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Abstract This thesis aims to synthesis and characterization of some lanthanide complexes. The prepared complexes were used to develop of a novel fluoremetric method for microdetermination of some doping drugs in pure form, biological fluid and in their pharmaceutical formulations. Four ligands were used during the thesis namely: acetylacetone (ACAC); 2 ,2’-bipyridine (Bipy); 1,1’-bi-2-naphthol (BINOL) and tetracycline-HCl (TC) and ten lanthanide complexes were prepared 1-10. The complexes 1, 2 and 3 were prepared by the reaction of ACAC, Bipy and BINOL with Eu(III) nitrate with molar ratio 2:1 ligand to metal respectively. Complexes 4, 5 and 6 were prepared by the reaction of ACAC, BINOL, and TC with Tb(III) nitrate with molar ratio 2:1 ligand to metal respectively; whereas the complexes 7, 8, 9 and 10 were prepared by reaction of ACAC, Bipy, BINOL and TC with Sm(III) nitrate respectively under the same experimental conditions. The ligands and their complexes have been characterized using elemental analysis, infrared spectroscopy, ultraviolet-visible spectroscopy, 1H NMR spectroscopy, molar conductivity, magnetic momentum, mass spectroscopy. On the basis of the physical and spectral data of the complexes 1-10 discussed, the structures of the complexes have been deduced and the representative structures have been illustrated. The complexes were used in determination of some doping drugs (such as testosterone, hydrochlorothiazide) using a simple, fast and sensitive Spectrofluorimetric analytical technique. The performances of these applications are optimized for some of doping drugs quantification in pure form, biological fluid and in their pharmaceutical formulations. The thesis is divided into 3 chapters: Chapter one: - This chapter contains general introduction on the doping drugs according to the published list of the World AntiDoping Agency (WADA). It includes also the principle and theory of fluoremetric analysis method and background of lanthanides luminescence with various ligands. In the latter literature review for lanthanides complexes and their uses in determination of doping drugs. Chapter two: - Includes the experimental part, involving preparation of various complexes, compounds and solutions, instruments and apparatus which were used during the thesis and working procedures. Chapter three: - Present the results of the prepared lanthanide complexes and their characterization as well as their applications in the determination of some doping drugs, and it is consist of four parts: Part one: Present the characterization of the used ligand. Part two: Present the characterization of the Eu(III)- complexes and their uses in the determination of some doping drugs. Part three: Present the characterization of the Tb(III)- complexes and their uses in the determination of some doping drugs. Part four: Present the characterization of the Sm(III)- complexes and their uses in the determination of some doping drugs. In the last, we present the sensitive Spectrofluorimetric method developed for the determination of testosterone, hydrochlorothiazide. The characteristic maximum emission fluorescence peak observed for testosterone at 615 nm, after its excitation at 385nm, was used as the basis for its quantities. Concentrations in the range 5.6×10-9ñ 3.1×10-5 mol L−1 could be quantitated rapidly by this method. The fluorescence process was pH dependent at pH 8.4 and the lower detection limit was 3.50 x 10-10 mol L−1 and the lower quantization limit was 1.0x 10-9 mol L−1 with average recovery ± RSD in urine was (99.11 ±0.43 %),, and serum was (98.87 ± 1.04 %). On other hand the characteristic maximum emission fluorescence peak observed for hydrochlorothiazide at 545 nm, after its excitation at 285nm, was used as the basis for its quantities. Concentrations in the range 1 ×10−8 - 1 ×10-5mol L−1 could be quantitated rapidly by this method. The fluorescence process was pH dependent at pH 6.3 and the lower detection limit was 4.5 ×10−9mol L−1 and the lower quantization limit was 1.4 x 10-8mol L−1 with average recovery ± RSD in tablet was (100.2 ± 1.46 %), urine was (100.04 ± 0.68 %), and serum was (98.95 ± 1.48 %). The high recovery percentage and low relative standard deviation of the proposed method reflects the high accuracy and precision. Moreover, the method is easy applicable to a wide range of concentrations, besides being less time consuming. |