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Published By "Institute Of Organic Chemistry & Biochemistry, Academy Of Sciences Of The Czech Republic"

1212-6950, 0010-0765

2011 ◽  
Vol 76 (4) ◽  
pp. 327-341 ◽  
Vladimír Špirko ◽  
Xiangzhu Li ◽  
Josef Paldus

Recently generated ground state potential energy curves (PECs) for the nitrogen molecule, as obtained with the reduced multireference (RMR) coupled-cluster (CC) method with singles and doubles (RMR-CCSD), and its version corrected for the secondary triples RMR-CCSD(T), using cc-pVXZ basis sets with X = D, T, and Q, as well as the extrapolated complete basis set (cbs) limit (X. Li and J. Paldus: J. Chem. Phys. 2008, 129, 054104), are compared with both the highly accurate theoretical configuration interaction PEC of Gdanitz (Chem. Phys. Lett. 1998, 283, 253) and analytic PECs obtained by fitting an extensive set of experimental data (R. J. Le Roy et al.: J. Chem. Phys. 2006, 125, 164310). These results are analyzed using a morphing procedure based on the reduced potential curve (RPC) method of Jenč. It is found that an RPC fit of both theoretical potentials can be achieved with only a few parameters. The RMR PECs are found to provide an excellent description of experimentally available vibrational levels, but significantly deviate from those of Gdanitz’s PEC for highly stretched geometries, yet still do provide a qualitatively correct PECs that lie within the region delimited by Le Roy’s analytical PECs.

2011 ◽  
Vol 76 (4) ◽  
pp. 277-294 ◽  
Roman Kanďár ◽  
Pavla Žáková ◽  
Miroslava Marková ◽  
Halka Lotková ◽  
Otto Kučera ◽  

We describe a relatively simple method for the determination of glutathione (GSH) and glutathione disulfide (GSSG) in human whole blood. We have used an HPLC with coulometric electrochemical detection for the simultaneous measurement of GSH and GSSG. Diluted and filtered trichloroacetic acid extracts were injected directly into the HPLC system and were eluted isocratically on a Polaris 5u C18-A, 250 × 4.6 mm analytical column. Glutathione in samples extracted with trichloroacetic acid and diluted with 1.0 mMhydrochloric acid was stable at 4 °C for at least 8 h. The analytical performance of this method is satisfactory: the intra-assay and inter-assay coefficients of variation were below 10%. Quantitative recoveries from spiked whole blood samples were at intervals 91.6–97.6% for GSH and 85.0–104.4% for GSSG. The linear range is 5.0–2000.0 μmol/l, with a detection limit of 2.1 μmol/l (signal-to-noise ratio = 3) for GSH and 2.0–250.0 μmol/l, with a detection limit of 0.9 μmol/l for GSSG.

2011 ◽  
Vol 76 (12) ◽  
pp. 1791-1797 ◽  
Wei-Lin Li ◽  
Jin-Ying Liang ◽  
Tian-Bao Wang ◽  
Ya-Qin Yang

FeCl3–SiO2 is environment-friendly heterogeneous catalyst for the condensation of kojic acid and aldehydes with dimedone to afford dihydropyrano[3,2-b]chromenediones. The solid acid catalyst is stable and can be easily recovered and reused without appreciable change in its efficiency.

2011 ◽  
Vol 76 (1) ◽  
pp. 65-74
Zdena Nováková ◽  
Jana Tomanová ◽  
Lucie Štěrbová ◽  
Pavel Drašar

New type of amide conjugates of steroid and bile acids with D-glucosamine 1 and 2 were prepared. Title compounds are prepared via acid chloride or using N-[({[(1E)-1-cyano-2-ethoxy-2-oxoethylidene]amino}oxy)(dimethylamino)methylidene]-N-methylmethanaminium tetrafluoroborate as condensation agent. They were examined for gelation properties with negative results. Per-O-acetylated D-glucosamine hydrochloride was prepared in one step procedure from D-glucosamine hydrochloride by acetylation in a mixture of acetyl chloride and acetic acid.

2011 ◽  
Vol 76 (12) ◽  
pp. 1699-1715 ◽  
Sławomira Skrzypek ◽  
Valentin Mirceski ◽  
Sylwia Smarzewska ◽  
Dariusz Guziejewski ◽  
Witold Ciesielski

Although 2-guanidinobenzimidazole (GBI; CAS: 5418-95-1) is a compound of biological interest, generally there is a lack of electrochemical studies and the methods of its determination. The GBI behavior at a mercury electrode was analyzed under conditions of linear sweep voltammetry (LSV), differential pulse voltammetry (DPV), square-wave voltammetry (SWV) and square-wave stripping voltammetry (SWSV). Although GBI is electrochemically inactive at mercury electrode it adsorbs at the mercury surface and catalyzes effectively the hydrogen evolution reaction. Theoretical analysis of two possible pathways, according to which the GBI electrode mechanism can be explained, is performed. Simple analysis of peak current and potential with respect to available time window, i.e. change of frequency can be helpful in discerning the character of the recorded SW current. The established electrode mechanism is assumed to involve a preceding chemical reaction in which the adsorbed catalyst (GBIads) is protonated and the protonated form of the catalyst (GBIH+(ads)) is irreversibly reduced at potential about –1.18 V vs Ag|AgCl (citrate buffer pH 2.5). New methods of voltammetric determination of 2-guanidinobenzimidazole were developed. The detection and quantifications limits were found to be 1 × 10–7, 1 × 10–6 mol l–1 (SWV); 8 × 10–8, 9 × 10–7 mol l–1 (SWSV); 4 × 10–7, 2 × 10–6 mol l–1 (DPV) and 6 × 10–7, 3 × 10–6 mol l–1 (LSV), respectively.

2011 ◽  
Vol 76 (5) ◽  
pp. 383-397 ◽  
Ferenc T. Pastor ◽  
Hana Dejmková ◽  
Jiří Zima ◽  
Jiří Barek

The possibility of determination of chloramphenicol by differential pulse voltammetry at four different carbon paste electrodes, in the full pH range (2–12) of Britton–Robinson (BR) buffer was investigated. Electrodes were prepared by mixing spectroscopic graphite powder or glassy carbon microbeads with mineral oil (Nujol) or tricresyl phosphate. Under optimal conditions (BR buffer pH 12, the electrode prepared from glassy carbon microbeads and tricresyl phosphate), linear calibration graph was obtained only in 10–5 M chloramphenicol concentration range. Determination of lower concentrations of chloramphenicol was complicated by irreproducible peak of oxygen from the carbon paste which overlapped with peak of chloramphenicol. Addition of sodium sulfite removed the oxygen peak without influence on the peak of chloramphenicol. Under optimal conditions (electrode paste made from glassy carbon microbeads, BR buffer pH 10 and 0.5 M sodium sulfite), straight calibration line was obtained in the 10–6 and 10–5 M chloramphenicol concentration range. Limit of determination was 5 × 10–7 mol/l.

2011 ◽  
Vol 76 (3) ◽  
pp. 159-176 ◽  
Ibrahim Hüdai Taşdemir ◽  
Orhan Çakirer ◽  
Nevin Erk ◽  
Esma Kiliç

Electrochemical properties and diffusion-adsorption behavior of risperidone (RPN), an antiphyscotic drug, on hanging mercury drop electrode (HMDE) were carried out in Britton–Robinson (BR) buffer. Some electrochemical parameters such as diffusion coefficient, number of transferred electrons and proton participated to its reduction mechanism and surface coverage coefficient were calculated from the results of cyclic voltammetry, square-wave voltammetry and constant potential electrolysis. RPN was found to be reduced with single two-electron/two-proton quasi-reversible mechanism controlled mainly by adsorption with some diffusion contribution at the potential about –1.58 V (vs Ag|AgCl electrode). Experimental parameters were optimized to develop a new, accurate, rapid, selective and simple square-wave cathodic adsorptive stripping voltammetric (SWCAdSV) method for direct determination of RPN in pharmaceutical dosage forms, spiked human urine and human serum samples without time-consuming steps prior to drug assay. This method was based on the relation between the peak current and the concentration of RPN and it was recognized that peak current of reduction wave linearly changes with the concentration of RPN in the concentration range of 1.5–150 nM, when optimum preconcentration potential –0.65 V and optimum preconcentration time 60 s were applied. In this method, limit of detection (LOD) was found as 5.18 nM (2.12 ppb). The method was successfully applied to determine the RPN content of commercial pharmaceutical preparations, spiked human serum and spiked human urine. The method was found to be highly accurate and precise, having a relative standard deviation of less than 4.80% for all applications.

2011 ◽  
Vol 76 (12) ◽  
pp. 1979-1990 ◽  
Reihaneh Malakooti ◽  
Sara Sobhani ◽  
Nasrin Razavi ◽  
Soheila Shafiei ◽  
Rezvan Mokhtari

Aminopropylated mesoporous SBA-15 silica (APMS) is introduced as a new, recyclable and efficient catalyst for the formylation of a variety of amines and alcohols by using readily available formic acid under solvent-free conditions.

2011 ◽  
Vol 76 (12) ◽  
pp. 1991-2004 ◽  
Vlastimil Vyskočil ◽  
Ivan Jiránek ◽  
Aleš Daňhel ◽  
Jiří Zima ◽  
Jiří Barek ◽  

Electrochemical behavior of genotoxic nitro derivatives of quinoline, namely 5-nitroquinoline (5-NQ), 6-nitroquinoline (6-NQ) and 8-nitroquinoline (8-NQ), was investigated by DC tast polarography (DCTP) and differential pulse polarography (DPP), both at a classical dropping mercury electrode (DME), and by differential pulse voltammetry (DPV) and adsorptive stripping differential pulse voltammetry (AdSDPV), both at a miniaturized hanging mercury drop minielectrode (HMDmE), in buffered aqueous (for 5-NQ) or aqueous-methanolic (for 6-NQ and 8-NQ) solutions. Optimum conditions were found for the determination of 5-NQ, 6-NQ and 8-NQ by DCTP at DME (with limits of quantification, LQ ≈ 9 × 10–7, 3 × 10–7 and 2 × 10–6 mol l–1, respectively), by DPP at DME (LQ ≈ 1 × 10–8, 9 × 10–8 and 1 × 10–7 mol l–1, respectively), by DPV at HMDmE (LQ ≈ 2 × 10–8, 1 × 10–7 and 1 × 10–7 mol l–1, respectively), and by AdSDPV at HMDmE (LQ ≈ 1 × 10–8 mol l–1 for 8-NQ; an attempt at increasing the sensitivity using AdSDPV at HMDmE was not successful for 5-NQ and 6-NQ). Practical applicability of the developed methods was verified on the direct determination of the studied compounds in model samples of drinking and river water in submicromolar concentrations and on the determination in model samples of drinking and river water using preliminary separation and preconcentration by solid phase extraction (SPE) in nanomolar concentrations.

2011 ◽  
Vol 76 (9) ◽  
pp. 1133-1139 ◽  
Pham Thi Nhat Trinh ◽  
Nguyen Cong Hao ◽  
Phan Thanh Thao ◽  
Le Tien Dung

From the ethanol extract of Drynaria fortunei (KUNZE) J. Sm., a new phenylpropanoid glycoside, fortunamide (1), was isolated and characterized by spectroscopic methods. Together with a new glycoside, 9 known compounds, including three curcuminoids (2–4), two isoprenylated flavonoids (5, 6), two flavonoids (7, 8), one monoterpenoid (9) and one phenolic acid (10) were isolated and identified by spectral data analysis from the rhizomes of Drynaria fortunei (KUNZE) J. Sm. Eight of them were isolated from Drynaria fortunei (KUNZE) J. Sm. for the first time.

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