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العنوان
Analytical Studies on some selected Antibiotics/
المؤلف
El Naggar, Mai Medhat.
هيئة الاعداد
باحث / مي مدحت النجار
مشرف / فوزي اسماعيل الياظبي
مشرف / طارق فتح الله بلال
مشرف / دينا احمد عبد الجواد
الموضوع
Pharmaceutical Analytical Chemistry. Antibiotics.
تاريخ النشر
2019.
عدد الصفحات
147 p. :
اللغة
الإنجليزية
الدرجة
ماجستير
التخصص
العلوم الصيدلية
تاريخ الإجازة
1/1/2019
مكان الإجازة
جامعة الاسكندريه - كلية الصيدلة - الكيمياء التحليليه
الفهرس
Only 14 pages are availabe for public view

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Abstract

Part I
This part contained a general introduction about the chemical names, structures, molecular formulae,molecular weights, physical properties, pharmacological actions and therapeutic uses of the studied drugs. It also contains literature reviews for the pharmacopoeial and other reported methods of analysis for selected drugs in pharmaceutical dosage forms, biological samples and other possible matrices.
Part II This part deals with the development, validation and application of an HPLC-DAD method for the determination of nine antimicrobials and proton pump inhibitors, namely, amoxicillin (AMX), doxycycline (DOX), furazolidone (FRZ), lansoprazole (LNS), levofloxacin (LVF), metronidazole (MTZ), omeprazole (OMZ), pantoprazole (PNZ) and tinidazole (TNZ). The nine drugs are used for treatment of Helicobacter Pylori infection. Effective chromatographic separation between the nine drugs was achieved using Agilent Zorbax Eclipse plus-C18 analytical column (250 x 4.6 mm, 5 μm particle size) and a mobile phase composed phosphate buffer pH 5 and acetonitrile in gradient elution program. The gradient elution started with buffer and acetonitrile ratio 90:10 then it waschanged in 15 min to reach 40:60 by volume. The mobile phase was pumped at a flow rate of 1mL/min. Quantification of the analytes was based on measuring peak areas of AMX at 230 nm, LVF, LNS and PNZ at 290 nm, OMZ at 300 nm, MTZ and TNZ at 320 nm, and DOX and FRZ at 360 nm. The separated compounds eluted at retention times 5.68, 6.43, 7.82, 8.84, 9.42, 10.75, 12.82, 13.74 and 14.90 min for AMX, MTZ, LVF, TNZ, DOX, FRZ, OMZ, PNZ and LNS respectively. Analytical performance of the proposed HPLC procedure was statistically validated with respect to linearity, ranges, precision, accuracy, robustness, detection and quantification limits. The linear dynamic ranges were 5-100, 5-50, 2-40, 10-100, 10-100, 5-50, 2.5-30, 3-30 and 2-30 μg/mL for AMX, MTZ, LVF, TNZ, DOX, FRZ, OMZ, PNZ and LNS, respectively with correlation coefficients > 0.9993. The validated method was successfully applied to the analysis of several laboratory-prepared binary dosage forms as well as analysis of several ternary mixtures in spiked simulated intestinal fluid.
Part III This part deals with a highly selective and sensitive fluorescence assay for kanamycin has been developed that depends on complementation of two splits of DNA aptamer. One DNA split was labeled with CuS nanoparticle and the other was decorated with biotin, which enabled coupling with streptavidin magnesphere paramagnetic particles (PMPs). Complementation of the two-aptamer splits happened only in the presence of kanamycin and the subsequent sandwich was separated via a magnet.
110The released Cu(II) was reduced to Cu(I) by sodium ascorbate and finally catalyzed the click reaction between fluorogenic 3-azido-7-hydroxycoumarin and propargyl alcohol to afford the corresponding fluorescent 1,4-disubstituted-1,2,3-triazole. The fluorescence signal produced (λex.= 365 nm, λem.= 470 nm) was dependent on kanamycin concentration. Fluorescence signal amplification was found to be in good linear relationship with the logarithm of kanamycin concentration in the range of 0.04-20nM. Furthermore, the proposed assay showed a good reproducibility, high selectivity and low detection limits for kanamycin determination. In addition, the capability of the proposed method to detect kanamycin in biological samples with satisfactory results was demonstrated.
Part IV This part describes two green and simple spectrophotometric methods were developed for the determination of kanamycin sulfate (KNM) in its dosage forms. Method I is based on formation of a binary complex with eosin in citric phosphate buffer pH 3.5 and the product was measured at 548 nm. Method II depends on the reaction of KNM with vanillin in borate buffer pH 12 to produce a colored chromogen which showed maximum absorbance at 404 nm. Different experimental variables influencing development and stability of the colored products were optimized. Validation of the developed procedures regarding linearity, ranges, precision, accuracy, robustness and limits of detection and quantification was performed. The absorbance-concentration plots were found linear over KNM ranges of 1-5 and 5-30 μg/mL for methods I and II respectively with correlation coefficients > 0.9993. The validated methods were successfully applied to the analysis of commercial suspension containing the drug. The main advantages of the proposed methods are being simple, inexpensive, green (done almost entirely in aqueous media) and with no requirement for laborious extraction procedure