHIMAKAMI, Masashi KURASHINA, Hitoshi MIZUG ...
    Type: Original Papers
    2016 Volume 32 Issue 12 Pages 1327-1332
    Published: December 10, 2016
    Released: December 10, 2016
    JOURNALS FREE ACCESS
    The acid-base equilibrium of hexamethylenetetramine (hexamine) was analyzed with its effective electrophoretic mobility by capillary zone electrophoresis. Although hexamine is degradable in a weakly acidic aqueous solution, and the degraded products of ammonia and formaldehyde can be formed, the effective electrophoretic mobility of hexamine was measured in the pH range between 2.8 and 6.9. An acid-base dissociation equilibrium of the protonated hexamine was analyzed based on the mobility change, and an acid dissociation constant of pKa = 4.93 ± 0.01 (mean ± standard error, ionic strength: 0.020 mol dm–3) was determined. The monoprotic acid-base equilibrium of hexamine was confirmed through comparisons of its electrophoretic mobility with the N-ethylquinolinium ion and with the monocationic N-ethyl derivative of hexamine, as well as a slope analysis of the dissociation equilibrium.
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  • Shubo DONG, Zhengyu YAN, Hanyue YANG
    Type: Original Papers
    2016 Volume 32 Issue 12 Pages 1333-1338
    Published: December 10, 2016
    Released: December 10, 2016
    JOURNALS FREE ACCESS
    A rapid and sensitive high-performance liquid chromatography–mass spectrometry method was established to determine the trace residues of piperazine in vortioxetine hydrobromide. The presence of piperazine was determined by precolumn derivatization with dansyl chloride. Chromatographic separation was performed on a Waters SunFire C8 column (150 × 4.6 mm, 3.5 μm) in gradient elution mode, using formic acid and acetonitrile as mobile phase. Detection was performed in a single quadrupole mass spectrometer in single ion monitoring mode using positive ionization. An m/z value of 553 was selected for monitoring disubstituted piperazine by DNS-Cl. Linearity, accuracy, and precision were found to be acceptable over the piperazine concentration range of 0.3525 – 2.35 ng mL–1. The limit of detection and limit of quantification of piperazine were 0.1175 and 0.3525 ng mL–1, respectively, which complied with the requirements of qualitative and quantitative analyses. The method was deemed sensitive and efficient.
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  • Manoj Kumar PANDEY, Kenjiro HASHI, Shinobu OHKI, Gen NISHIJIMA, Shinji ...
    Type: Original Papers
    2016 Volume 32 Issue 12 Pages 1339-1345
    Published: December 10, 2016
    Released: December 10, 2016
    JOURNALS FREE ACCESS
    Solid-state NMR observations of low-gamma half-integer quadrupolar nuclei, 35Cl and 37Cl, were demonstrated using a 24 T hybrid magnet (1H resonance frequency of 1.02 GHz) comprised of the high-temperature (HTS) and low-temperature (LTS) superconductors, and compared with results using a 14.1 T standard NMR magnet. While at 24 T the linewidth is 1.7 times narrower than that at 14.1 T, the gain in the sensitivity is 7.0 times because of enhanced polarization, reduced linewidth, and the use of larger rotor. A simple theoretical model was used to rationalize the sensitivity enhancements. The ratio of 35Cl and 37Cl quadrupolar couplings agrees well with the ratio of quadrupolar moments, and no isotope-dependent chemical shift has been observed. In addition, the 3QMAS spectrum of 35Cl is shown to demonstrate the high sensitivity rendered by the 24 T spectrometer.
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  • Kazuaki OHARA, Masahide TOMINAGA, Hyuma MASU, Isao AZUMAYA, Kentaro YA ...
    Type: Original Papers
    2016 Volume 32 Issue 12 Pages 1347-1352
    Published: December 10, 2016
    Released: December 10, 2016
    JOURNALS FREE ACCESS
    Bidentate organic molecules with imidazole or benzimidazole moieties connected to a rigid 1,3-diphenyladamantane spacer are simple and unique building blocks that facilitate the assembly of supramolecular architectures in the solid state via metal-coordination. Single-crystal X-ray analysis revealed that the complexation of bidentate ligand-bearing imidazole moieties with cobalt(II) or cadmium(II) ions in methanol/chloroform produced complexes that showed doubly-interpenetrated two-dimensional (2D) sheets through the formation of coordination bonds between the cobalt or cadmium metal centers and the nitrogen atoms of the imidazole groups. In the complexation of another ligand bearing a bulky benzimidazole group with cobalt(II) ion generated in methanol/chloroform, extended zigzag one-dimensional (1D) chains were formed, indicating that the molecular shape and bulkiness of the ligand design are crucial in the control of coordination polymers. The crystallization solutions were subjected to cold-spray ionization mass spectrometry (CSI-MS), and ion peaks derived from complexes with metal-ligand 1:2 and 1:1 were observed in complexation with ligands bearing the imidazole and benzimidazole moieties, respectively. The metal-ligand ratio in the CSI-MS analysis was identical to that found in the single-crystal X-ray analysis of an independent molecule. In addition, coordination oligomers with large molecular weight were detected as part of the obtained coordination polymers observed by CSI-MS/MS.
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  • Daichi OKUNO, Minako HIRANO, Hiroaki YOKOTA, Yukiko ONISHI, Junya ICHI ...
    Type: Original Papers
    2016 Volume 32 Issue 12 Pages 1353-1357
    Published: December 10, 2016
    Released: December 10, 2016
    JOURNALS FREE ACCESS
    The artificial bilayer single-channel recording technique is commonly used to observe detailed pharmacological properties of various ion channel proteins. It permits easy control of the solution and membrane lipid composition, and is also compatible with pharmacological screening devices. However, its use is limited due to low measurement efficiency. Here, we develop a novel artificial bilayer single-channel recording technique in which bilayers are made and channels are reconstituted into the membranes by contacting a gold electrode to the lipid-solution interface. Using this technique, we measured the single-channel currents of two channel-forming peptides, gramicidin and alamethicin, and a channel-forming protein, α-hemolysin. This technique requires only one action, allowing the technique to potentially be combined with high-throughput screening devices.
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Notes
Advancements in Instrumentation
  • Masayuki UEHARA
    Type: Advancements in Instrumentation
    2016 Volume 32 Issue 12 Pages 1375-1379
    Published: December 10, 2016
    Released: December 10, 2016
    JOURNALS FREE ACCESS
    We have developed a rapid genetic testing system integrating nucleic acid extraction, purification, amplification, and detection in a single cartridge. The system performs real-time polymerase chain reaction (PCR) after nucleic acid purification in a fully automated manner. RNase P, a housekeeping gene, was purified from human nasal epithelial cells using silica-coated magnetic beads and subjected to real-time PCR using a novel droplet-real-time-PCR machine. The process was completed within 13 min. This system will be widely applicable for research and diagnostic uses.
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  • Takeshi KONDO, Masaki HOSHINO, Takeshi WATANABE, Tatsuo AIKAWA, Makoto ...
    Type: Advancements in Instrumentation
    2016 Volume 32 Issue 12 Pages 1381-1384
    Published: December 10, 2016
    Released: December 10, 2016
    JOURNALS FREE ACCESS
    Electrolytic cells for electrochemical oxygen demand (ECOD) measurements based on total electrolytic decomposition at a boron-doped diamond (BDD) electrode were developed for rapid measurement of organic pollutants at low concentrations. Using improved electrolytic cells designed for efficient mass transfer, the ECOD for 10 μM potassium hydrogen phthalate (theoretical ECOD: 2.3 mg-O2 L–1) was determined in a relatively short electrolysis time. Thus, ECOD measurements using these cells would be useful for estimating organic water pollution in industrial waste and lake water.
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