الفهرس 
General introductionOnly 14 pages are availabe for public view
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Abstract
; This thesis is devoted to the analysis of metal ions ( copper aluminum) , and some pharmaceutical compounds (diclofenac Inn, aminoglycosides, heparin sodium and insulin) . Moreover the fcis is also devoted to determine chemical properties of some frmaceutical compounds using computer calculator. The thesis prises six main parts:
TRACE ANALYSIS OF COPPER IONS
INTRODUCTION
It is an introduction reviewing the different methods reported ■r the determination of copper ions.
[t2 PROPOSED SENSITIVE COLORIMETRIC DETERMINATION OF COPPER (II)
IONS IN SOME CHEMICALS AND MULTIVITAMINS
This chapter describes a sensitive and selective colorimetric ’method for the micro-determination of copper (II) ions in pure form, in some chemicals and multivitamin preparations. The method [is based on the formation of stable blue complexes in an ammonia media (XM« 615 nm) between copper ions, oxalyldihydrazide and one of the following aldehydes: 4-nitrobenzaldehyde, 2-nitrocinmmaldehyde and formaldehyde with minimum detection limits 0.1,0.16 and 1.1 ppm, respectively. Other metal ions do not interfere. The optimum reaction conditions were studied and the results obtained were compared favorably to the diethyldithiocarbamte method.
t2 PROPOSED HPLC DETERMINATION OF TRACES OF COPPER (II) IONS IN
TAP WATER, BIOLOGICAL FLUIDS AND PHARMACEUTICALS.
This chapter describes a selective HPLC procedure for the determination of copper (II) ions in tap water, in biological fluids and in pharmaceutical preparations. The method is based on Che formation of a dithiocarbamic acid -copper complex. Pindolol fas chosen as the secondary amine to react with carbon disulfide for the formation of dithiocarbamic acid. HPLC separation of the ;omplex formed was achieved on a Licrosorb RP18 column, using icetonitrile-acetate buffer (pH 5.5) as the mobile phase with jpectrophotometric detection at 270 nm and 435 nm. The optimum reaction conditions were studied. The minimum detection limit was 1.24 ppm copper (II) ions and the results obtained were compared avorably to the diethyldithiocarbamte method.
’art II SPECTROPHOTOMETRIC DETERMINATION OF ALUMINUM AND COPPER
IONS USING SPADNS. tl INTRODUCTION FOR ALUMINUM ION
It is an introduction reviewing the different methods reported or the determination of aluminum ions.
£2 PROPOSED METHOD FOR DETERMINATION OF ALUMINUM AND COPPER IONS.
This chapter describes a selective spectrophotometric rocedure for the determination of aluminum and copper ions. The
method is based on the formation of colored complexes with spadns
land these ions. These complexes have a maximum absorbance at 580
I run. The complexes formed with both cations are stable and pH
[dependant; aluminum is favorably complexed at pH 5, while copper
complexed at pH 7. The percentage recoveries were found to be 99.69
+0.75 and 99.32 ± 0.6 with a minimum detection limit of 0.08 and
!0.23 ug ml”1 for aluminum and copper ions respectively. There is
insignificant interference from 10 folds greater concentration of
other metal ions under the proposed reaction conditions.
PART HI LANTHANIDE PROBE ION SPECTROSCOPY IN PHARMACEUTICALS AND
BIOLOGICAL FLUIDS. IIL INTRODUCTION
It is an introduction for the applications of lanthanide ion probes in Pharmaceuticals and biological fluids. ILL DETERMINATION OF DICLOFENAC SODIUM.
III. 1.1 INTRODUCTION
It is an introduction reviewing the different methods reported for the determination of diclofenac sodium.
III. 1.2 PROPOSED METHOD FOR DETERMINATION OF DICLOFENAC SODIUM
This chapter describes a new method for the determination of Hiclofenac sodium in bulk and in pharmaceutical preparations using Su3+ ions as the fluorescent probe. The technique was built around
the hypersensitive property of the transitions of the fluorescent probe ion, Eu3+, at 616 nm. This transition is normally a forbidden transition, but the interaction with diclofenac sodium, which contains a carboxylic group, makes the transition allowed and enhances the intensity of its fluorescence emission. The Eu3 + fluorescence emission at 592 nm, comes from a non hypersensitive transition and is not affected by ligation. The intensity ratio, R, defined as I592/I616/ was used as a measure of percentage of probe ions bound. Diclofenac and Eu3+ forms (1:1) molar complex. The relative stability constant of the complex was found to be 10s. A linear relationship between bound Eu3+ and concentration of diclofenac sodium was found for concentrations from 10 to 200 ug.mL” ’with a recovery percentage of 100.22 ± 2.27. The method shows good agreement with a spectrophotometric method.
III-2 DETERMINATION OF AMINOGLYCOSIDE ANTIBIOTICS . III.2.1 INTRODUCTION.
It is an introduction reviewing the different methods reported for the determination of aminoglycoside antibiotics.
HI.2.2 PROPOSED METHOD FOR DETERMINATION OF AMINOGLYCOSIDE
ANTIBIOTICS
This chapter describes the application of probe ion Eluorimetry for the microdetermination of six aminoglycoside antibiotics; neomycin, streptomycin, gentamicin, tobramycin,
■nikacin and kanamycin as sulphate salts in pure form and in some pharmaceutical preparations. The method is based on the reaction of IEU3+ ions with aminoglycosides through amino and hydroxy groups. Buch interactions enhance the intensity of the 616 nm fluorescence
■ emission of the Eu 3+ ion. The fluorescence at 592 nm, comes from
■ non hypersensitive transition and is not affected by the ligand Bhich is bound to the probe ions. The intensity ratio R, defined as ■S92/I6]6 was used to determine the amount of free and bound europium lions. A linear relationship between bound europium ions and I aminoglycoside was found within concentration ranges, 20 to 100 ppm [for neomycin, 5 to 60 ppm for streptomycin, and 10 to 70 ppm for
gentamicin, tobramycin, amikacin, and kanamycin as sulphate salts. I Percentage recoveries range from 99.22 to 101.07 with standard deviations ranging from ± 1.5 to + 4.38. The relative stability constants ranged from 5X103 to 2X1O4. The optimum reaction conditions were studied and the results obtained compared favorably with the fluorimetric method using fluorescmine reagent.
III-3 DETERMINATION OF HEPARIN SODIUM. HI.3.1 INTRODUCTION.
It is an introduction reviewing the different methods reported for the determination of heparin.
Ill.3.2 PROPOSED METHOD FOR DETERMINATION OF HEPARIN SODIUM
This chapter describes a sensitive, rapid, accurate and
recise procedure for the microdetermination of heparin sodium in ilk, in injection and in blood serum. The procedure was built round the fact that heparin possesses many active binding sites; irboxylic, hydroxylic, aiaino and sulphonated groups, which are :rongly bound to Eu3+ ions. Such binding enhances the europium fenission at 616 nm which is a forbidden transition. The emission ■of europium at 592 nm comes from a non hypersensitive transition ■and is not affected by the ligand which is bound to europium ions. I The intensity ratio R, defined as 1592/^616 was used to determine the 1 amount of free and bound europium ions. There was a linear ■relationship between bound europium ions and heparin sodium within ■ the concentration range 1- 12 ug. ml/1 ( 0.07 -0.84 USP.IN) . I Reaction conditions were studied and percentage recoveries was I 99.77 ± 1.68. The relative stability of the complex was 1.2E5 and the correlation coefficient was 0.99923. Heparin was isolated from serum using ECTEOLA-cellulose and Sephadex G25 columns. The method shows good agreement with an anilinonaphthalene-1-sulfonate (ANS) and protamine fluorometric method.
Part IV DETERMINATION OF INSULIN AND PHARMACEUTICAL PREPARATIONS
BY FLUOROIMMUNOASSAY USING FLUORESCAMINE IV. 1 INTRODUCTION.
It is an introduction reviewing the different methods reported for the determination of insulin.
IV.2
PROPOSED METHOD FOR DETERMINATION OF INSULIN
This chapter describes a sensitive fluoroimmunoassay method [for the determination of insulin in bulk and in pharmaceutical preparations. The method is based on isolation of insulin using an actigel ALD-antibody, followed by reaction with fluorescamine at pH 1.5. The reaction products exhibit a characteristic emission intensity at 478 nm (excitation at 398 nm) . Reaction conditions were studied and insulin was determined within the concentration range 0.2-2 ppm (0.0055- 0.055 lU.mL”1) . The percentage recovery was 100.37 ±2.90 and the correlation coefficient was 0.99883. The results obtained were compared favorably to the USP chromatographic method.
ESTIMATION OF IONIZATION pK, OF PHARMACEUTICAL SUBSTANCES
V.I
USING SPARC INTRODUCTION.
It is an introduction reviewing the different methods reported for the determination of j8-adrenergic blockers, benzodiazepines, arginine and niflumic acid.
V.2. PROPOSED ESTIMATION OF IONIZATION pK, OF PHARMACEUTICAL
SUBSTANCES
This chapter describes the prototype computer program SPARC to calculate the pK, values of some important pharmaceutical
substances. The SPARC calculated pK/s are in a good agreement with the reported values. The SPARC models proved to be suitable for estimating the pK/s of Beta-adrenergic blocking agents and benzodiazepine drugs. Ionization macroconstants, microconstants, zwitterionic equilibria, speciation curves as function of the pH and the isoelectric points of a semi-essential amino acid, arginine and the antiinflammatory niflumic acid were calculated.
Part VI.
This part is describing the instruments, materials, reagents and procedures.