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Article
SPECTROPHOTOMETRIC DETERMINATION OF BINARY MIXTURE OFSOME آ-LACTAM ANTIBIOTICS

Authors: Shahbaz A. Maki --- Nabil S. Nassory --- Khaleda H. Al-Saidi
Journal: Al-Nahrain Journal of Science مجلة النهرين للعلوم ISSN: (print)26635453,(online)26635461 Year: 2009 Volume: 12 Issue: 3 Pages: 33-44
Publisher: Al-Nahrain University جامعة النهرين

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Abstract

Derivative spectrophotometric techniques (first, second, third and fourth derivative) were
developed for the determination of four â-lactam antibiotic binary mixtures; in combinations
containing these compounds. The simultaneous determination of these compounds was
accomplished by derivative (1D, 2D, 3D and 4D) spectrophotometric technique and applying zerocrossing
technique amoxiclline trihydrate with cephalexin monohydrate (mix I) using 1D spectrum
zero crossing at valley 238.2 nm, and 2D spectrum at valley 263.8 nm, respectively, amoxiclline
trihydrate with cloxacillin sodium (mix II) using 2D at valley 281 and 4D at valley 230.6,
respectively, cephalexin monhydrate with cloxacillin sodium (mix III) using 1D spectrum zero
crossing at 272 nm and 2D spectrum at 253.2 nm, respectively and ampicillin trihydrate with
cloxacillin sodium (mix IV) using 1D at 282nm and 2D at 271.6 nm, respectively. From this
studying it was noticed that in all the applications of the previous methods the correlation
coefficient of calibration curves not less than 0.999 and the relative standard deviation not exceed to
0.214. The four described procedures were successfully applied to the determination of these
compounds in synthetic mixtures and in preparations with high percentage of recovery, accuracy
and precision .The procedures do not require any separation step.


Article
PREPARATION AND STUDY OF AMOXICILLIN SELECTIVE ELECTRODES AND THEIR APPLICATION WITH DERIVATIVE SPECTROPHOTOMETER IN PHARMACEUTICAL DRUGS

Authors: Shahbaz A. Maki --- Nabil S. Nassory --- Khaleda H. Al-Saidi
Journal: Al-Nahrain Journal of Science مجلة النهرين للعلوم ISSN: (print)26635453,(online)26635461 Year: 2009 Volume: 12 Issue: 1 Pages: 29-37
Publisher: Al-Nahrain University جامعة النهرين

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Abstract

Amoxicillin trihydrate selective electrodes were prepared based on amoxicillin-phosphotungstate (Amox-PT) as an active sensor with different plasticizers, di-butyl phosphate (DBP), di-butyl phthalate (DBPH), di-octyl phthalate (DOPH), tri-butyl phosphate (TBP) and o-nitro phenyl octyl ether (NPOE) in PVC matrix membranes. The study was carried out to investigate the electrode parameters, effect of pH, selectivity and UV-derivative spectrophotometer technique. Internal filling solution of 10-3 M + 10-3 M NaCl was used to fill the electrodes. The best electrode was based on DBP plasticizer which gave a slope 58.7 mV/decade and detection limit of 2 x 10-6 M displayed good stability and reproducibility. The electrode was used to determine the amoxicillin in oral suspension and capsules. The results were compared with UV-derivative spectrophotometer technique and the recovery for the drugs obtained by second derivative are quite comparable with the recovery obtained by amoxicillin electrodes.

حضرت أقطاب ﺇنتقائية للأموكسيسلين بتحضير المادة الفعالة (أموكسيسلين- فوسفوتنكستيت) Amox-PT مع الملدنات المختلفة وهي داي بيوتيل فوسفيت (DBP) , داي بيوتيل فثاليت (DBPH) ,داي اوكتيل فثاليت (DOPH) ,ثراي بيوتيل فوسفيت (TBP) و اورثو نيترو فنيل ﺇيثر (NPOE) في غشاء اصله من بولي فاينيل كلورايد .(PVC) الدراسة شملت خواص ألأقطاب كتأثير الدالة الحامضية pH, المحلول الداخلي للأقطاب, الأنتقائية . ﺇن أفضل قطب المحضر باستعمــال المـلدن DBP والمحـلول الداخلـي (10-3M Amox+10-3M NaCl) حيث ان الميل 58.7 mV/decade وبحدود تحسس 2x10-6M وله ثبوتية وتكرارية جيدة. ﺇن هذا القطب أستخدم لتقدير الأموكسيسلين في المستحضرات الدوائية الكبسول والمعلق الفموي. النتائج تطابقت مع نتائج المشتقة الطيفية الثانية.


Article
Preparation of New HPLC Stationary Phase and Study of Its Chromatographic Performance Toward the Separation of Some Water-Soluble Vitamins

Authors: Saif S. Abdull-Sattar --- Shahbaz A. Maki --- Noor M. Ali
Journal: Al-Nahrain Journal of Science مجلة النهرين للعلوم ISSN: (print)26635453,(online)26635461 Year: 2013 Volume: 16 Issue: 2 Pages: 51-58
Publisher: Al-Nahrain University جامعة النهرين

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Abstract

A new stationary phase was prepared by the reaction of a crystal violet solution with silica gel. The capacity of the new prepared resin was calculated and the found average was 6.6meq./g. The resulted resin was highly rigid with high stability and used as stationary phase for HPLC column. Some water-soluble vitamin C, B2, B6, and B12 were examined by this column with isocratic eluention distilled water and methanol (2:98, (v/v)) as a mobile phase with flow rate of 0.5 ml/min and UV detection of 230 nm. The chromatographic performance of the packed column was characterized. The number of plate numbers (N), height equivalent of a theoretical plates (H), capacity factors (K), selectivity factors (α), peaks asymmetry and Resolution (Rs) were measured by analyzing different analytes on the new columns using different mobile phase compositions and flow rates.

تم تحضير طور ثابت جديد بطريقة كروموتوكرافيا السائل ذات الاداء العالي من تفاعل صبغة البنفسجي مع السليكا جيل. وقد تم حساب سعة الراتنج الجديد وقد وجدت 6.6 meq/g. درست استقرارية المجموعة الفعالة الجديدة المرتبطة مع مذيبات مختلفة مثل الميثانول ,الايثانول ,البنزين, الكلوروفورم وغيرها من المذيبات وقد وجد أن الراتنج الجديد مستقر ولم يلاحظ أي استنفاذ أو إفراغ. تم تحليل بعض الفيتامينات بواسطة هذا العمود مثل (C,B2,B6 and B12) باستخدام طورمتحرك يتكون من 2% ماء مقطر و98 % ميثانول وسرعة جريان 0.5 مل بالدقيقه عند طول موجي 230 nm باستخدام كاشف الاشعه فوق البنفسجيه.بعدها تم قياس كفاءة العمود المعبأ بحساب عدد الصفيحات النظرية, الارتفاع المكافئ للصفيحات النظرية , عوامل الاستيعاب وعوامل الانتقائية بواسطة تحليل محاليل مختلفة على العمود الجديد باستخدام أطوار متحركة مختلفة النسب وسرع جريان مختلفة.

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