• Title/Summary/Keyword: Differential pulse polarography (DPP)

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Electrochemical Behavior and Differential Pulse Polarographic Determination of Piperacillin Sodium

  • Hahn, Young-hee;Son, Ean-ji
    • Archives of Pharmacal Research
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    • v.23 no.3
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    • pp.197-201
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    • 2000
  • In an aqueous piperacillin sodium solution, a well-defined single wave or single peak was observed by direct current(DC) polarography or differential pulse polarography(DPP). The peak potential change per pH unit was -54 mV in the phosphate buffer at $18^{\circ}C$, which indicated that protons were involved in the electrochemical reduction of the 2,3-dioxopiperazine moiety of piperacillin sodium with a $H^{+}e^{-}$ ratio of one. Using a phosphate buffer of pH 4.3, the $1.0{times}10^{-7}$ M piperacillin sodium single peak could be determined by DPP with relative standard deviation of 1.6 %(n=3). Piperacillin sodium could be analyzed with-out interference from penicillin G-potassium, which enabled the employment of DPP as a fast and simple technique for monitoring the synthetic process of the antibiotic.

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A Study on the Trace Analysis of Germanium in Inorganic Matrices by Differential Pulse Polarography (Differential Pulse Polarography에 의한 무기물 시료 중 Germanium의 미량 분석에 관한 연구)

  • Shin, Ho-Sang;Oh, Yun-Suk;Shin, Hak-Soo
    • Analytical Science and Technology
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    • v.9 no.3
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    • pp.253-261
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    • 1996
  • Analytical method for the determination of trace germanium in inorganic matrices by differential pulse polarography(DPP) was studied. The reduction peak of germanium(IV) in perchloric acid solution containing 1, 2, 3-trihydroxy benzene appeared at -0.45V(vs. Ag/AgCl) and the peak current for germanium complex varied linearly with concentration variation. Factors affecting sensitivity and precision for germanium quantification were studied and detection limit under the investigated parameters was 1ng/ml. Inorganic samples were decomposed by fusion with potassium pyrosulfate. Serious interferences of Se(IV), Pb(II), As(III) for the determination of germanium were discussed. Interferences of these elements could be avoided by extraction of germanium from decomposed matrices by $CCl_4$ in 10M HCl solution. The germanium contents of inorganic samples(Pb bf. dust, Cu bf. dust, gneiss, Cu anode slime) were determined by the above method.

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Electrochemical Behavior and Differential Pulse Polarographic Determination of Rifampicin in the Pharmaceutical Preparations

  • Hahn, Young-Hee;Shin, Sun-Mi
    • Archives of Pharmacal Research
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    • v.24 no.2
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    • pp.100-104
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    • 2001
  • Differential pulse polarographic(DPP) analytical procedure for the rifampicin antibiotic, which can be applied to monitor its synthetic process from the starting antibiotic of rifamycin B or rifamycin SV has been developed based on the electrochemical reduction of an azomethine group. Rifampicin exhibited a cathodic peak due to the azomethine group in the side chain of 3-[(4-methyl-1-piperazinyl)imino]methyl moiety and another cathodic peak due to the carbonyl group in rifamycin SV by DPP. The experimental peak potential shift of an azomethine reduction was -73 mV/pH in the pH range between 3.0 and 7.5, agreeing with involvement of 4 e-and 5 $H^5$ in its reduction. By the cyclic voltammetric(CV) studies, the azomethine and the carbonyl reductions in rifampicin were processed irreversibly on the mercury electrode. The plot of peak currents vs. concentrations of rifampicin ranging $1.0{\times}10^{-7} M~$1.0{\times}10^{-5} M yielded a straight line with a correlation coefficient of 0.9996. The detection limit was $1.0{\times}10^{-8} M with a modulation amplitude of 50 mV DPP has been successfully applied for the determination of rifampicin in the pharmaceutical preparations.

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$^1H$ NMR Estimation of Multi-Redox potentials of Cytochrome $c_3$ from Desulfovibrio vulgaris Hildenborough

  • 박장수;강신원;최성낙
    • Bulletin of the Korean Chemical Society
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    • v.16 no.4
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    • pp.331-336
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    • 1995
  • The macroscopic and microscopic redox potentials of tetrahemoprotein, cytochrome c3 from Desulfovibrio vulgaris(Hildenborough) (DvH) were estimated from 1H NMR and differential pulse polarography(DPP). Five sets of NMR resonances were confirmed by a redox titration. They represent cytochrome c3 molecules in five macroscopic redox states. The electron transfer in cytochrome c3 involves four consecutive one-electron steps. The saturation transfer method was used to determine the chemical shifts of eight heme methyl resonances in five different oxidation states. Thirty two microscopic redox potentials were estimated. The results showed the presence of a strong positive interaction between a pair of particular hemes. Comparing the results with those of Desulfovibrio vulgaris Miyazaki F (DvMF), it was observed that the two proteins resemble each other in overall redox pattern, but there is small difference in the relative redox potentials of four hemes.

Determination of Chloramphenicol by Differential Pulse Polarography (미분 펄스 폴라로그래피에 의한 Chloramphenicol의 정량분석)

  • Younghee Hahn;Jung-Sun Jeon
    • Journal of the Korean Chemical Society
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    • v.36 no.4
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    • pp.552-557
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    • 1992
  • Chloramphenicol was studied by differential pulse polarography (DDP). A reduction peak which is dependent on pH of the solution appeared in the voltage range between zero and -1.50 volt vs. Ag/AgCl (sat. KCl) reference electrode. A plot of peak potentials (Ep) measured at room temperature (20$^{\circ}C$) vs. pH of the chloramphenicol solutions showed linear relationship changing slope (Ep/pH) at pH 8.9. The slope was -59.7 mV/pH in pH 2.7∼8.9 and -24.3 mV/pH in pH 8.9∼11.2, respectively. A log plot of peak currents (ip) vs. concentrations showed a linearity at the concentrations between 4.8 ${\times}$ 10$^{-7}$ M and 6.2 ${\times}$ 10$^{-5}$ M (0.16 ppm∼20 ppm) chloramphenicol in pH 8.0 ammonium buffer. Between the DPP method and the reference method measuring absorbance at 278 nm, the correlation coefficient was 0.996, which means an excellent linearity. The DPP method was able to detect degradation products of chloramphenicol in mild alkaline solution (pH = 8.0) more distinctly than the spectrophotometric method.

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Electrochemical Determination of Artemisinin in Artemisia annua L Herbal Tea Preparation and Optimization of Tea Making Approach (개똥쑥 약초차 제조에서 아르테미시닌의 전기화학적 측정과 차를 만드는 최적화로의 접근법)

  • Debnath, Chhanda;Dobernig, Andrea;Saha, Pijus;Ortner, Astrid
    • Journal of the Korean Chemical Society
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    • v.55 no.1
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    • pp.57-62
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    • 2011
  • Sometimes inhabitants in remote areas have inadequate or no access to modern medicines or medical services. They can get benefit in term of the treatment against malaria by cultivating selected breeding of A. annua and making teas or decoctions from the plant materials following the proper way of tea preparation. In order to have the maximum extraction efficiency for artemisinin, different ways of tea preparations of A. annua were investigated by applying the developed DPP method and described in this article. Tea was prepared by three different ways (cooking, without cooking with/without shaking and microwave oven) with different times. From the results, it has been found that higher concentration of artemisinin (84.7%) can be attained by following the approach for tea preparation without cooking with shaking for 15 minutes (R.S.D. 2.34%). The concentration of artemisinin decreases with cooking more than 1.5 min in microwave oven. The utmost extraction (88.9% of artemisinin) is possible to extract by shaking with boiled 5% ethanol in distilled water (R.S.D. 2.28%).

Electrochemical Properties of Pentadentate Binucleated Schiff Base Cobalt(Ⅱ) and Manganese(Ⅱ) Complexes in Nonaqueous Solvent (비수용매에서 이핵성 다섯자리 Schiff Base Cobalt(Ⅱ) 및 Manganese(Ⅱ) 착물들의 전기화학적 성질)

  • Ki-Hyung Chjo;Yong-Kook Choi;Song-Ju Lee;Seong-Seop Seo
    • Journal of the Korean Chemical Society
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    • v.36 no.3
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    • pp.428-441
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    • 1992
  • We synthesized a series of binuclear pentadentate Schiff base complexes such as $Co(Ⅱ)_2$ (BSPP)($H_2O)_2$, $Co(Ⅱ)_2$ (BSPD)($H_2O)_2$, $Mn(Ⅱ)_2$ (BSPP)($H_2O)_2$ and $Mn(Ⅱ)_2$ (BSPD)($H_2O)_2$, mononuclear pentadentate Schiff base complexes such as Co(Ⅱ)(BSP)($H_2O)$ and Mn(Ⅱ)(BSP)($H_2O)$. The composition of these complexes identified by IR, UV-visible spectrum, T.G.A., DSC, and elemental analysis. The electrochemical redox processes have been examined by cyclic voltammetry and differential pulse polarography with glassy carbon electrode in 0.1M TEAP-Py(-DMSO and -DMF) as a supporting electrolyte solution. As a result of electrochemical measurements, the reduction processes for pentadentate binuclear Schiff base cobalt(Ⅱ) and manganese(Ⅱ) complexes occurred to four steps in $M(Ⅲ)_2$ / $Mn(Ⅱ)_2$ and $Mn(Ⅱ)_2$ / $M(Ⅰ)_2$ (M; Co, Mn) two processes through each two reduction steps with one electron, by contrast, the mononuclear pentadentate Schiff base cobalt(Ⅱ) and manganese(Ⅱ) complexes occurred to two steps in M(Ⅲ) / M(Ⅱ) and M(Ⅱ) / M(Ⅰ) (M; Co, Mn) two processes with one electron reduction steps.

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