الفهرس 
LITERATURE SURVEY
Chromatographic methodsOnly 14 pages are availabe for public view
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Abstract
(1) Chapter I:
A literature survey was presented on nalbuphine hydrochloride (NP.HCl), ritodrine hydrochloride (RT.HCl) and cinchocaine hydrochloride (CC.HCl) concerning their biological activities, micro determination at various electrodes. A literature survey on the preparation of ZrO2 nano particles was studied using X- ray diffraction (XRD), transmission electron microscope (TEM), scanning electron microscope (SEM), UV spectroscopy and IR analysis, in order to elucidate the formation of ZrO2 nano particles.
(2) Chapter II:
It includes the experimental part, the material, solutions, instruments used and working procedures.
(3) Chapter III:
First part:
It includes the results that confirm the formation of ZrO2 nano particles, XRD gave the mean grain size of ZrO2 crystals that can be calculated from the peak width using the Debye-Scherrer’s formula. It follows the structural characterization of ZrO2 where it exists mainly in three phases, monoclinic, tetragonal, and cubic. The average crystalline size according to the X-ray phase analysis data for the sample C (51% cubic phase and 49% tetragonal phase) was more than other samples (A, B and D). SEM images shown that the particle size of the combustion product was significantly different and the particle shape was regular when calcination was carried out at high temperature and yttrium oxide as stabilizer contrast in low temperature and without stabilizer. TEM pictures of the ZrO2 nano particles showed that the average diameter of the prepared ZrO2 nanoparticle is about 10-21, 14-25, 6-17 and 9-19 nm for A, B, C and D samples, respectively, and has a very narrow particle distribution. At absorption spectra (271 nm) for samples C and D The obtained data agree with the information that the band gap energy for cubic zirconia is 3.8-6.1 eV. IR spectra of zirconium oxide samples essentially showed the various stretching frequencies at 1600 cm-1 in sample B and C. This feature almost disappears as in other samples and this may be due to carbonate related signature.
Second part:
Simple, rapid and reliable voltammetric methods were adopted for the micro determination of NP.HCl, RT.HCl and CC.HCl drugs via oxidation-reduction reaction using carbon past electrode (CPE), modified nano ZrO2 carbon past electrode (ZrO2-MCPE), graphite pencil electrode (GPE) and glassy carbon past electrode (GCE). The effect of different parameters was studied.
Cyclic voltammetry, differential pulse voltammetry and square wave voltammetry were used to explore the oxidation behavior of NP.HCl, RT.HCl and CC.HCl and also reduction behavior of CC.HCl. The oxidation peaks of NP.HCl were obtained in Britton-Robinson buffer of pH 6 and 7 at GPE and GCE electrodes, respectively, pH 9 at CPE and ZrO2-MCPE electrodes. The diffusion response was evaluated as a function of some variables such as the scan rate and pH. For determination of NP. HCl, a linear calibration graphs were obtained from 2.0 × 10-5 to 24.5 × 10-5, 6.66 × 10-7 to 73.3 × 10-7, 16 × 10-6 to 15 × 10-5 and 12.5 × 10-6 to 13.75 × 10-5 mol L-1 by using differential pulse at CPE, ZrO2-MCPE, GPE and GCE electrodes, respectively. Also a linear calibration graphs were obtained stabilizer contrast in low temperature and without stabilizer. TEM pictures of the ZrO2 nano particles showed that the average diameter of the prepared ZrO2 nanoparticle is about 10-21, 14-25, 6-17 and 9-19 nm for A, B, C and D samples, respectively, and has a very narrow particle distribution. At absorption spectra (271 nm) for samples C and D The obtained data agree with the information that the band gap energy for cubic zirconia is 3.8-6.1 eV. IR spectra of zirconium oxide samples essentially showed the various stretching frequencies at 1600 cm-1 in sample B and C. This feature almost disappears as in other samples and this may be due to carbonate related signature.
Second part:
Simple, rapid and reliable voltammetric methods were adopted for the micro determination of NP.HCl, RT.HCl and CC.HCl drugs via oxidation-reduction reaction using carbon past electrode (CPE), modified nano ZrO2 carbon past electrode (ZrO2-MCPE), graphite pencil electrode (GPE) and glassy carbon past electrode (GCE). The effect of different parameters was studied.
Cyclic voltammetry, differential pulse voltammetry and square wave voltammetry were used to explore the oxidation behavior of NP.HCl, RT.HCl and CC.HCl and also reduction behavior of CC.HCl. The oxidation peaks of NP.HCl were obtained in Britton-Robinson buffer of pH 6 and 7 at GPE and GCE electrodes, respectively, pH 9 at CPE and ZrO2-MCPE electrodes. The diffusion response was evaluated as a function of some variables such as the scan rate and pH. For determination of NP. HCl, a linear calibration graphs were obtained from 2.0 × 10-5 to 24.5 × 10-5, 6.66 × 10-7 to 73.3 × 10-7, 16 × 10-6 to 15 × 10-5 and 12.5 × 10-6 to 13.75 × 10-5 mol L-1 by using differential pulse at CPE, ZrO2-MCPE, GPE and GCE electrodes, respectively. Also a linear calibration graphs were obtained from 2.0 × 10-5 to 48 × 10-5, 6.66 × 10-7 to 10.66 × 10-6, 16 × 10-6 to 15 × 10-5 and 2.5 × 10-6 to 2.75 × 10-5 mol L-1 by using square wave voltammetry at CPE, ZrO2-MCPE, GPE and GCE electrodes, respectively. The scan rate was studied from 20-240 Vs-1, and the number of electron involved in the reaction was calculated. It is found to be one electron. The method was applied for determination of NP.HCl in raw material, biological fluid (urine) and pharmaceutical preparation (Nalufin). The results obtained were compared with those obtained from the official methods.
Third part
Cyclic voltammetry was used to explore the oxidation behavior of RT.HCl. The oxidation peaks of RT.HCl were obtained in Britton-Robinson buffer of pH 8 and 7 for ZrO2-MCPE and GCE electrodes, respectively, and at pH 9 for CPE and GPE electrodes. For the determination of RT.HCl, the diffusion response was evaluated as a function of some variables such as the scan rate and pH. A linear calibration graphs were obtained from 3.33 × 10-6 to 4.33 × 10-5, 6.67 × 10-8 to 7.33 × 10-7, 4 × 10-6 to 5.2 × 10-5 and 5 × 10-6 to 4 × 10-5 mol L-1 by using differential pulse at CPE, ZrO2-MCPE, GPE and GCE electrodes, respectively. Also a linear calibration graphs were obtained from 1.33 × 10-6 to 1.47 × 10-5, 3.33 × 10-8 to 3.67 × 10-7, 4 × 10-6 to 6 × 10-5 and 5 × 10-6 to 4 × 10-5 mol L-1 by using square wave voltammetry at CPE, ZrO2-MCPE, GPE and GCE, respectively. The scan rate was studied from 20-240 Vs-1 and the number of electron involved in the reaction was calculated where it was found to be two electrons. The method was applied to determination of RT.HCl in raw material, biological fluid (urine) and pharmaceutical preparation (Yutopar). The results obtained were compared with those obtained from the official methods.
Fourth part
Voltammetric techniques were used to explore the oxidation behavior of CC.HCl. The oxidation peaks of CC.HCl were obtained in Britton-Robinson buffer of pH 7 and 9 for ZrO2-MCPE and GPE electrodes, respectively, and at pH 5for CPE and GCE electrodes. The diffusion and adsorption responses were evaluated as a function of some variables such as the scan rate and pH. The determination of CC.HCl at oxidation process a linear calibration graphs were obtained from 2.67 × 10-6 to 3.47 × 10-5, 1.3 × 10-8 to 3.46 × 10-7, 1.5 × 10-6 to 1.8 × 10-5 and 1.25 × 10-6 to 1.37× 10-5 mol L-1 by using differential pulse at CPE, ZrO2-MCPE, GPE and GCE, respectively. Also a linear calibration graphs were obtained from 1.67 × 10-6 to 2.33 × 10-5, 1.3 × 10-8 to 2.86 × 10-7, 1 × 10-6 to 1.1 × 10-5 and 2.5× 10-6 to 3 × 10-5 mol L-1 by using square wave voltammetry at CPE, ZrO2-MCPE, GPE and GCE electrodes, respectively. CC.HCl drug also undergoes reduction process at CPE and GPE electrodes at pH 7. A linear calibration graphs were determined at reduction process. The scan rate was studied from 20-240 Vs-1 and the number of electron involved in the reaction was calculated it found to be one electrons in both oxidation and reduction processes. The method was applied to determination of CC.HCl in raw material and biological fluid (urine). The results obtained were compared with those obtained from the official methods.