الفهرس 
Doping DrugsOnly 14 pages are availabe for public view
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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.